Fundamentals of Vacuum Technologies Part 2
Fundamentals of Vacuum Technologies Part 2
4.4 Gas admission and pressure areas for the metallic, glass and ceramic components will be needed along
adaptation with specifications on the material and dimensions of the cathode (and
ultimately regarding the electron impact energy for the ion source as well).
The CIS is divided into two sections: a cathode chamber where the
4.4.2 Pressure converter electrons are emitted, and an impact chamber, where the impact ionization
of the gas particles takes place. The two chambers are pumped
In order to examine a gas mix at total pressure exceeding 1 á 10-4 mbar it is differentially: the pressure in the cathode chamber comes to about
necessary to use pressure converters which will not segregate the gases. 10-5 mbar, that in the impact room about 10-3 mbar. The gas from the
Figure 4.7 is used to help explain how such a pressure converter works: vacuum chamber is allowed to pass into the impact chamber by way of a
a. Process pressure < 1 mbar: Single-stage pressure converter. Gas is metal-sealed, bakeable valve (pressure converter, ultrahigh vacuum
allowed to pass out of the vacuum vessel in molecular flow, through a technology). There high-yield ionization takes place at about 10-3 mbar. The
diaphragm with conduc- tance value L2 and into the Òsensor chamberÓ (with electrons exerting the impact are emitted in the cathode chamber at about
its own high vacuum system). Molecular flow causes segregation but this 10-5 mbar and pass through small openings from there into the impact
will be independent of the pressure level (see Section 1.5). A second chamber. The signal-to-noise ratio (residual gas) via ˆ vis the open ion
diaphragm with molecular flow, located between the sensor chamber and source will be increased overall by a factor of 10+3 or more. Figure 4.8
the turbomolecular pump, will compensate for the segregation occurring at shows the fundamental difference between the configurations for open and
L2. closed ion sources for a typical application in sputter technology. With the
modified design of the CIS compared with the open ion source in regard to
b. Process pressure > 1 mbar: Two-stage pressure converter. Using a small both the geometry and the electron energy (open ion source 102 eV, CIS
(rotary vane) pump a laminar stream of gas is diverted from the rough 75 or 35 eV), different fragment distribution patterns may be found where a
vacuum area through a capillary or diaphragm (conductance value L3). lower electron energy level is selected. For example, the argon36++ isotope
Prior to entry into the pump, at a pressure of about 1 mbar, a small part of at mass of 18 cannot be detected at electron energy of less than 43.5 eV
this flow is again allowed to enter the sensor chamber through the and can therefore not falsify the detection of H2O+ at mass 18 in the sputter
diaphragm with conductance value L2, again as molecular flow. processes using argon as the working gas Ð processes which are of great
A falsification of the gas composition resulting from adsorption and importance in industry.
condensation can be avoided by heating the pressure converter and the
capillary.
4.4.4 Aggressive gas monitor (AGM)
To evaluate the influence on the gas composition by the measurement unit
itself, information on the heating temperature, the materials and surface In many cases the process gas to be examined is so aggressive that the
cathode would survive for only a short period of time. The AGM uses the
Non-segregating gas inlet system property of laminar flow by way of which there is no ÒreverseÓ flow of any
kind. Controlled with a separate AGM valve, a part of the working gas fed to
Stage B Stage A the processes is introduced as Òpurging gasÓ, ahead of the pressure
p ≤ 10 –4 mbar p = 1 ... 10 mbar p = 10 ... 1000 mbar
converter, to the TRANSPECTOR; this sets up a flow toward the vacuum
L2 L3
chamber. Thus process gas can reach the TRANSPECTOR only with the
Mass Capillary
⌣
⌢ AGM valve closed. When the valve is open the TRANSPECTOR sees only
spectrometer QHV
pure working gas. Fig. 4.9 shows the AGM principle.
⌣
⌢
L1
Seff QPumping
No
Molecular flow Laminar flow
segregation
L2 molecular → λ ≫ dL 2
1 QHV ≪ QPumping
L2 ~ CD
M (Transition laminar/molecular)
1
L1 ~ CD
M
Seff ≫ L1 → Seff ~ 1
CD
M
Fig. 4.7 Principle of the pressure converter (stage B only in the single-stage version and
stages A and B in two-stage units)
99
Mass spectrometry
Impact chamber
10 -5
10 -5
10 -5
10 -3 Cathode chamber
Example of the sputter „Exit diaphragm“
process
To be detected is 1 ppm N2 as
contamination in argon,
the working gas
10 -5 10 -5 10 -5 10 -5
Fig. 4.8 Open ion source (left) and closed ion source (right)
Impact chamber
Working gas for the process (Ar)
Cathode chamber
“Exit diaphragms”
AGM protective gas valve
10 -5
Process:
e. g. 50 mbar 10 -3 10 -5
Diaphragm Pump
10 -5
100
Mass spectrometry
Often an expression such as Òunit resolution with 15% valleyÓ is used. This Noise amplitude Æ á i+ = 4 á 10Ð14 A
R
means that the Òbottom of the valleyÓ between two adjacent peaks of
4 ⋅ 10 – 14A
identical height comes to 15 % of the height of the peak or, put another pmin(FC) = = 4 ⋅10 – 10 mbar
1⋅10 – 4A / mbar
way, at 7.5 % of its peak height the line width DM measured across an
individual peak equals 1 amu (atomic mass unit); see in this context the
schematic drawing in Fig. 4.10.
100%
+
i
15%
1 amu
7,5%
∆M
101
Mass spectrometry
H 1 1 99.985
2 0.015
He 2 3 0.00013
4 Å 100.0
B 5 10 19.78
11 80.22
+
log i
C 6 12 98.892
Regulation
13 1.108
N 7 14 99.63
Exact measurement 15 0.37
range
O 8 16 99.759
Automatic shut-down:
17 0.0374
≈ 5 · 10 –4 18 0.2039
F 9 19 100.0
Ne 10 20 90.92
21 0.257
22 8.82
10–8
10 –7
10 –6 –5
10 10–4
10 –3 log P
Na 11 23 100.0
Fig. 4.12 Qualitative linearity curve Table 4.2 Relative frequency of isotopes
102
Mass spectrometry
Al 13 27 100.0 10
+
Ar
P 15 31 100.0 4
S 16 32 95.06 2
33 0.74
34 4.18
0 100 200 300 400 500
36 0.016
Electron energy (eV)
Cl 17 35 75.4
Threshold
37 24.6 energy Ar+ 15,7 eV Ar++ 43,5 eV Ar3+ 85,0 eV Ar4+ 200 eV
for argon ions
Ar 18 36 0.337
38 0.063 Fig. 4.13 Number of the various Ar ions produced, as a factor of electron energy level
40 99.60
4) Finally, gas molecules are often broken down into fragments by
Kr 36 78 0.354 ionization. The fragment distribution patterns thus created are the so-
80 2.27 called characteristic spectra (fingerprint, cracking pattern). Important: In
82 11.56 the tables the individual fragments specified are standardized either against
83 11.55 the maximum peak (in % or ä of the highest peak) or against the total of all
84 56.90 peaks (see the examples in Table 4.4).
86 17.37
Both the nature of the fragments created and the possibility for multiple
ionization will depend on the geometry (differing ion number, depending on
Xe 54 124 0.096 the length of the ionization path) and on the energy of the impacting
126 0.090 electrons (threshold energy for certain types of ions). Table values are
128 1.919 always referenced to a certain ion source with a certain electron energy
129 26.44 level. This is why it is difficult to compare the results obtained using devices
130 4.08 made by different manufacturers.
131 21.18
132 26.89 Often the probable partial pressure for one of the masses involved will be
134 10.44 estimated through critical analysis of the spectrum. Thus the presence of air
136 8.87 in the vacuum vessel (which may indicate a leak) is manifested by the
detection of a quantity of O2+ (with mass of 32) which is about one-quarter
Table 4.2 Relative frequency of isotopes
There are threshold energy levels for the impacting electrons for all
ionization states for every type of gas, i.e., each type of ion can be formed
only above the associated energy threshold. This is shown for Ar in Fig.
4.13.
3) Specific ionization of the various gases Sgas, this being the number of
ions formed, per cm and mbar, by collisions with electrons; this will vary
from one type of gas to the next. For most gases the ion yield is greatest at
an electron energy level between about 80 and 110 eV; see Fig. 4.14.
In practice the differing ionization rates for the individual gases will be taken
into account by standardization against nitrogen; relative ionization Electron energy (eV)
probabilities (RIP) in relationship to nitrogen will be indicated (Table 4.3).
Fig. 4.14 Specific ionization S for various gases by electrons exhibiting energy level E
103
Mass spectrometry
104
Mass spectrometry
Table 4.5 Spectrum library of the 6 highest peaks for the TRANSPECTOR
of the share of N2+ with its mass of 28. If, on the other hand, no oxygen is of carbon monoxide, on the other hand, there will always appear Ð in
detected in the spectrum, then the peak at atomic number 28 would addition to CO+ Ð the fragmentary masses of 12 (C+) and 16 (O++
2 )).
indicate carbon monoxide. In so far as the peak at atomic number 28
Figure 4.15 uses a simplified example of a Òmodel spectrumÓ with
reflects the CO+ fragment of CO2 (atomic number 44), this share is 11 % of
superimpositions of hydrogen, nitrogen, oxygen, water vapor, carbon
the value measured for atomic number 44 (Table 4.5). On the other hand, in
monoxide, carbon dioxide, neon and argon to demonstrate the difficulties
all cases where nitrogen is present, atomic number 14 (N++ 2 ) will always be involved in evaluating spectra.
found in the spectrum in addition to the atomic number 28 (N2+); in the case
105
Mass spectrometry
CO+
O+
O+
H2+ Ar++ CO+
H 2 O+ O2 + Ar+ CO2+
H2+
O+
N+
H+ OH+ Ne+ N2+
C+ O+
13C+ H3O+ 22Ne +
13CO+
+
H+ Ne++ C 16O18O+ 36Ar+ 13C16O +
2
14N15N+
0 5 10 15 20 25 30 35 40 45 50
Hydrogen Oxygen Carbon dioxide Argon
Nitrogen Water Neon Carbon monoxide
Evaluation problems: The peak at atomic number 16 may, for example, be due to oxygen fragments resulting from O2, H2O, CO2 and CO; the peak at atomic number 28 from contributions
by N2 as well as by CO and CO as a fragment of CO2; the peak at atomic number 20 could result from singly ionized Ne and double-ionized Ar.
In order to maintain the number of ions arriving at the ion trap, it is 4.6.3 Qualitative gas analysis
necessary to multiply the number above with the transmission factor TF(m),
The analysis of spectra assumes certain working hypotheses:
which will be dependent on mass, in order to take into account the
permeability of the separation system for atomic number m (analogous to 1. Every type of molecule produces a certain, constant mass spectrum or
this, there is the detection factor for the SEMP; it, however, is often already fragment spectrum which is characteristic for this type of molecule
contained in TF). The transmission factor (also: ion-optical transmission) is (fingerprint, cracking pattern).
thus the quotient of the ions measured and the ions produced.
2. The spectrum of every mixture of gases is the same as would be found
106
Mass spectrometry
through linear superimposition of the spectra of the individual gases. many gas components; here a qualitative analysis will have to be made
The height of the peaks will depend on the gas pressure. before attempting quantitative analysis. The degree of difficulty encountered
will depend on the number of superimpositions (individual / a few / many).
3. The ion flow for each peak is proportional to the partial pressure of each
component responsible for the peak. Since the ion flow is proportional to In the case of individual superimpositions, mutual, balancing of the ion
the partial pressure, the constant of proportionality (sensitivity) varies flows during measurement of one and the same type of gas for several
from one gas to the next. atomic numbers can often be productive.
Although these assumptions are not always correct (see Robertson: Mass Where there is a larger number of superimpositions and a limited number of
Spectrometry) they do represent a useful working hypothesis. gases overall, tabular evaluation using correction factors vis ˆ vis the
spectrum of a calibration gas of known composition can often be helpful.
In qualitative analysis, the unknown spectrum is compared with a known
spectrum in a library. Each gas is Òdefinitively determinedÓ by its spectrum.
The comparison with library data is a simple pattern recognition process.
Depending on the availability, the comparison may be made using any of a
number ancillary aids. So, for example, in accordance with the position,
size and sequence of the five or ten highest peaks. Naturally, comparison is Parent spectrum
possible only after the spectrum has been standardized, by setting the
height of the highest line equal to 100 or 1000 (see Table 4.5 as an
example).
The comparison can be made manually on the basis of collections of tables A A = Parent
range
(for example, A. Cornu & R. Massot: Compilation of Mass Spectral Data) or
may be effected with computer assistance; large databases can be used
(e.g. Mass Spectral Data Base, Royal Society of Chemistry, Cambridge).
When making comparisons with library information, it is necessary to pay Parent spectrum Assumption:
Groups
attention to whether identical ion sources or at least identical electron 2 1
1 = Kr ypton +
impact energies were used. 2 = Krypton ++
All these capabilities are, however, generally too elaborate for the problems
encountered in vacuum technology. Many commercial mass spectrometers Library spectrum:
can show a number of library spectra in the screen so that the user can see Krypton
immediately whether the Òlibrary substanceÓ might be contained in the sub-
stance measured. Usually the measured spectrum was the result of a mix
of gases and it is particularly convenient if the screen offers the capacity for Parent spectrum without krypton Assumption:
subtracting (by way of trial) the spectra of individual (or several) gases from 3 Argon +
4
the measured spectrum. The gas can be present only when the subtraction 3 4 Argon ++
does not yield any negative values for the major peaks. Figure 4.16 shows
such a step-by-step subtraction procedure using the Transpector-Ware
software. Library spectrum:
Argon
Regardless of how the qualitative analysis is prepared, the result is always
just a ÒsuggestionÓ, i.e. an assumption as to which gases the mixture might
contain. This suggestion will have still to be examined, e.g. by considering Parent spectrum without argon Assumption:
the likelihood that a certain substance would be contained in the spectrum. 5 Neon +
In addition, recording a new spectrum for this substance can help to 5
achieve clarity.
Library spectrum:
4.6.4 Quantitative gas analysis Neon
107
Mass spectrometry
In the most general case a plurality of gases will make a greater or lesser FFT á i = FFT á FF á I
contribution to the ion flow for all the masses. The share of a gas g in each
which can be evaluated direct by the computer. The ion current vector for
case for the atomic number m will be expressed by the fragment factor
the individual gases is then:
Ffm,g. In order to simplify calculation, the fragment factor Ffm,g will also
–1
contain the transmission factor TF and the detection factor DF. Then the ion [FF T ⋅ i] ⋅ [FF T ⋅ BF ]
current to mass m, as a function of the overall ion currents of all the gases I=
det[FF T ⋅ BF ]
involved, in matrix notation, is:
i j+ BFj, k ⋅ ⋅ ⋅ ⋅ ⋅ BF j,o I k+
⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅
⋅
⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅
i + ⋅ ⋅ ⋅ FFm, g ⋅ ⋅ ⋅ · I g+
= 4.7 Software
m
⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅
⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅
+ 4.7.1 Standard SQX software (DOS) for
iu BFu, k ⋅ ⋅ ⋅ ⋅ ⋅ BFu,o I o+
stand-alone operation (1 MS plus 1
PC, RS 232)
The ion current vector for the atomic numbers m (resulting from the contri-
butions by the fragments of the individual gases) is equal to the fragment The conventional software package (SQX) contains the standard routines
matrix times the vector of the sum of the flows for the individual gases. for the operation of the mass spectrometer (MS)Ð various spectra
0 depictions, queries of individual channels with the corresponding screen
or: im+ = ∑ BFm, g · I g+ displays as tables or bar charts, partial pressure conversion, trend displays,
g=k comparison with spectra libraries (with the capability for trial subtraction of
library spectra), leak testing mode etc. Ð and for sensor balancing, as well.
(in simplified notation: i = FF á I) Using PCs as the computer and display unit naturally makes available all
+ the usual functions including storing and retrieving data, printing, etc.
where im = ion flow vector for the atomic numbers, resulting from
contributions of fragments of various individual gases Characteristic of the conventional software package is that specific
individual spectra will be measured, even though the measurement is fully
0
∑ BFm, g = fragment matrix
automated and takes place at a point in time which is specified in advance.
g=k A spectrum of this type can thus be only a ÒsnapshotÓ of a process in
progress.
I+g = Vector of the sum of the flows for the individual gases or:
Ff m, g
6444474448 4.7.2 Multiplex/DOS software MQX
im = ∑ pg ⋅ E N2 ⋅ RIPg ⋅ FFm ⋅ TFm
+ (1 to 8 MS plus 1 PC, RS 485)
Transmission factor The first step toward process-oriented software by LEYBOLD is the MQX. It
for the mass m
makes possible simultaneous monitoring of a maximum of eight sensors
Fragment factor
for the gas to mass m and you can apply all the SQX functions at each sensor.
Relative ionization probability
for the gas
Nitrogen sensitivity (equipment constant)
Partial pressure of the gas 4.7.3 Process-oriented software –
Ion current for atomic number m
Transpector-Ware for Windows
One sees that the ion flow caused by a gas is proportional to the partial
Transpector-Ware is based on an entirely new philosophy. During the
pressure. The linear equation system can be solved only for the special
course of the process (and using settings Ð the ÒrecipeÓ Ð determined
instance where m = g (square matrix); it is over-identified for m > g. Due to
beforehand) data will be recorded continuously Ð like the individual frames
unavoidable measurement error (noise, etc.) there is no set of overall ion
in a video. These data can be stored or otherwise evaluated. It is possible
flow I+g (partial pressures or concentrations) which satisfies the equation
in particular to analyze interesting process sections exactly, both during the
system exactly. Among all the conceivable solutions it is now necessary to
process and retroactively, once the process has run to completion, without
identify set Ig+* which after inverse calculation to the partial ion flows Im
+
*
having to interrupt the measurement operations which are running in the
will exhibit the smallest squared deviation from the partial ion currents i+m
background. Where ongoing monitoring of identical processes is
actually measured. Thus:
undertaken the program can generate statistics (calculating mean values
∑(im − im*) = min
+ + 2 and standard deviations) from which a bandwidth for Òfavorable process
operationÓ can be derived. Error reports are issued where limit values are
This minimization problem is mathematically identical to the solution of exceeded.
another equation system
108
Mass spectrometry
4.7.4 Development software – seconds (thus by an overall factor of 100), respectively. By comparison, in
TranspectorView the sequence a-d-e-f, at constant integration time, the total pressure was
raised in three steps, from 7.2 á 10-6 mbar to 7.2 á 10-5 mbar (or by a factor
This software used to for develop custom software versions for special of just 10 overall).
situations. It is based on the LabView development package and includes
the drivers required to operate the Transpector.
4.9 Maintenance
4.8 Partial pressure regulation (Cathode service life, sensor balancing, cleaning the ion source and rod
system)
Some processes, such as reactive sputter processes, require the most
constant possible incidence rates for the reacting gas molecules on the The service life of the cathode will depend greatly on the nature of the
substrate being coated. loading. Experience has shown that the product of operating period
multiplied by the operating pressure can serve as a measure for the
The Òincidence rateÓ is the same as the Òimpingement rateÓ discussed in loading. Higher operating pressures (in a range of 1 á 10-4 to 1 á 10-3 mbar)
Chapter 1; it is directly proportional to the partial pressure. The simplest have a particularly deleterious effect on service life, as do certain chemical
attempt to keep the partial pressure for a gas component constant is influences such as refrigerants, for example. Changing out the cathode is
throughput by regulating with a flow controller; it does have the quite easy, thanks to the simple design of the sensor. It is advisable,
disadvantage that the regulator cannot determine whether, when and where however, to take this opportunity to change out or at least clean the entire
the gas consumption or the composition of the gas in the vacuum chamber ion source.
changes. The far superior and more effective option is partial pressure
control using a mass spectrometer via gas inlet valves. Here the significant Sensor balancing at the mass axis (often erroneously referred to as
peaks of the gases being considered are assigned to channels in the mass calibration) is done today in a very easy fashion with the software (e.g.
spectrometer. Suitable regulators compare the analog output signals for SQX, Transpector-Ware) and can be observed directly in the screen.
these channels with set-point values and derive from the difference Naturally, not only the arrangement along the mass axis will be determined
between the target and actual values for each channel the appropriate here, but also the shape of the lines, i.e. resolution and sensitivity (see
actuation signal for the gas inlet valve for the channel. A configuration of Section 4.5).
this kind has been realized to control six channels in the QUADREX PPC. It will be necessary to clean the sensor only in exceptional cases where it
Gas inlet valves matching the unit can also be delivered. is heavily soiled. It is usually entirely sufficient to clean the ion source,
The gas used to measure the impingement rate (partial pressure) must which can be easily dismantled and cleaned. The rod system can be
naturally be drawn from a representative point in the vacuum chamber. cleaned in an ultrasonic bath once it has been removed from the config-
When evaluating the time constant for a regulation circuit of this type it is uration. If dismantling the system is unavoidable due to particularly
important to take into account all the time aspects and not just the electrical stubborn grime, then the adjustment of the rods which will be required
signal propagation and the processing in the mass spectrometer, but also afterwards will have to be carried out at the factory.
the vacuum-technology time constants and flow velocities, as illustrated in
Figure 4.17. Pressure converters or unfavorably installed gas inlet lines
joining the control valve and the vacuum vessel will make particularly large
contributions to the overall time constant. It is generally better to establish a
favorable S/N ratio with a large signal (i.e. through an inlet diaphragm with
a large opening) rather than with long integration periods at the individual
channels. Contrasted in Figure 4.18 are the effects of boosting pressure a b c
and lengthening the integration time on signal detectability. In depictions a,
b and c only the integration period was raised, from 0.1 to 1.0 and 10
t4
t5
Mass spectrometer
Pressure stage
d e f
Regulation valve t1 ⌣
ef
⌢
Sensor
t6 t2 t3
e Vacuum vessel ef
e
TMP50CF
Fig. 4.18 Improving the signal-to-noise ratio by increasing the pressure or extending the
Fig. 4.17 Partial shares for overall time constants integration time
109
Leak detection
5. Leaks and their 5.2 Leak rate, leak size, mass flow
detection No vacuum device or system can ever be absolutely vacuum-tight and it
does not actually need to be. The simple essential is that the leak rate be
Apart from the vacuum systems themselves and the individual components low enough that the required operating pressure, gas balance and ultimate
used in their construction (vacuum chambers, piping, valves, detachable pressure in the vacuum container are not influenced. It follows that the
[flange] connections, measurement instruments, etc.), there are large requirements in regard to the gas-tightness of an apparatus are the more
numbers of other systems and products found in industry and research stringent the lower the required pressure level is. In order to be able to
which must meet stringent requirements in regard to leaks or creating a so- register leaks quantitatively, the concept of the Òleak rateÓ with the symbol
called ÒhermeticÓ seal. Among these are many assemblies and processes QL was introduced; it is measured with mbar á l/s or cm3/s (STP) as the unit
in the automotive and refrigeration industries in particular but also in many of measure. A leak rate of QL = 1 mbar á l/s is present when in an enclosed,
other branches of industry. Working pressure in this case is often above evacuated vessel with a volume of 1 l the pressure rises by 1 mbar per
ambient pressure. Here Òhermetically sealedÓ is defined only as a relative second or, where there is positive pressure in the container, pressure drops
Òabsence of leaksÓ. Generalized statements often made, such as Òno by 1 mbar. The leak rate QL defined as a measure of leakiness is normally
detectable leaksÓ or Òleak rate zeroÓ, do not represent an adequate basis specified in the unit of measure mbar á l/s. With the assistance of the status
for acceptance testing. Every experienced engineer knows that properly equation (1.7) one can calculate QL when giving the temperature T and the
formulated acceptance specifications will indicate a certain leak rate (see type of gas M, registering this quantitatively as mass flow, e.g. in the g/s
Section 5.2) under defined conditions. Which leak rate is acceptable is also unit of measure. The appropriate relationship is then:
determined by the application itself.
∆(p ⋅ V ) R ⋅ T ∆m
QL = = ⋅ (5.1)
∆t M ∆t
5.1 Types of leaks where R = 83.14 mbar á l/mol á K, T = temperature in K; M = molar mass in
Differentiation is made among the following leaks, depending on the nature g/mole; ∆m for the mass in g; ∆t is the time period in seconds. Equation
of the material or joining fault: 5.1 is then used
• Leaks in detachable connections: a) to determine the mass flow ∆m / ∆t at a known pV gas flow of ∆p á V/∆t
Flanges, ground mating surfaces, covers (see in this context the example at 5.4.1) or
• Leaks in permanent connections: b) to determine the pV leak gas flow where the mass flow is known (see
Solder and welding seams, glued joints the following example).
• Leaks due to porosity: particularly following mechanical deformation Example for case b) above:
(bending!) or thermal processing of polycrystalline materials and cast
A refrigeration system using Freon (R 12) exhibits refrigerant loss of 1 g of
components
Freon per year (at 25 ¡C). How large is the leak gas flow QL? According to
• Thermal leaks (reversible): opening up at extreme temperature loading equation 5.1 for M(R12) = 121 g/mole:
(heat/ cold), above all at solder joints ∆( p ⋅V ) . mbar ⋅ ℓ⋅ 298K ⋅ 1g
8314
QL = =
∆t mol ⋅ K ⋅ 121g ⋅ mol –1⋅ 1year
• Apparent (virtual) leaks: quantities of gas will be liberated from hollows
and cavities inside cast parts, blind holes and joints (also due to the
. ⋅ 2.98 ⋅102⋅ 1 mbar ⋅ ℓ
8314
evaporation of liquids) = ⋅
121⋅1 . ⋅107s
315
• Indirect leaks: leaking supply lines in vacuum systems or furnaces
. ⋅ 2.98⋅102 –7 mbar ⋅ ℓ
8314
(water, compressed air, brine) = ⋅ 10 ⋅
1.21⋅102⋅ 315
. s
• ÒSerial leaksÓ: this is the leak at the end of several Òspaces connected in
seriesÓ, e.g. a leak in the oil-filled section of the oil pan in a rotary vane mbar ⋅ ℓ
= 65 ⋅10–7⋅
pump s
• ÒOne-way leaksÓ: these will allow gas to pass in one direction but are Thus the Freon loss comes to QL = 6.5 á 10Ð6 mbar á l/s. According to the
tight in the other direction (very seldom) Òrule of thumbÓ for high vacuum systems given below, the refrigeration
system mentioned in this example may be deemed to be very tight.
An area which is not gas-tight but which is not leaky in the sense that a
Additional conversions for QL are shown in Tables VIIa and VIIb in
defect is present would be the
Chapter 9.
• Permeation (naturally permeability) of gas through materials such as
The following rule of thumb for quantitative characterization of high vacuum
rubber hoses, elastomer seals, etc. (unless these parts have become
equipment may be applied:
brittle and thus ÒleakyÓ).
Total leak rate < 10-6 mbar á l/s:
Equipment is very tight
110
Leak detection
Total leak rate 10-5 mbar á l/s: hole 1 cm in diameter QL (air) will be 2.6 á 104 mbar á l/s. If all other
Equipment is sufficiently tight conditions are kept identical and helium is allowed to flow into the hole at its
speed of sound of 970 m/s, then in analogous fashion the QL (helium) will
Total leak rate > 10-4 mbar á l/s:
come to 7.7 á 10+4 mbar á l/s, or a pV leaking gas current which is larger by
Equipment is leaky
a factor of 970 / 330 = 2.94. This greater ÒsensitivityÓ for helium is used in
A leak can in fact be ÒovercomeÓ by a pump of sufficient capacity because it leak detection practice and has resulted in the development and mass
is true that (for example at ultimate pressure pend and disregarding the gas production of highly sensitive helium-based leak detectors (see Section
liberated from the interior surfaces): 5.5.2).
QL Shown in Figure 5.1 is the correlation between the leak rate and hole size
p = (5.2) for air, with the approximation value of QL (air) of 10+4 mbar á l/s for the
end S
eff
Ò1 cm holeÓ. The table shows that when the hole diameter is reduced to
1 µm (= 0.001 mm) the leak rate will come to 10-4 mbar á l/s, a value which
(QL Leak rate, Seff the effective pumping speed at the pressure vessel)
in vacuum technology already represents a major leak (see the rule of
Where Seff is sufficiently great it is possible Ð regardless of the value for the thumb above). A leak rate of 10-12 mbar á l/s corresponds to hole diameter
leak rate QL Ð always to achieve a pre-determined ultimate pressure of of 1 •; this is the lower detection limit for modern helium leak detectors.
pend. In practice, however, an infinite increase of Seff will run up against Since the grid constants for many solids amount to several • and the
economic and engineering limitations (such as the space required by the diameter of smaller molecules and atoms (H2, He) are about 1 •, inherent
system). permeation by solids can be registered metrologically using helium leak
detectors. This has led to the development of calibrated reference leaks
Whenever it is not possible to achieve the desired ultimate pressure in an
with very small leak rates (see Section 5.5.2.3). This is a measurable Òlack
apparatus there are usually two causes which can be cited: The presence
of tightnessÓ but not a ÒleakÓ in the sense of being a defect in the material
of leaks and/or gas being liberated from the container walls and sealants.
or joint. Estimates or measurements of the sizes of atoms, molecules,
Partial pressure analysis using a mass spectrometer or the pressure rise viruses, bacteria, etc. have often given rise to everyday terms such as
method may be used to differentiate between these two causes. Since the ÒwatertightÓ or Òbacteria-tightÓ; see Table 5.1.
pressure rise method will only prove the presence of a leak without
Compiled in Figure 5.2 are the nature and detection limits of frequently
indicating its location in the apparatus, it is advisable to use a helium leak
used leak detection methods.
detector with which leaks can, in general, also be located much more
quickly.
Fig. 5.1 Correlation between leak rate and hole size Table 5.1 Estimating borderline leak rates
111
Leak detection
Leak <----> Hole Substance quantity trhough hole per unit of time Helium standard leak rate:
Q ... Leak rate, ∆ (p · V) p1 = 1 bar, p2 < 1 mbar (∆p = 1 bar)
In short: Leak Definition: Q = Test gas = Helium
Helium leak detector ULTRATEST UL 200 dry/UL 500 ∆t
Vacuum method
➔
Contura Z
Familiar leaks: Quantity escaping: Standard He leak rate:
mg mbar · ø mbar · ø
Helium leak detector ULTRATEST UL 200/UL 500 dry/Modul 200/LDS 1000
Dripping water faucet 34 s Water 1 = 6.45 s Air 2 0.17 s He Std
4 mm diam., 1 Hz, ∆p = 4 bar
Pressure rise
mbar · ø mbar · ø
Hair on a gasket 10 –2 s Air 0.9 · 10 –2 s He Std
103................100 10-1 10-2 10-3 10-4 10-5 10-6 10-7 10-8 10-9 10-10 10-11 10-12 mbar · l · s-1
Bicycle tube in water
(bubble test) 3
–3 Ncm mbar · ø
Ecotec II / Protec 2 mm diam., 1 Hz, ∆p = 0.1 bar 4.19 · 10 s 1 = 4.24 · 10 –3
s Air 2 1.88 · 10 –2
mbar · ø
s He Std
Overpressure method
ULTRATEST with helium sniffer Car tire loses air mbar · ø
mbar · ø 4.3 · 10 –5 s He Std
25 l, 6 Mo: 1.8 --> 1.6 bar 3.18 · 10 –4 s Air
Halogen sniffer HLD4000A
Small refrigerant cylinder
g mbar · ø
Bubble test
empties in 1 year 1
430 a Frigen = 2.8 · 10 –3 s F12 2 4.33 · 10 –5
mbar · ø
s He Std
430 g refrigerant R12, 25°C
Fig. 5.2 Leak rate ranges for various leak detection processes and devices Fig. 5.3 Examples for conversion into helium standard leak rates
5.2.1 The standard helium leak rate Here indices ÒIÓ and ÒIIÓ refer to the one or the other pressure ratio and
indices Ò1Ó and Ò2Ó reference the inside and outside of the leak point,
Required for unequivocal definition of a leak are, first, specifications for the respectively.
pressures prevailing on either side of the partition and, secondly, the nature
of the medium passing through that partition (viscosity) or its molar mass.
The designation Òhelium standard leakÓ (He Std) has become customary to
designate a situation frequently found in practice, where testing is carried 5.3 Terms and definitions
out using helium at 1 bar differential between (external) atmospheric
pressure and the vacuum inside a system (internal, p < 1 mbar), the When searching for leaks one will generally have to distinguish between
designation Òhelium standard leak rateÓ has become customary. In order to two tasks:
indicate the rejection rate for a test using helium under standard helium 1. Locating leaks and
conditions it is necessary first to convert the real conditions of use to 2. Measuring the leak rate.
helium standard conditions (see Section 5.2.2). Some examples of such
conversions are shown in Figure 5.3. In addition, we distinguish, based on the direction of flow for the fluid,
between the
112
Leak detection
In the simplest case a leak can be determined qualitatively and, when using
Helium
certain test techniques, quantitatively as well (this being the leak rate)
without the assistance of a special leak detector. Thus the quantity of water
dripping from a leaking water faucet can be determined, through a certain
period of time, using a graduated cylinder but one would hardly refer to this
as a leak detector unit. In those cases where the leak rate can be deter-
mined during the course of the search for the leak without using a leak
Helium
detector (see, for example, Sect. 5.4.1), this will often be converted to the
b: Local leak detection; vacuum inside d: Local leak detection; pressurized test gas helium standard leak rate (Sect. 5.2.1). This standard leak rate value is
specimen inside the specimen
frequently needed when issuing acceptance certificates but can also be of
Fig. 5.4 Leak test techniques and terminology service when comparing leak rate values determined by helium leak
detector devices.
The leak rate which is no longer tolerable in accordance with the
acceptance specifications is known as the rejection rate. Its calculation is In spite of careful inspection of the individual engineering components,
based on the condition that the test specimen may not fail during its leaks may also be present in an apparatus following its assembly Ð be it
planned utilization period due to faults caused by leaks, and this to a due to poorly seated seals or damaged sealing surfaces. The processes
certain degree of certainty. Often it is not the leak rate for the test specimen used to examine an apparatus will depend on the size of the leaks and on
under normal operating conditions which is determined, but rather the the degree of tightness being targeted and also on whether the apparatus is
throughput rate of a test gas Ð primarily helium Ð under test conditions. The made of metal or glass or other materials. Some leak detection techniques
values thus found will have to be converted to correspond to the actual are sketched out below. They will be selected for use in accordance with
application situation in regard to the pressures inside and outside the test the particular application situations; economic factors may play an important
specimen and the type of gas (or liquid) being handled. part here.
113
Leak detection
a shut-off valve, then one may expect an effective pumping speed of about
Seff = 30 l/s. Thus the ultimate pressure will be
Q 6 ⋅ 10 – 5 mbar ⋅ ℓ ⋅ s – 1
pend = L =
Seff 30 ℓ ⋅ s – 1
= 2 ⋅10 – 6 mbar
Pressure
114
Leak detection
As a variation on the spray technique mentioned above, in which the A less frequently employed example of a chemical effect would be that of
escaping gas causes the bubbles, it is possible to place a so-called escaping ammonia when it makes contact with ozalid paper (blueprint
Òvacuum boxÓ with a seal (something like a diverÕs goggles) on the surface paper) or with other materials suitably prepared and wrapped around the
being examined once it has been sprayed with a soap solution. This box is outside of the specimen. Leaks are then detected based on the
then evacuated with a vacuum pump. Air entering from the outside through discoloration of the paper.
leaks will cause bubbles inside the box, which can be observed through a An example of a dye penetration test is the inspection of the tightness of
glass window in the box. In this way it is also possible, for example, to rubber plugs or plungers in glass tubes, used for example in testing
examine flat sheet metal plates for leaks. Vacuum boxes are available for a materials suitability for disposable syringes or pharmaceutical packages.
variety of applications, made to suit a wide range of surface contours. When evaluating tiny leaks for liquids it will be necessary to consider the
115
Leak detection
wetability of the surface of the solid and the capillary action; see also Table 5.5.1 Halogen leak detectors
5.1. Some widely used leak detection methods are shown Ð together with (HLD 4000, D-Tek)
the test gas, application range and their particular features Ð in Table 5.4.
Gaseous chemical compounds whose molecules contain chlorine and/or
Method Test gas Smallest detectable Pressure range Quantitative fluorine Ð such as refrigerants R12, R22 and R134a Ð will influence the
leak rate measurement
mbar ℓ/s g/a R 134 a
emissions of alkali ions from a surface impregnated with a mixture of KOH
Foaming Air and others 10
–4
7 · 10
–1
Positive pressure No and Iron(III)hydroxide and maintained at 800 ¡C to 900 ¡C by an external
liquids
Pt heater. The released ions flow to a cathode where the ion current is
–2
Ultrasonic Air and others 10 70 Positive pressure No
microphone
measured and then amplified (halogen diode principle). This effect is so
–3 –5 –1
great that partial pressures for halogens can be measured down to
Thermal conducti- Gases other 10 – 10 10 – 7 Positive pressure No
vity leak detector than air and vacuum 10-7 mbar.
Halogen Substances 10
–6
7 · 10
–3
Positive pressure With Whereas such devices were used in the past for leak testing in accordance
–5 –1
leak detection containing (10 ) (10 ) (vacuum) limitations
halogens
with the vacuum method, today Ð because of the problems associated with
Universal Refrigerants, 10
–5
7 · 10
–3
Positive pressure Yes
the CFCs Ð more sniffer units are being built. The attainable detection limit
sniffer helium and is about 1 á 10-6 mbar á l/s for all the devisces. Equipment operating in
leak detector other gases
–12 –9
accordance with the halogen diode principle can also detect SF6.
Helium Helium 10 7 · 10 Vacuum, Yes
leak detection 10
–7
7 · 10
–4
positive pressure Consequently these sniffer units are used to determine whether refrigerants
Bubble test Air and other 10
–3
7 Positive pressure No
are escaping from a refrigeration unit or from an SF6 type switch box (filled
gases with arc suppression gas).
–2
Water pressure Water 10 70 Positive pressure No
test
–4 –1
Pressure Air and other 10 7 · 10 Positive pressure Yes
drop test gases 5.5.2 Leak detectors with mass
Pressure Air 10
–4
7 · 10
–1
Vacuum Yes spectrometers (MSLD)
rise test
116
Leak detection
individual component groups are the required electrical- and electronic microprocessor to multiply the signal arriving from the mass spectrometer
supply systems and software which, via a microprocessor, allow for the by a numerical constant and to have the leak rate displayed direct.
greatest possible degree of automation in the operating sequence, including
all adjustment and calibration routines and measured value display.
5.5.2.2 Detection limit, background, gas storage in
oil (gas ballast), floating zero-point
5.5.2.1 The operating principle for a MSLD suppression
The basic function of a leak detector and the difference between a leak The smallest detectable leak rate is dictated by the natural background
detector and mass spectrometer can be explained using Figure 5.6. This level for the gas to be detected. Even with the test connector at the leak
sketch shows the most commonly found configuration for leak detection detector closed, every gas will pass Ð counter to the pumping direction Ð
using the helium spray method (see Section 5.7.1) at a vacuum component. through the exhaust and through the pumps (but will be reduced
When the sprayed helium is drawn into the component through a leak it is accordingly by their compression) through to the spectrometer and will be
pumped thorough the interior of the leak detector to the exhaust, where it detected there if the electronic means are adequate to do so. The signal
again leaves the detector. Assuming that the detector itself is free of leaks, generated represents the detection limit. The high vacuum system used to
the amount of gas flowing through each pipe section (at any desired point) evacuate the mass spectrometer will normally comprise a turbomolecular
per unit of time will remain constant regardless of the cross section and the pump and an oil-sealed rotary vane pump. (Diffusion pumps were used
routing of the piping. The following applies for the entry into the pumping earlier instead of the turbomolecular pumps.) Like every liquid, the sealing
port at the vacuum pump: oil in the rotary vane pump has the capability of dissolving gases until
Q=páS (5.4) equilibrium is reached between the gas dissolved in the oil and the gas
outside the oil. When the pump is warm (operating temperature) this
At all other points equilibrium state represents the detection limit for the leak detector. The
Q = p á Seff (5.4a) helium stored in the oil thus influences the detection limit for the leak
detector. It is possible for test gas to enter not only through the test
applies, taking the line losses into account. connection and into the leak detector; improper installation or inept handling
The equation applies to all gases which are pumped through the piping and of the test gas can allow test gas to enter through the exhaust and the
thus also for helium. airing or gas ballast valve and into the interior of the detector, to increase
the helium level in the oil and the elastomer seals there and thus to induce
QHe = pHe á Seff, He (5.4b) a background signal in the mass spectrometer which is well above the
In this case the gas quantity per unit of time is the leak rate being sought; normal detection limit. When the device is properly installed (see Fig. 5.7)
the total pressure may not be used, but only the share for helium or the the gas ballast valve and the airing valve will be connected to fresh air and
partial pressure for helium. This signal is delivered by the mass the discharge line (oil filter!) should at least be routed to outside the room
spectrometer when it is set for atomic number 4 (helium). The value for Seff where the leak test takes place.
is a constant for every series of leak detectors, making it possible to use a An increased test gas (helium) background level can be lowered by
opening the gas ballast valve and introducing gas which is free of the test
gas (helium-free gas, fresh air). The dissolved helium will be flushed out, so
Test gas
to speak. Since the effect always affects only the part of the oil present in
e.g. He the pump body at the particular moment, the flushing procedure will have to
Test connection
Test specimen
Test connection
Mass spectrometer
Turbomolecular
MS pump
Venting
Leak detector valve
Gas ballast
valve
QHe = pHe · SeffHe Roughing pump
Exhaust
Exhaust
Fig. 5.6 Basic operating principle for a leak detector Fig. 5.7 Correct set-up for a MSLD
117
Leak detection
be continued until all the oil from the pumpÕs oil pan has been recirculated differentiate between two types of calibration: with an internal or external
several times. This period of time will usually be 20 to 30 minutes. test leak. When using a test leak built into the leak detector the unit can
itself be calibrated but it can only calibrate itself. When using an external
In order to spare the user the trouble of always having to keep an eye on
test leak not just the device but also a complete configuration, such as a
the background level, what has been dubbed floating zero-point
partial flow arrangement, can be included. Internal test leaks are
suppression has been integrated into the automatic operating concepts of
permanently installed and cannot be misplaced. At present all the leak
all INFICON leak detectors (Section 5.5.2.5). Here the background level
detectors being distributed by INFICON are fitted with an automatic
measured after the inlet valve has been closed is placed in storage; when
calibration routine.
the valve is then opened again this value will automatically be deducted
from subsequent measurements. Only at a relatively high threshold level Sniffer units or configurations will as a rule have to be calibrated with
will the display panel show a warning indicating that the background noise special, external test leaks in which there is a guarantee that on the one
level is too high. Figure 5.8 is provided to illustrate the process followed in hand all the test gas issuing from the test leak reaches the tip of the probe
zero point suppression. Chart on the left. The signal is clearly larger than and on the other hand that the gas flow in the sniffer unit is not hindered by
the background. Center chart: the background has risen considerably; the calibration. When making measurements using the sniffer technique (see
signal can hardly be discerned. Chart on the right: the background is Section 5.7.2) it is also necessary to take into account the distance from the
suppressed electrically; the signal can again be clearly identified. probe tip to the surface of the specimen and the scanning speed; these
must be included as a part of the calibration. In the special case where
Independent of this floating zero-point suppression, all the leak detectors
helium concentration is being measured, calibration can be made using the
offer the capability for manual zero point shifting. Here the display for the
helium content in the air, which is a uniform 5 ppm world-wide.
leak detector at the particular moment will be Òreset to zeroÓ so that only
rises in the leak rate from that point on will be shown. This serves only to Test leaks (also known as standard leaks or reference leaks) normally
facilitate the evaluation of a display but can, of course, not influence its comprise a gas supply, a choke with a defined conductance value, and a
accuracy. valve. The configuration will be in accordance with the test leak rate
required. Figure 5.9 shows various test leaks. Permeation leaks are usually
Modern leak detectors are being more frequently equipped with oil-free
used for leak rates of 10-10 < QL < 10-7, capillaries, between 10-8 and 10-4
vacuum systems, the so-called Òdry leak detectorsÓ (UL 200 dry, UL 500
and, for very large leak rates in a range from 10 to 1000 mbar á l/s, pipe
dry). Here the problem of gas being dissolved in oil does not occur but
sections or orifice plates with exactly defined conductance values
similar purging techniques will nonetheless be employed.
(dimensions).
Test leaks used with a refrigerant charge represent a special situation since
5.5.2.3 Calibrating leak detectors; test leaks the refrigerants are liquid at room temperature. Such test leaks have a
supply space for liquid from which, through a shut-off valve, the space filled
Calibrating a leak detector is to be understood as matching the display at a only with the refrigerant vapor (saturation vapor pressure) can be reached,
leak detector unit, to which a test leak is attached, with the value shown on ahead of the capillary leak. One technological problem which is difficult to
the ÒlabelÓ or calibration certificate. The prerequisite for this is correct solve is posed by the fact that all refrigerants are also very good solvents
adjustment of the ion paths in the spectrometer, also known as tuning. for oil and grease and thus are often seriously contaminated so that it is
Often the distinction is not made quite so carefully and both procedures difficult to fill the test leaks with pure refrigerant. Decisive here is not only
together are referred to as calibration. the chemical composition but above all dissolved particles which can
In the calibration process proper the straight-line curve representing the repeatedly clog the fine capillaries.
numerically correct, linear correlation between the gas flow per unit of time
and the leak rate is defined by two points: the zero point (no display where
no emissions are detected) and the value shown with the test leak (correct
display for a known leak).
10Ð6
cautio 10Ð7
10Ð8
fine 10Ð9
prec 10Ð10
10Ð11 a b c d e
Equipment background level: < 2 á 10Ð10 1 á 10Ð8 1 á 10Ð10 (suppressed) a Reference leak without gas supply, TL4, TL6 d Permeation (diffusion) reference leak, TL8
b Reference leak for sniffer and vacuum e Refrigerant calibrated leak
Leak: 2 á 10Ð8 2 á 10Ð8 2 á 10Ð8
applications, TL4-6
Display: 2 á 10Ð8 3 á 10Ð8 2 á 10Ð8 c (Internal) capillary test leak TL7
Fig. 5.8 Example of zero-point suppression Fig. 5.9 Examples for the construction of test leaks
118
Leak detection
5.5.2.4 Leak detectors with quadrupole mass 5.5.2.5 Helium leak detectors with 180° sector
spectrometer (ECOTEC II) mass spectrometer (UL 200, UL 500)
INFICON builds leak detectors with quadrupole mass spectrometers to These units are the most sensitive and also provide the greatest degree of
register masses greater than helium. Apart from special cases, these will be certainty. Here ÒcertainÓ is intended to mean that there is no other method
refrigerants. These devices thus serve to examine the tightness of with which one can, with greater reliability and better stability, locate leaks
refrigeration units, particularly those for refrigerators and air conditioning and measure them quantitatively. For this reason helium leak detectors,
equipment. even though the purchase price is relatively high, are often far more
economical in the long run since much less time is required for the leak
Figure 4.2 shows a functional diagram for a quadrupole mass spectrometer.
detection procedure itself.
Of the four rods in the separation system, the two pairs of opposing rods
will have identical potential and excite the ions passing through along the A helium leak detector comprises basically two sub-systems in portable
center line so that they oscillate transversely. Only when the amplitude of units and three in stationary units. These are:
these oscillations remains smaller than the distance between the rods can
1. the mass spectrometer
the appropriate ion pass through the system of rods and ultimately reach
the ion trap, where it will discharge and thus be counted. The flow of 2. the high vacuum pump and
electrons thus created in the line forms the measurement signal proper. The
3. the auxiliary roughing pump system in stationary units.
other ions come into contact with one of the rods and will be neutralized
there. The mass spectrometer (see Fig. 5.11) comprises the ion source (1Ð4) and
the deflection system (5Ð9). The ion beam is extracted through the orifice
Figure 5.10 shows the vacuum schematic for an ECOTEC II. The mass
plate (5) and enters the magnetic field (8) at a certain energy level. Inside
spectrometer (4) only operates under high vacuum conditions, i.e. the
the magnetic field the ions move along circular paths whereby the radius for
pressure here must always remain below 10-4 mbar. This vacuum is
a low mass is smaller than that for higher masses. With the correct setting
generated by the turbomolecular pump (3) with the support of the
of the acceleration voltage during tuning one can achieve a situation in
diaphragm pump (1). The pressure PV between the two pumps is
which the ions describe a circular arc with a defined curvature radius.
measured with a piezo resistive measuring system (2) and this pressure
Where mass 4 (helium) is involved, they pass thorough the aperture (9) to
lies in the range between 1 to 4 mbar while in the measurement mode. This
the ion trap (13). In some devices the discharge current for the ions
pressure must not exceed a value of 10 mbar as otherwise the
impinging upon the total pressure electrodes will be measured and
turbomolecular pump will not be capable of maintaining the vacuum in the
mass spectrometer. The unit can easily be switched over at the control unit
from helium to any of various refrigerants, some of which may be selected
as desired. Naturally the unit must be calibrated separately for each of
these masses. Once set, however, the values remain available in storage
so that after calibration has been effected for all the gases (and a separate
reference leak is required for each gas!) it is possible to switch directly from 14 1
one gas to another.
5 1 Diaphragm pump 13
2 Piezo-resistive 2
external flow internal
limiter 1 particle
pressure sensor
3 Turbomolecular
12 3
particle
filter filter pump
4 Quadrupole mass 4
6
spectrometer
5 Sniffer line
11 5
6 Gas flow limiter
QMA 200 flow divider 1 7 Gas flow limiter 6
flow 8 Gas flow meter
limiter 2
4
flow divider 2
flow 10
3 7 limiter 3
flow meter
7
pv
1
8 9 8
2
1 Ion source flange 5 Extractor 11 Suppressor
1 2 Cathode 6 Ion traces for M > 4 12 Shielding of the ion trap
2 (2 cathodes, Ir + Y2O3) 7 Total pressure electrode 13 Ion trap
3 Anode 8 Ion traces for M = 4 14 Flange for ion trap with
4 Shielding of the ion 9 Intermediate orifice preamplifier
source with discharge plate
orifice 10 Magnetic field
Fig. 5.10 Vacuum schematic for the ECOTEC II Fig. 5.11 Configuration of the 180¡ sector mass spectrometer
119
Leak detection
evaluated as a total pressure signal. Ions with masses which are too small In the case of direct-flow leak detectors, an increase in the sensitivity can
or too great should not be allowed to reach the ion trap (13) at all, but some be achieved by reducing the pumping speed, for example by installing a
of these ions will do so in spite of this, either because they are deflected by throttle between the turbomolecular pump and the cold trap. This is also
collisions with neutral gas particles or because their initial energy deviates employed to achieve maximum sensitivity. To take an example:
too far from the required energy level. These ions are then sorted out by the
The smallest detectable partial pressure for helium is
suppressor (11) so that only ions exhibiting a mass of 4 (helium) can reach
pmin,He = 1 á 10-12 mbar. The pumping speed for helium would be
the ion detector (13). The electron energy at the ion source is 80 eV. It is
SHe = 10 l/s. Then the smallest detectable leak rate is
kept this low so that components with a specific mass of 4 and higher Ð
Qmin = 1 á 10-12 mbar á 10 l/s = 1 á 10-11 mbar á l/s. If the pumping speed is
such as multi-ionized carbon or quadruply ionized oxygen Ð cannot be
now reduced to 1/s, then one will achieve the smallest detectable leak rate
created. The ion sources for the mass spectrometer are simple, rugged and
of 1 á 10-12 mbar á l/s. One must keep in mind, however, that with the
easy to replace. They are heated continuously during operation and are
increase in the sensitivity the time constant for achieving a stable test gas
thus sensitive to contamination. The two selectable yttrium oxide coated
pressure in the test specimen will be correspondingly larger (see Section
iridium cathodes have a long service life. These cathodes are largely
5.5.2.9).
insensitive to air ingress, i.e. the quick-acting safety cut-out will keep them
from burning out even if air enters. However, prolonged use of the ion In Figure 5.12 the right hand diagram shows the schematic for the counter-
source may eventually lead to cathode embrittlement and can cause the flow leak detector. The mass spectrometer, the high vacuum system and
cathode to splinter if exposed to vibrations or shock. also the auxiliary roughing pump system correspond exactly to the
configuration for the direct-flow arrangement. The feed of the gas to be
Depending on the way in which the inlet is connected to the mass
examined is however connected between the roughing pump and the
spectrometer, one can differentiate between two types of MSLD.
turbomolecular pump. Helium which reaches this branch point after the
valve is opened will cause an increase in the helium pressure in the turbo-
molecular pump and in the mass spectrometer. The pumping speed Seff
5.5.2.6 Direct-flow and counter-flow leak inserted in equation 5.4b is the pumping speed for the rotary vane pump at
detectors the branch point. The partial helium pressure established there, reduced by
Figure 5.12 shows the vacuum schematic for the two leak detector types. In the helium compression factor for the turbomolecular pump, is measured at
both cases the mass spectrometer is evacuated by the high vacuum the mass spectrometer. The speed of the turbomolecular pump in the
pumping system comprising a turbomolecular pump and a rotary vane counter-flow leak detectors is regulated so that pump compression also
pump. The diagram on the left shows a direct-flow leak detector. Gas remains constant. Equation 5.5b is derived from equation 5.5a:
from the inlet port is admitted to the spectrometer via a cold trap. It is QHe = pHe á Seff á K (5.5b)
actually equivalent to a cryopump in which all the vapors and other
contaminants condense. (The cold trap in the past also provided effective Seff = effective pumping speed at the rotary vane pump at the
protection against the oil vapors of the diffusion pumps used at that time). branching point
The auxiliary roughing pump system serves to pre-evacuate the K = Helium compression factor at the turbomolecular pump
components to be tested or the connector line between the leak detector The counter-flow leak detector is a particular benefit for automatic vacuum
and the system to be tested. Once the relatively low inlet pressure units since there is a clearly measurable pressure at which the valve can be
(pumping time!) has been reached, the valve between the auxiliary pumping opened, namely the roughing vacuum pressure at the turbomolecular
system and the cold trap will be opened for the measurement. The Seff pump. Since the turbomolecular pump has a very large compression
used in equation 5.4b is the pumping speed of the turbomolecular pump at capacity for high masses, heavy molecules in comparison to the light test
the ion source location: gas, helium (M = 4), can in practice not reach the mass spectrometer. The
QHe = pHe á Seff,turbomolecular pump ion source (5.5a) turbomolecular pump thus provides ideal protection for the mass
spectrometer and thus eliminates the need for an LN2 cold tap, which is
certainly the greatest advantage for the user. Historically, counter-flow leak
detectors were developed later. This was due in part to inadequate
Solution 1: Direct-flow leak Solution 2: Counter-flow
pumping speed stability, which for a long time was not sufficient with the
detector leak detector
rotary vane pumps used here. For both types of leak detector, stationary
Test specimen Test specimen
units use a built-in auxiliary pump to assist in the evacuation of the test
Test gas stream Test gas stream port. With portable leak detectors, it may be necessary to provide a
separate, external pump, this being for weight reasons.
p TOT < 10–4 mbar
LN 2 pHe pHe
MS MS
p TOT < 10–4 mbar High vacuum pump
High vacuum pump 5.5.2.7 Partial flow operation
Auxiliary pump Roughing pump Auxiliary pump Roughing pump
Cold trap:
Where the size of the vacuum vessel or the leak makes it impossible to
2
S = 6.1 ℓ/s · cm
Fl ≈ 1000 cm
S = 6,100 ℓ/s
2
evacuate the test specimen to the necessary inlet pressure, or where this
would simply take too long, then supplementary pumps will have to be
Fig. 5.12 Full-flow and counter-flow leak detector used. In this case the helium leak detector is operated in accordance with
120
Leak detection
the so-called Òpartial flowÓ concept. This means that usually the larger part expected vis ˆ vis a diffusion pump with pumping speed of 12000 l/s, for
of the gas extracted from the test object will be removed by an additional, example Ð which leak rates can be detected at all. In systems with high
suitably dimensioned pump system, so that only a part of the gas stream vacuum- and Roots pumps, the surest option is to connect the leak detector
reaches the helium leak detector (see Fig. 5.13). The splitting of the gas between the rotary vane pump and the roots pump or between the roots
flow is effected in accordance with the pumping speed prevailing at the pump and the high vacuum pump. If the pressure there is greater than the
branching point. The following then applies: permissible inlet pressure for the leak detector, then the leak detector will
have to be connected by way of a metering (variable leak) valve. Naturally
QVacuum vessel = γ á DisplayLeak detector (5.6)
one will have to have a suitable connector flange available. It is also
where g is characterized as the partial flow ratio, i.e. that fraction of the advisable to install a valve at this point from the outset so that, when
overall leak current which is displayed at the detector. Where the partial needed, the leak detector can quickly be coupled (with the system running)
flow ratio is unknown, g can be determined with a reference leak attached and leak detection can commence immediately after opening the valve. In
at the vacuum vessel: order to avoid this valve being opened inadvertently, it should be sealed off
with a blank flange during normal vacuum system operation.
Display at the leak detector
γ = ÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑ (5.7)
QL for the reference leak A second method for coupling to larger systems, for example, those used
for removing the air from the turbines in power generating stations, is to
couple at the discharge. A sniffer unit is inserted in the system where it
5.5.2.8 Connection to vacuum systems discharges to atmosphere. One then sniffs the increase in the helium
concentration in the exhaust. Without a tight coupling to the exhaust,
The partial flow concept is usually used in making the connection of a
however, the detection limit for this application will be limited to 5 ppm, the
helium leak detector to vacuum systems with multi-stage vacuum pump
natural helium content in the air. In power plants it is sufficient to insert the
sets. When considering where to best make the connection, it must be kept
tip of the probe at an angle of about 45 ¡ from the top into the discharge
in mind that these are usually small, portable units which have only a low
line (usually pointing upward) of the (water ring) pump.
pumping speed at the connection flange (often less than 1 l/s). This makes
it all the more important to estimate Ð based on the partial flow ratio to be
V V V
ℓ S/2
S S’ S
Signal to Leak detector: 3 · 10–5 mbars · ℓ · 8 s
= 9.73 · 10–6 mbar · ℓ
s MS MS MS
(8 + 16.66) ℓs
}
ℓ Q Throttle
Signal to partial flow pump: 3 · 10 –5 mbar · ℓ
· 16,668s ℓ = 2.02 · 10 –5 mbar · ℓ Signal S
LD LD LD
s (8 + 16.66) s
s amplitude
Faster, less sensitive normal Slower, more sensitive
Check: Overall signal QHe = QLD + QPFP = 3.00 · 10–5 mbars · ℓ Q = 2p 100%
S
2,0
/2
95%
Partial flow ratio = Fraction of the overall flow to the leak detector 3
Q QLD 1
γ = LD =
or γ=
SLD
=
QHe QLD + QPFP 1 + nnn
= 1
Q
Q
S
PFP H
QLD = γ · QHe
LD
1
Signal rise
Fig. 5.13 Partial flow principle Fig. 5.14 Signal responses and pumping speed
121
Leak detection
1. Center: The specimen with volume of V is joined directly with the leak either due to one large leak or several smaller leaks Ð more gas flows into
detector LD (effective pumping speed of S). the unit than the maximum permissible throughput rate for the leak detector.
122
Leak detection
ppm share of helium in the air is sufficient for detection purposes. The leak determined (operating period) the change in concentration inside the
rate is then: envelope will be measured with a sniffer connected to the helium detection
Display (pure He) Display (atmosph. He) unit. The overall leak rate (integral leak rate) can be calculated following
ÑÑÑÑÑÑÑÑÐ = ÑÑÑÑÑÑÑÑÑÑÐ calibration of the test configuration with a reference concentration, e.g.
1 5 á 10-6
atmospheric air. This method makes it possible to detect even the smallest
QL = Display (pure He) (5.11) overall leakiness and is suitable in particular for automated industrial leak
= 2 á 10+5 á Display (atmospheric He) testing. Due to gas accumulation, the limits for normal sniffer techniques
are shifted toward lower leak rates and the ambient conditions such as
temperature, air flow and sniffer tracing speed lose influence. When using
5.7.2 Sniffer technology plastic envelopes it is necessary to take into account helium permeation
(local leak test using the positive through the plastic envelope during long enrichment periods.
pressure method)
b) Direct measurement of the leak rate with the leak detector
Here the points suspected of leaking at the pressurized test specimen (see (rigid envelope)
Fig. 5.4, d) are carefully traced with a test gas probe which is connected
with the leak detector by way of a hose. Either helium or hydrogen can be When the test specimen, pressurized with helium, is placed in a rigid
detected with the INFICON helium leak detectors. The sensitivity of the vacuum chamber, connected to a helium leak detector, the integral leak rate
method and the accuracy of locating leaky points will depend on the nature can be read directly at the leak detector.
of the sniffer used and the response time for the leak detector to which it is
connected. In addition, it will depend on the speed at which the probe is
passed by the leak points and the distance between the tip of the probe 5.7.3.2 Envelope test with test specimen
and the surface of the test specimen. The many parameters which play a evacuated
part here make it more difficult to determine the leak rates quantitatively.
a) Envelope = Òplastic tentÓ
Using sniffer processes it is possible, virtually independent of the type of
gas, to detect leak rates of about 10-7 mbar á l/s. The limitation of sensitivity The evacuated test specimen is surrounded by a light-weight (plastic)
in the detection of helium is due primarily to the helium in the atmosphere enclosure and this is then filled with helium once the atmospheric air has
(see Chapter 9, Table VIII). In regard to quantitative measurements, the been removed. When using a plastic bag as the envelope, the bag should
leak detector and sniffer unit will have to be calibrated together. Here the be pressed against the test specimen before filling it with helium in order to
distance from the specimen and the tracing speed will have to be included expel as much air as possible and to make the measurement with the
in calibration, too. purest helium charge possible. The entire outside surface of the test object
is in contact with the test gas. If test gas passes through leaks and into the
test specimen, then the integral leak rate will be indicated, regardless of the
5.7.3 Vacuum envelope test number of leaks. In addition, it is necessary to observe when repeating
(integral leak test) testing in enclosed areas that the helium content of the room will rise quite
rapidly when the envelope is removed. Using plastic bags is thus more
Vacuum envelope tests are integral leak tests using helium as the test gas, advisable for Òone-offÓ testing of large plants. The plastic envelope used
in which the test specimen is enclosed either in a rigid (usually metal) here is often referred to as a ÒtentÓ.
enclosure or in a light plastic envelope. The helium which enters or leaves
(depending on the nature of the test) the test specimen is passed to a
b) Rigid envelope
helium leak detector, where it is measured. Envelope tests are made either
with the test specimen pressurized with helium (Fig. 5.4c) or with the test The use of a solid vacuum vessel as the rigid envelope, on the other hand,
specimen evacuated (Fig. 5.4a). In both cases it may be necessary to is better for repetitive testing where an integral test is to be made. When
convert the helium enrichment figure (accumulation) to the helium standard solid envelopes are used it is also possible to recover the helium once the
leak rate. test has been completed.
123
Leak detection
The advantages of the helium test method, seen from the industrial point of
view, may be summarized as follows:
• The leak rates which can be detected with this process go far beyond all
practical requirements.
• The integral leak test, i.e. the total leak rate for all individual leaks,
facilitates the detection of microscopic and sponge-like distributed leaks
which altogether result in leakage losses similar to those for a larger
individual leak.
124
Thin film controllers/control units
6 Thin film controllers The selection of the ÒrightÓ crystal holder thus plays an important role in all
measurements with quartz oscillators. Various crystal holder designs are
and control units recommended for the different applications: with or without shutter,
bakeable for UHV, double crystal holder or crystal six as well as special
with quartz versions for sputter applications. In addition to these important and more
ÒmechanicalÓ aspects, the advances in measuring and control technology
oscillators and equipment features will be discussed in the following.
6.1 Introduction
It took a long time to go from the coating of quartz crystals for frequency
6.2 Basic principles of coating
fine tuning, which has long been in practice, to utilization of frequency thickness measurement with
change to determine the mass per unit area as a microbalance with the quartz oscillators
present-day degree of precision. In 1880 two brothers, J. and P. Curie, The quartz oscillator coating thickness gauge (thin film controller) utilizes
discovered the piezoelectric effect. Under mechanical loads on certain the piezoelectric sensitivity of a quartz oscillator (monitor crystal) to the
quartz crystal surfaces, electrical charges occur that are caused by the supplied mass. This property is utilized to monitor the coating rate and final
asymmetrical crystalline structure of SiO2. Conversely, in a piezocrystal thickness during vacuum coating.
deformations appear in an electrical field and mechanical oscillations occur
in an alternating field. A distinction is made between bending oscillations, A very sharp electromechanical resonance occurs at certain discrete
thickness shear mode and thickness shear oscillations. Depending on the frequencies of the voltage applied. If mass is added to the surface of the
orientation of the cut plane to the crystal lattice, a number of different cuts quartz crystal oscillating in resonance, this resonance frequency is
are distinguished, of which only the so-called AT cut with a cut angle of diminished. This frequency shift is very reproducible and is now understood
35¡10" is used in thin film controllers because the frequency has a very low precisely for various oscillation modes of quartz. Today this phenomenon,
temperature dependence in the range between 0 and 50 ¡C with this cut. which is easy to understand in heuristic terms, is an indispensable
Accordingly, an attempt must be made not to exceed this temperature measuring and process control tool, with which a coating increase of less
range during coating (water cooling of crystal holder). than one atomic layer can be detected.
Since there is still a problem with Òquartz capacityÓ (i.e. the maximum In the late 1950s Sauerbrey and Lostis discovered that the frequency shift
possible coating thickness of the quartz at which it still oscillates reliably) connected with the coating of the quartz crystal is a function of the change
despite refined technology, a number of approaches have been developed in mass due to the coating material in the following way:
to expand this capacity: Mf ∆F ∆F
= or Mf = Mq · with (6.1)
1. The use of several crystals, one behind the other, in a multiple crystal Mq Fq Fq
holder with automatic change and data updating in the event of
imminent failure of a quartz: CrystalSix. Mf mass of the coating
Mq mass of the quartz prior to coating
2. The RateWatcher function, in which the quartz is alternately exposed to Fq frequency prior to coating
the coating beam for a short time until all measurements and regulation Fc frequency after coating
have been carried out and then remains covered by a shutter for a ∆F = Ff Ð Fc ... frequency shift due to coating
longer period of time.
If the following are now applied: Mf = (Mc Ð Mq) = Df á ρf á A and
Mq = Dq á ρq á A, where T = the coating thickness, ρ = density and A stands
for area while the index q stands for the state of the Òuncoated quartzÓ and
c for the state after Òfrequency shift due to coatingÓ, the following results are
obtained for the coating thickness:
rel. frequency change (ppm)
Fq ∆F ∆F
Df = · Dq · ρ q · =K·
Fq Fq · ρ f ρf with
Dq · Fq · ρq NAT · ρq
K= =
2 2 where
Fq Fq
125
Thin film controllers/control units
E
↔
Node
Fig. 6.2 Thickness shear oscillations Fig. 6.3 Shape of LEYBOLD-Inficon quartz crystals
density ρf of the coating material. The equation oscillation, which is called the fundamental wave. The characteristic
motions of the thickness shear oscillation are parallel to the main crystal
∆F
Df = K ·
ρf boundary surfaces. In other words: the surfaces are shift antinodes, see
Fig. 6.2. The resonance frequencies slightly above the basic frequency are
called ÒanharmonicÓ and are a combination of thickness shear and
for the coating thickness was used in the first coating thickness measuring
thickness rotation oscillation forms. The resonance frequency at around
units with Òfrequency measurementÓ ever used. According to this equation,
three times the value for the fundamental wave is called Òquasi-harmonicÓ.
a crystal with a starting frequency of 6.0 MHz displays a decline in
Near the quasi-harmonic there are also a number of anharmonics with a
frequency of 2.27 Hz after coating with 1• of aluminum (de = 2.77 g/cm3).
slightly higher frequency.
In this way the growth of a fixed coating due to evaporation or sputtering
can be monitored through precise measurement of the frequency shift of The design of the monitor crystals used nowadays (see Fig. 6.3) displays a
the crystal. It was only when knowledge of the quantitative interrelationship number of significant improvements over the original square crystals. The
of this effect was acquired that it became possible to determine precisely first improvement was the use of round crystals. The enlarged symmetry
the quantity of material that is deposited on a substrate in a vacuum. greatly reduced the number of possible oscillation modes. A second group
Previously this had been practically impossible. of improvements involved providing one of the surfaces with a contour and
making the excitation electrode smaller. The two together ensure that the
acoustic energy is recorded. Reducing the electrode diameter limits the
excitation to the middle area. The surface contour consumes the energy of
6.3 The shape of quartz oscillator the moving acoustic waves before they reach the crystal edge. It is not
crystals reflected into the center where it could interfere with new incoming waves.
Regardless of how sophisticated the electronic environment is, the main Such a small crystal behaves like an infinitely expanded crystal. However, if
component for coating measurement remains the monitor quartz crystal. the crystal vibrations remain restricted to the center, one can clamp the
Originally monitor quartzes had a square shape. Fig. 6.4 shows the outer edge to a crystal holder, without engendering undesired side effects.
resonance spectrum of a quartz resonator with the design used today (Fig. Moreover, contouring reduces the resonance intensity of undesired
6.3). The lowest resonance frequency is initially given by a thickness shear anharmonics. This limits the capacity of the resonator to maintain these
oscillations considerably.
Fig. 6.4 shows the frequency behavior of a quartz crystal shaped as in Fig.
6.3. The ordinate represents the amplitude of the oscillation or also the
current flowing through the crystal as a function of the frequency on the
abscissa.
126
Thin film controllers/control units
Since one cannot distinguish between measurements on the order of magnitude of the frequency measurement
accuracy, good rate regulation becomes impossible (rate regulation:
• coating: frequency reduction = negative influence
regulation of the energy supply to the coating source so that a specified
• temperature change: coating thickness growth per time unit is maintained). The great
negative or positive influence measurement uncertainty then causes more noise in the closed loop, which
can only be countered with longer time constants. This in turn makes the
• temperature gradients on the crystal, positive or negative
corrections due to system deviation slow so that relatively long deviations
• stresses caused by the coating from the desired rate result. This may not be important for simple coatings,
but for critical coatings, as in the case of optical filters or very thin, slowly
it is important to minimize the temperature influence. This is the only way to
growing single-crystal coatings, errors may result. In many cases, the
measure small differences in mass.
desired properties of such coatings are lost if the rate deviations are more
than one or two percent. Finally, frequency and stability of the reference
oscillator determine the precision of the measurement.
6.4 Period measurement
Although the instruments that functioned according to equation 6.2 were
very useful, it soon became obvious that for the desired accuracy their area
of application was typically limited to ÆF < 0.02 Fq. Even at a relative 6.5 The Z match technique
frequency change of (Fq Ð Fc) / Fq < 2 %, errors of around 2 % occurred in
Miller and Bolef (1968) treated the quartz oscillator and coating system as a
the coating thickness measurement so that the "usable service life" of the
single-dimensional, coherent acoustic resonator. Lu and Lewis (1972)
coating in the case of a 6-MHz monitor crystal was about 120 kHz.
developed the simplified Z match equation on that basis. Simultaneous
In 1961 Behrndt discovered that: advances in electronics, particularly the microprocessor, made it possible to
solve the Z match equation in real time. Most coating process control units
Mf (Tc − Tq) ∆F
= = with (6.3) sold today use this sophisticated equation, which takes into account the
Mq Tq Fc
acoustic properties of the quartz oscillator/coating system:
127
Thin film controllers/control units
output phase
amplifier
| impedance |
phase (degrees)
log .Z. (Ohm)
series resonance
Frequency (MHz)
Fig. 6.5 Circuit of the active oscillator Fig. 6.6 Crystal frequencies near the series resonance point
Normally an oscillator circuit is designed such that the crystal requires a suddenly significantly smaller, i.e. by the amount of the frequency difference
phase shift of 0 degrees to permit work at the series resonance point. Long- between the fundamental wave and the anharmonic adopted by the
and short-term frequency stability are properties of crystal oscillators oscillation.
because very small frequency differences are needed to maintain the phase
shift necessary for the oscillation. The frequency stability is ensured through
the quartz crystal, even if there are long-term shifts in the electrical values
that are caused by Òphase jitterÓ due to temperature, ageing or short-term 6.7 The mode-lock oscillator
noise. If mass is added to the crystal, its electrical properties change.
INFICON has developed a new technology for overcoming these
Fig. 6.7 shows the same graph as Fig 6.6, but for a thickly coated crystal. It constraints on the active oscillator. The new system constantly analyzes the
has lost the steep slope displayed in Fig. 6.6. Because the phase rise is response of the crystal to an applied frequency: not only to determine the
less steep, any noise in the oscillator circuit leads to a larger frequency shift (series) resonance frequency, but also to ensure that the quartz oscillates in
than would be the case with a new crystal. In extreme cases, the original the desired mode. The new system is insensitive to mode hopping and the
phase/frequency curve shape is not retained; the crystal is not able to carry resultant inaccuracy. It is fast and precise. The crystal frequency is
out a full 90 ¡ phase shift. determined 10 times a second with an accuracy to less than 0.0005 Hz.
The impedance |Z| can increase to very high values. If this happens, the The ability of the system to initially identify and then measure a certain
oscillator prefers to oscillate in resonance with an anharmonic frequency. mode opens up new opportunities thanks to the advantages of the
Sometimes this condition is met for only a short time and the oscillator additional information content of these modes. This new, "intelligent"
oscillation jumps back and forth between a basic and an anharmonic measuring device makes use of the phase/frequency properties of the
oscillation or it remains as an anharmonic oscillation. This phenomenon is quartz crystal to determine the resonance frequency. It works by applying a
well known as "mode hopping". In addition to the noise of the rate signal synthesized sinus wave of a certain frequency to the crystal and measuring
created, this may also lead to incorrect termination of a coating because of the phase difference between the applied signal voltage and the current
the phase jump. It is important here that, nevertheless, the controller flowing through the crystal. In the case of series resonance, this difference
frequently continues to work under these conditions. Whether this has is exactly zero degrees; then the crystal behaves like an ohmic resistance.
occurred can only be ascertained by noting that the coating thickness is By disconnecting the applied voltage and the current that returns from the
crystal, one can determine with a phase comparator whether the applied
frequency is higher or lower than the crystal resonance point.
sweep is carried out until the phase comparator changes over and thus
log .Z. (Ohm)
marks the resonance. For AT quartzes we know that the lowest usable
frequency is the fundamental wave. The anharmonics are slightly above
that. This information is not only important for the beginning, but also in the
rare case that the instrument loses ÒtrackÓ of the fundamental wave. Once
the frequency spectrum of the crystal is determined, the instrument must
track the shift in resonance frequency, constantly carry out frequency
Frequency (MHz)
measurements and then convert them into thickness.
128
Thin film controllers/control units
advantages over the earlier generation of active oscillators, primarily of the anharmonic in relation to the fundamental oscillation.
insensitivity to mode hopping as well as speed and accuracy of
If one side of the quartz is coated with material, the spectrum of the
measurement. This technique also enables the introduction of sophisticated
resonances is shifted to lower frequencies. It has been observed that the
properties which were not even conceivable with an active oscillator setup.
three above mentioned modes have a somewhat differing mass sensitivity
The same device that permits the new technology to identify the
and thus experience somewhat different frequency shifts. This difference is
fundamental wave with one sweep can also be used to identify other
utilized to determine the Z value of the material. By using the equations for
oscillation modes, such as the anharmonics or quasi-harmonics. The unit
the individual modes and observing the frequencies for the (100) and the
not only has a device for constantly tracking the fundamental wave, but can
(102) mode, one can calculate the ratio of the two elastic constants C60 and
also be employed to jump back and forth between two or more modes. This
C55. These two elastic constants are based on the shear motion. The key
query of different modes can take place for two modes with 10 Hz on the
element in WajidÕs theory is the following equation:
same crystal.
(C55 / C66 )coated 1
≈ (6.5)
(C55 / C66 )uncoated (1 + M ⋅ Z )
129
Thin film controllers/control units
6.9 Coating thickness regulation Due to the simplicity with which the experimental data can be obtained, we
preferred the open loop method. Moreover, application of this technique
The last point to be treated here is the theory of the closed loop for coating permits extensive elimination of the trial and error method.
thickness measuring units to effect coating growth at a controlled (constant)
growth rate. The measuring advantages of the instruments, such as speed, The Auto Control Tune function developed by INFICON characterizes a
precision and reliability, would not be completely exploited if this information process on the basis of its step responses. After a step-by-step change in
were not inputted into an improved process monitoring system. For a the power the resulting changes in the rate as a function of time are
coating process this means the coating rate should be kept as close and smoothed and stored. The important step responses are determined, see
stable as possible to a setpoint. The purpose of the closed loop is to make Fig. 6.8.
use of the information flow of the measuring system in order to regulate the In general, it is not possible to characterize all processes exactly, so several
capacity for a special evaporation source in an appropriately adapted way. approximations have to be made. Normally one assumes that the dynamic
When the system functions correctly, the controller translates small characteristic can be reproduced by a process of the first order plus dead
deviations of the controlled parameter (the rate) from the setpoint into time. The Laplace transformation for this assumption (transfer to the s
correction values of the re-adjusted evaporation capacity parameter. The plane) is approximated:
ability of the controller to measure quickly and precisely keeps the process
−L
from deviating significantly from the setpoint.
Output K p ⋅ 10 s
= with(6.8)
The most widespread type of controller is the PID controller. Here P stands Input τ ⋅ s +1
for proportional, I for integral and D for differential control function. In the
following some of the properties of this controller are described in detail. Kp = amplification in stationary state
Information on the system behavior is gained through a step response to a L = dead time
control fault in certain controller settings. τ = time constant
This response is recorded, and then improved control parameters for a new These three parameters are determined through the response curve of the
test are estimated. This procedure is continued until a satisfactory result is process. An attempt has been made by means of several methods to
achieved. At the end the controller is optimized so that its parameters calculate the required parameters of the system response from curves, as
exactly match the characteristics of the evaporator source. shown in Fig. 6.8. This results in a 1-point accordance at 63.2 % of the
It is a long and frustrating process to adjust a controller to an evaporation transition (a time constant), an exponential accordance at two points and an
source, requiring several minutes for stabilization and hours to obtain exponential accordance weighted according to the method of the smallest
satisfactory results. Often the parameters selected for a certain rate are not squares. A process is sufficiently characterized by this information so that
suitable for an altered rate. Thus, a controller should ideally adjust itself, as the controller algorithm can be applied. Equation 6.9 shows the Laplace
the new controllers in INFICON coating measuring units do. At the transformation for the very often used PID controller:
beginning of installation and connection the user has the unit measure the S
characteristics of the evaporation source. Either a PID controller is used as M(s) = Kc · 1 + + Td · S · E (s) (6.9)
Ti
the basis for slow sources or another type of controller for fast sources
without significant dead time. with
In relevant literature a distinction is made between three different ways of M(s) = controlled variable or power
setting controllers. Depending on which data are used for the setting, a Kc = Control amplification (the proportional term)
distinction is made between the closed loop, open loop and resonance Ti = integration time
response method. Td = differentiation time
E(s) = process deviation
Fig. 6.9 shows the control algorithm and a process with a phase shift of the
1.00 K p first order and a dead time. The dynamics of the measuring device and the
control elements (in our case the evaporator and the power supply) are
0.0632 K p
point of
maximum
rise
[process] [controller]
T1 = t(0.632) – L
Kp = (change in output signal)/(change in control signal)
Fig. 6.8 Process response to a step change with t = 0 (open loop, control signal amplified) Fig. 6.9 Block diagram of the PID controller
130
Thin film controllers/control units
implicitly contained in the process block. R(s) represents the rate setpoint. .
– 0947
. L
136
The return mechanism is the deviation created between the measured Kc = ⋅ (6.13)
precipitation rate C(s) and the rate setpoint R(s). p T1
K
The key to use of any control system is to select the correct values for Kc, 0.738
119
. L
Td and Ti. The Òoptimum controlÓ is a somewhat subjective term that is Ti = ⋅ (6.14)
T1 T1
made clear by the presence of different mathematical definitions:
0995
.
Usually the smallest square error ISE (Integral Square Error) is used as a L
measure of the quality of the control: Td = (0.381⋅ T1) ⋅ (6.15)
T1
ISE = ∫ e2(t) ⋅ dt (6.10)
For slow systems the time interval between the forced changes in control
Here e is the error (the deviation): e = rate setpoint minus measured rate. voltage is extended to avoid ÒhangingÓ the controller (hanging = rapid
ISE is relatively insensitive to small deviations, but large deviations growth of the control signal without the system being able to respond to the
contribute substantially to the value of the integral. The result is small altered signal). This makes a response to the previous change in the
ÒovershootsÓ, but long ripple times because deviations occurring late controller setting and ÒpowerfulÓ controller settings possible. Another
contribute little to the integral. advantage is the greater insensitivity to process noise because the data
used for control do not come from merely one measurement, but from
The integral of the absolute value of the deviation IAE (Integral Absolute several, so that the mass-integrating nature of the quartz crystal is utilized.
Error) was also proposed as a measure for control quality:
In processes with short response times (short time constants) and small to
IAE = ∫ e(t) ⋅ dt (6.11) unmeasurable dead times, the PID controller often has difficulties with the
noise of the coating process (beam deflection, rapid thermal short-circuits
between melt and evaporator, etc.). In these cases a control algorithm of
This is more sensitive for small deviations, but less sensitive for large
the integral reset type is used with success. This controller always
deviations than ISE.
integrates the deviation and presses the system towards zero deviation.
Graham and Lanthrop introduced the integral over time, multiplied by the This technique works well with small or completely imperceptible dead
absolute error ITAE (Integral Time Absolute Error), as a measure for control times. However, if it is used with a noticeable phase shift or dead time, the
quality: controller tends to generate oscillations because it overcompensates the
controller signal before the system has a chance to respond. Auto Control
ITAE = ∫ t ⋅ e(t) ⋅ dt (6.12) Tune recognizes the properties of these fast systems during the
measurement of a step response and utilizes the information to calculate
The ITAE is sensitive to initial and, to a certain extent, unavoidable the control amplification for a non-PID control algorithm.
deviations. Optimum control responses defined through ITAE consequently
have short response times and larger ÒovershootsÓ than in the case of the
other two criteria. However, ITAE has proven to be very useful for
evaluating the regulation of coating processes. 6.10 INFICON instrument variants
INFICONÕs Auto Control Tune is based on measurements of the system The instrument models available differ both in hardware and software
response with an open loop. The characteristic of the system response is equipment: the simplest unit, the XTM/2, is purely a measuring or display
calculated on the basis of a step change in the control signal. It is device that cannot control vacuum coating.
determined experimentally through two kinds of curve accordance at two The XTC/2 and XTC/C group can control vacuum coating sources and up
points. This can be done either quickly with a random rate or more precisely to three different coatings of a process (not to be confused with nine
with a rate close to the desired setpoint. Since the process response different coating programs). In the case of XTM/2, XTC/2 and XTC/C units,
depends on the position of the system (in our case the coating growth rate), the AutoZero and AutoTune functions are not available, and measurement
it is best measured near the desired work point. The process information with several sensors simultaneously as well as simultaneous control of two
measured in this way (process amplification Kp, time constant T1 and dead vacuum coating sources are not possible.
time L) are used to generate the most appropriate PID control parameters.
However, the IC/5 offers all comfort functions available today: measurement
The best results in evaluating coating control units are achieved with ITAE. with up to eight sensors with AutoZero and AutoTune as well as capability
There are overshoots, but the reaction is fast and the ripple time short. of simultaneous control of two evaporator sources. Moreover, it offers 24
Controller setting conditions have been worked up for all integral evaluation material programs, with which 250 coatings in 50 processes can be
criteria just mentioned so as to minimize the related deviations. With a programmed. To simplify operation and avoid errors, the unit also has a
manual input as well as with experimental determination of the process diskette drive. All types of crystal holders can be connected here. The
response coefficients, the ideal PID coefficients for the ITAE evaluation can thickness resolution is around 1 •, the rate resolution for rates between 0
easily be calculated from equations 6.13, 6.14 and 6.15: and 99.9 •/s around 0.1 •/s and for rates between 100 and 999 •/s around
1 •/s. A particularly attractive option offered by the IC/5 is a microbalance
131
Thin film controllers/control units
board with a highly stable reference quartz. This oscillator is 50 times more
stable than the standard oscillator; long-term stability and accuracy are
then 2 ppm over the entire temperature range. This option is specially
designed for coatings of material with low density and at low coating rates.
This is important for space contamination and sorption studies, for
example.
132
Applications of vacuum technology
7. Application of addition to metal and alloy coatings, layers may be produced from various
chemical compounds or layers of different materials applied in sandwich
vacuum technology form. A significant advantage of vacuum coating over other methods is that
many special coating properties desired, such as structure, hardness,
for coating electrical conductivity or refractive index, are obtained merely by selecting a
specific coating method and the process paramaters for a certain coating
techniques material.
Annealing of metals
Degassing of melts
Evaporation
Sputtering of metals
Drying of plastics
–10 –7 –3 0 3
10 10 10 10 10
Pressure [mbar]
133
Applications of vacuum technology
6
Hairpin-sheped evaporator 5
made of twisted tungsten wire 7
4
Evaporator made of electrically conductive
ceramics
3 8
134
Coating methods
7.3 Vacuum coating technology/ 7.5. The system consists of four separate stations made up of a drum
coating systems rotating around the vertical axis with four substrate chambers and process
stations mounted in the vacuum chamber. During rotation, a substrate
chamber moves from the loading and unloading station to the pretreatment
7.3.1 Coating of parts station, to the metallization station, to the protective coating station and
For molded-plastic parts, vacuum coating techniques are increasingly then back to the initial position. Since each station has its own pumping
replacing conventional coating methods, such as electroplating. For system, all four processes can run simultaneously with entirely independent
example, using vacuum coating methods, automobile reflectors obtain a adjustable process parameters. The vacuum system comprises of
mirror-like surface, plastic articles in the furniture, decoration, clock and turbomolecular pumps and backing pump sets consisting of Roots and
watch as well as electronics industry are metal-coated and optical effects rotary vane pumps.
are created on articles in the decoration industry.
Fig. 7.4 shows a type of vacuum system in which large batches of molded-
7.3.2 Web coating
plastic parts can be coated simultaneously. The substrates are placed on a
cage that rotates past the coating source, a sputter cathode in this Metal-coated plastic webs and papers play an important role in food
example. In some applications, by using a glow discharge treatment, the packaging. They preserve food longer according to storage and transport
substrates are cleaned and the surface is activated prior to the coating logistics requirements and give packaging an attractive appearence.
process. This enhances the adhesive strength and reproducibility of the Another important area of application of metal-coated web is the production
coating properties. A corrosion protection coating can be applied after of film capacitors for electrical and electronics applications. Metal-coating is
sputtering. In this case, a monomer vapor is admitted into the system and a carried out in vacuum web coating systems. Fig. 7.6 shows a typical
high-frequency plasma discharge ignited. The monomer is actived in the scheme. The unit consists of two chambers, the winding chamber with the
plasma and deposits on the substrates as a polymer coating. In this type of roll of web to be coated and the winding system, as well as the coating
system there may be plastic substrates with a surface area of several chamber, where the evaporators are located. The two chambers are sealed
10 m2 on the cage, causing a correspondingly high desorption gas flow. from each other, except for two slits through which the web runs. This
The vacuum system must be able to attain the required pressures reliably makes it possible to pump high gas loads from the web roll using a
despite these high gas loads. In the example shown, the system is relatively small pumping set. The pressure in the winding chamber may be
evacuated with a combination of a backing and Roots pump. A diffusion more than a factor of 100 higher than the pressure simultaneously
pump along with a cold surface forms the high vacuum pump system. The established in the coating chamber. The pump set for the winding chamber
cold surfaces pump a large portion of the vapor and volatile substances usually consists of a combination of Roots and rotary vane pumps.
emitted by the plastic parts while the diffusion pump basically removes the
With strongly degassing rolls of paper, it may be necessary to install a cold
non-condensable gases as well as the noble gas required for the sputter
surface in the winding chamber to act as a water vapor pump. The rolls of
process.
the plastic web or paper typically have diameters between 400 and 1000
A completely different concept for the same process steps is shown in Fig. mm and a width of 400 to 3000 mm. A precise, electronically controlled
Fig. 7.4 Diagramm of a batch system for coating parts Fig. 7.5 Multi-chamber parts-coating unit (rotationally symmetric in-line system DynaMet 4V)
135
Applications of vacuum technology
High-perfor-
mance
plasma
source
Electron
beam
evaporator
Monomer O2
1 Unwinder 4 Drawing roller
2 Coating source 5 Take-up reel
3 Coating roller Ar
Fig. 7.6 Schematic diagram of a vacuum web coating system Fig. 7.7 Coating unit for optical coating systems
winding system is required for winding and unwinding as well as web different materials. The substrates are mounted on a rotating calotte above
guidance. the evaporators. Application of suitable shieldings combined with relative
movement between evaporators and substrates, results in a very high
During the coating process the web, at a speed of more than 10 m/s,
degree of coating uniformity. With the help of quartz coating thickness
passes a group of evaporators consisting of ceramic boats, from which
monitors (see Section 6) and direct measurement of the attained optical
aluminium is evaporated. To achieve the necessary Al-coating thickness at
properties of the coating system during coating, the coating process is fully
these high web speeds, very high evaporation rates are required. The
controlled automatically.
evaporators must be run at temperatures in excess of 1400 ¡C. The
thermal radiation of the evaporators, together with the heat of condensation One of the key requirements of coatings is that they retain their properties
of the growing layer, yields a considerable thermal load for the web. With under usual ambient conditions over long periods of time. This requires to
the help of cooled rollers, the foil is cooled during and after coating so that produce the densest coatings possible, into which neither oxygen nor water
it is not damaged during coating and has cooled down sufficiently prior to can penetrate. Using glass lenses, this is achieved by keeping the
winding. substrates at temperatures up to 300 ¡C during coating by means of
radiation heaters. However, plastic lenses, as those used in eyeglass
During the entire coating process the coating thickness is continuously
optics, are not allowed to be heated above 80 ¡C. To obtain dense, stable
monitored with an optical measuring system or by means of electrical
coatings these substrates are bombarded with Ar ions from an ion source
resistance measurement devices. The measured values are compared with
during coating. Through the ion bombardement the right amount of energy
the coating thickness setpoints in the system and the evaporator power is
is applied to the growing layer so that the coated particles are arranged on
thus automatically controlled.
the energetically most favorable lattice sites, without the substrate
temperature reaching unacceptably high values. At the same time oxygen
can be added to the argon. The resulting oxygen ions are very reactive and
7.3.3 Optical coatings ensure that the oxygen is included in the growing layer as desired.
Vacuum coatings have a broad range of applications in production of
The vacuum system of such a coating unit usually consists of a backing
ophthalmic optics, lenses for cameras and other optical instruments as well
pump set comprising a rotary vane pump and Roots pump as well as a high
as a wide variety of optical filters and special mirrors. To obtain the desired
vacuum pumping system. Depending on the requirements, diffusion pumps,
transmission or reflection properties, at least three, but sometimes up to 50
cryo pumps or turbomolecular pumps are used here, in most cases in
coatings are applied to the glass or plastic substrates. The coating
connection with large refrigerator-cooled cold surfaces. The pumps must be
properties, such as thickness and refractive index of the individual coatings,
installed and protected by shieldings in a way that no coating material can
must be controlled very precisely and matched to each other. Most of these
enter the pumps and the heaters in the system do not thermally overload
coatings are produced using electron beam evaporators in single-chamber
them. Since shielding always reduces the effective pumping speed, the
units (Fig. 7.7). The evaporators are installed at the bottom of the chamber,
system manufacturer must find a suitable compromise between shielding
usually with automatically operated crucibles, in which there are several
effect and reduction of pumping speed.
136
Coating methods
7.3.4 Glass coating All major functions of a plant, such as glass transport, control of the sputter
processes and pump control, are carried out fully automatically. This is the
Coated glass plays a major role in a number of applications: window panes only way to ensure high productivity along with high product quality.
in moderate and cold climate zones are provided with heat-reflecting
coating systems to lower heating costs; in countries with high intensity solar
radiation, solar protection coatings are used that reduce air conditioning
costs; coated car windows reduce the heating-up of the interior and mirrors
7.3.5 Systems for producing data storage
are used both in the furniture and the automobile industry. Most of these disks
coatings are produced in large in-line vacuum systems. Fig. 7.8 shows a Coatings for magnetic- or magneto-optic data storage media usually consist
typical system. The individual glass panes are transported into a entrance of several functional coatings that are applied to mechanically finished
chamber at atmospheric pressure. After the entrance valve is closed, the disks. If several plates are placed on one common carrier, the coating
chamber is evacuated with a forepump set. As soon as the pressure is low processes can be carried out in a system using a similar principle to that
enough, the valve to the evacuated transfer chamber can be opened. The used for glass coating. However, most disks must be coated on both sides
glass pane is moved into the transfer chamber and from there at constant and there are substantially greater low particle contamination requirements
speed to the process chambers, where coating is carried out by means of as compared to glass coating. Therefore, in-line systems for data memories
sputter cathodes. On the exit side there is, in analogy to the entrance side, use a vertical carrier that runs through the system (Fig. 7.10). The sputter
a transfer chamber in which the pane is parked until it can be transferred cathodes in the process stations are mounted on both sides of the carrier
out through the exit chamber. so that the front and back side of the disk can be coated simultaneously.
Most of the coatings consist of a stack of alternative layers of metal and An entirely different concept is applied for coating of single disks. In this
oxide. Since the metal layers may not be contaminated with oxygen, the case the different process stations are arranged in a circle in a vacuum
individual process stations have to be vacuum-isolated from each other and chamber (Fig. 7.11). The disks are transferred individually from a magazine
from the transfer stations. Utilization of valves for separating process to a star-shaped transport arm. The transport arm cycles one station further
chambers is unsatisfactory because it increases plant dimensions. To avoid after each process step and in this way transports the substrates from one
frequent and undesirable starting and stopping of the glass panes, the process station to the next. During cycling all processes are switched off
process chambers are vacuum-separated through so-called Òslit locksÓ, i.e. and the stations are vacuum-linked to each other. As soon as the arm has
constantly open slits combined with an intermediate chamber with its own reached the process position, the individual stations are seperated from
vacuum pump (Fig. 7.9). The gaps in the slits are kept as small as each other by closing seals. Each station is pumped by means of its own
technically possible to minimize clearance and therefore conductance as turbomolecular pump and the individual processes are started. As many
the glass panes are transported through them. The pumping speed at the process stations as there are in the system as many processes can be
intermediate chamber is kept as high as possible in order to achieve a performed in parallel. By sealing off the process stations, excellent vacuum
considerably lower pressure in the intermediate chamber than in the pro- separation of the individual processes can be achieved. However, since the
cess chambers. This lower pressure greatly reduces the gas flow from a slowest process step determines the cycle interval, two process stations
process chamber via the intermediate chamber to the adjacent process may have to be dedicated for particularly timeconsuming processes.
chamber. For very stringent separation requirements it may be necessary to
place several intermediate chambers between two process chambers.
The glass coating process requires high gas flows for the sputter processes
as well as low hydrocarbon concentration. The only vacuum pump which
satisfies these requirements as well as high pumping speed stability over
time are turbo-molecular pumps which are used almost exclusively.
While the transfer and process chambers are constantly evacuated, the
entrance and exit chambers must be periodically vented and then
evacuated again. Due to the large volumes of these chambers and the
Process chamber Intermediate chamber Process chamber
short cycle times, a high pumping speed is required. It is provided by 1 2
combinations of rotary vane pumps and Roots pumps. For particularly short L1Z LZ2
cycle times gas cooled Roots pumps are also used. ← Slits →
S1 SZ S2
to backing pumps
Entrance chamber Transfer chamber 2 Exit chamber L1Z, LZ2 = conductance between intermediate chamber and process chamber 1 or 2
Transfer chamber 1
Sputter chambers SZ = pumping speed at intermediate chamber
S1, S2 = pumping speed at process chamber 1 or 2
Fig. 7.8 Plant for coating glass panes Ð 3-chamber in-line system, throughput up to Fig. 7.9 Principle of chamber separation through pressure stages
3,600,000 m2 / year
137
Applications of vacuum technology
Fig. 7.10 Plant for coating data storage disks with carrier transport system
138
Instructions for equipment operation
8. Instructions for gauge) with and without a cold trap inserted in the line: Filling the cold trap
with liquid nitrogen will cause the pressure to drop abruptly, by one power
vacuum equipment of ten or more, if the container is contaminated since the vapors will freeze
out in the trap.
operation
Eliminating contamination for glass equipment
If the contaminants exhibit a high vapor pressure, then they can be pumped
8.1 Causes of faults where the out relatively quickly. If this is not successful, then the apparatus will have
desired ultimate pressure is not to be cleaned. Contaminated glass components will first be cleaned with
achieved or is achieved too chromic-sulfuric acid mixture or Ð if this is necessary Ð with dilute
slowly hydrofluoric acid (1:30). They are then rinsed with distilled water. If this
does not bring about the desired results, then an organic solvent can be
If the desired ultimate pressure is not reached at all in vacuum equipment tried. Then the glass components will again have to be rinsed with
or if it is attained only after an excessively long pumping period, then the methanol and distilled water. (Do not use denatured alcohol!)
following problems may be the reason:
If the desired ultimate pressure is not reached, then Eliminating contamination at metallic equipment
Metal components will usually exhibit traces of contamination by oil and
• the apparatus may be leaky or dirty, greases. If these cannot be readily removed by pumping down the vessel,
• the pump may dirty or damaged, then an appropriate organic solvent (denatured alcohol is unsuitable in all
cases) will have to be used for cleaning. Maximum cleanliness can be
• the vacuum gauge may be defective. achieved with vapor baths such as those commonly found in industry. If one
If the desired ultimate pressure is reached only after a very long running desires to get down to extremely low pressure ranges (< 10-7 mbar), then Ð
time, then after cleaning Ð the metal components will have to be baked out at
temperatures of up to 200 ¡C. Seriously contaminated metal components
• the apparatus may be dirty, will first have to be cleaned by cutting away or sandblasting the top surface.
• the pumping line may be restricted, These methods suffer the disadvantage that the surface area for the
surface thus treated will be increased through roughening and active
• the pump may be dirty or of too small a capacity, centers may potentially be formed which would readily adsorb vapor
• the pumping speed may be restricted due to other causes. molecules. Supplementary cleaning in the vapor bath (see above) is
advisable. In some cases electrolytic pickling of the surface may be
In order to locate the fault, one normally proceeds by separating the beneficial. In the case of high vacuum components it is necessary to pay
evacuated vessel from the pump system (where this is possible) and attention to ensuring that the pickling does not turn into etching, which
checking the vessel alone for leaks and contamination using the pressure would seriously increase the surface area. Polishing surfaces which have
rise method, for example. If it has been found that the vessel is free of been sandblasted is not necessary when working in the rough and medium
defects in this regard, then the measurement system will be checked for vacuum ranges since the surface plays only a subordinate role in these
cleanliness (see Section 8.38) and ultimately Ð if required Ð the pump or the pressure regimes.
pumping system itself will be examined.
139
Instructions for equipment operation
8.3.1 Oil-sealed rotary vacuum pumps If an oil-filled rotary pump is operated without an oil separation and return
(Rotary vane pumps and device, then it will be necessary to expect a certain amount of oil
consumption, the extent of which will depend on the size of the pump and
rotary piston pumps)
the nature of the operations. In the worst case this can amount to about 2
cm3 for every cubic meter of air pumped (at STP and including the gas
8.3.1.1 Oil consumption, oil contamination, oil ballast also drawn in). Figure 8.1 makes it possible to predict the amount of
change oil loss to be expected in practical situations. The example demonstrates
The oil serves to: that greater oil losses must be expected when operating the pump with gas
• lubricate moving parts, ballast. This situation, which is generally valid, is always to be taken into
• seal moving parts against atmospheric pressure, account in practice.
• seal the valve, If the pump oil has become unusabledue to exposure to the vapors or
• fill the dead space below the valve, contaminants which are encountered in the process, then the oil will have
• to seal the various operational spaces one from another. to be replaced. It is impossible to formulate any hard-and-fast rules as to
In all pumps it is possible to check the oil charge during operation using the when an oil change will be required since the nature of the operations will
built-in oil level sight glass. During continuous operation in particular it is determine how long the oil will remain good. Under clean conditions (e.g.
necessary to ensure that the oil charge never falls below the minimum backing pumps for diffusion pumps in electro-nuclear accelerators) rotary
level. During a pumping process oil-sealed rotary pumps will emit oil vapors vacuum pumps can run for years without an oil change. Under extremely
from the discharge port, this being due to the high operating temperature. ÒdirtyÓ conditions (e.g. during impregnation) it may be necessary to change
This leads to oil loss to an extent which will depend on the quantity of gas the oil daily. The oil will have to be replaced when its original light brown
or vapor which is drawn into the pump. Larger oil droplets can be retained color, has turned dark brown or black due to ageing or has become cloudy
by installing a coarse separator in the discharge line. This will reduce oil because liquid (such as water) has entered the pump. An oil change is also
loss considerably. The fine oil mist filter installed in some pumps will also necessary when flakes form in corrosion protection oil, indicating that the
retain the finest oil droplets (fine separation) so that no oil at all will leave corrosion protection agent is exhausted.
the outlet of the pump and oil loss is reduced practically to zero since Ð as
in coarse separation Ð the oil which is separated out is returned to the Changing the oil
pump. With pumps without an integral fine separator this device is offered The oil change should always be carried out with the pump switched off but
as an optional extra. at operating temperature. The oil drain (or fill) opening provided for each
pump is to be used for this purpose. Where the pump is more seriously
contaminated, then it should be cleaned. The applicable operating instruct-
ions are to be observed in this case.
normal pump oil (N 62). These types of vapors will then react with the basic
(alkaline) corrosion protection agent in the oil. The continuous neutralization
reactions will exhaust the corrosion protection agent at a rate depending on
the quantity and acidity of the vapors. The oil will have to be changed more
frequently, in accordance with these factors. Corrosion protection oils are
either very hygroscopic or they easily form emulsions with water.
Consequently a pump which is filled with corrosion protection oil will absorb
moisture from the air if it is out of service for an extended period of time. In
no case should one ever use a pump filled with corrosion protection oil in
order to pump water vapor since the lubricating and corrosion inhibition
Intake pressure [mbar] properties of the oil would be adversely affected. Once the oil has absorbed
water it will no longer be possible for such pumps to achieve the ultimate
Example: Oil losses for a TRIVAC S 16 A at pressure of 1 mbar:
a) Without gas ballast: in accordance with the pumping speed curve S = 15 m3 / h; according pressures which would be the case with fresh corrosion protection oil or
to diagram: oil loss = 0.03 cm3 / h (line a) standard pump oil (N 62). Oil-filled pumps should, under normal operating
b) With gas ballast: S = 9 m3/h at 1 mbar; oil loss = 0.018 cm3 / h (line b1), plus additional
loss due to gas ballast quantity (0.1 times the 1.6 m3 / h rated pumping speed); that is: Chart on con-ditions, not be filled with corrosion protection oil. N 62 oil is preferred
the horizontal line b2 up to atmospheric pressure: additional loss: 3 cm3 / h (diagonal line). when pumping air, water vapor and non-corrosive organic vapors in so far
Overall loss during gas ballast operation 0.018 + 3 = 3.018 cm3 / h.
as there is positive protection against the vapors condensing inside the
Fig. 8.1 Oil loss for oil-sealed pumps (referenced to an approximate maximum value of 2 cm3 pump.
oil loss per cubic meter of air drawn in [STP])
140
Instructions for equipment operation
8.3.1.3 Measures when pumping various chemical assist in solving such problems.
substances
b) Anhydrides
This discussion cannot provide exhaustive coverage of the many and varied
CO (carbon monoxide) is a strong reducing agent. When CO is being
application fields for oil-filled vacuum pumps in the chemicals industry. Our
pumped it is therefore important that air not be used as the gas ballast but
many years of experience with the most difficult of chemicals applications
rather that inert gases be used at the very outside (e.g. Ar or N2). Inert gas
can be used to solve your particular problems. Three aspects should,
ballast should also be used when pumping SO2, SO3, and H2S. A corrosion
however, be mentioned briefly: pumping explosive gas mixes, condensable
inhibiting oil is also to be used when handling these three anhydrides.
vapors, and corrosive vapors and gases.
Carbon dioxide (CO2) can be pumped without making any special
arrangements.
Explosion protection
Applicable safety and environmental protection regulations shall be
c) Alkaline solutions
observed when planning and engineering vacuum systems. The operator
Normal N 62 pump oil is to be used to pump basic (alkaline) solutions.
must be familiar with the substances which the system will be pumping and
Sodium hydroxide and caustic potash solutions should not be pumped in
take into account not only normal operating conditions but also abnormal
their concentrated form. Ammonia is highly amenable to pumping with the
situations, operating outside normal parameters. The most important aids to
gas ballast valve closed. Alkaline organic media such as methylamine and
avoiding explosive mixtures are Ð in addition to inertization by adding
dimethylamine can also be pumped satisfactorily, but with the gas ballast
protective gases Ð maintaining the explosion limit values with the aid of
valve open.
condensers, adsorption traps and gas scrubbers.
d) Elementary gases
Protection against condensation
Pumping nitrogen and inert gases requires no special measures.
LEYBOLD pumps offer three options for keeping vapors from condensing in
the pumps: When handling hydrogen it is necessary to make note of the hazard of
creating an explosive mixture. The gas ballast valve may in no case be
• The gas ballast principle (See Fig. 2.14). This increases considerably
opened when dealing with hydrogen. The motors driving the pumps must
the amount of vapor which the pump can tolerate.
be of explosion-proof design.
• Increased pump temperature. The rugged design of our pumps makes it
possible to run them at temperatures of up to 120 ¡C. Thus the Oxygen: Particular caution is required when pumping pure oxygen!
tolerance for pure water vapor, for example, will rise by a factor of five Specially formulated pump oils must be used for this purpose. We can
when compared with normal gas ballast operation. supply these, accompanied by an approval certificate issued by the German
• Using vacuum condensers (see Section 2.15). These act as selective Federal Materials Testing Authority (BAM), following consultation.
pumps and should be sized so that the downstream gas ballast pump
will not receive more vapor than the amount corresponding to the e) Alkanes
appropriate vapor tolerance. The low molecular weight alkanes such as methane and butane can be
pumped with the gas ballast valve closed or using inert gas as the gas
Corrosion protection ballast and/or at increased temperature of the pump. But important Ð
Oil-sealed pumps are already quite satisfactorily protected against corrosion Increased explosion hazard!
due to the oil film which will be present on all the component surfaces.
Corrosion is defined here as the electrochemical dissolution of metals, i.e. f) Alcohols
the release of electrons by the metal atom and their acceptance by the Once operating temperature has been reached, methanol and ethanol can
oxidation agent (corrosive gas). A metal atom which is susceptible to be extracted without using gas ballast (N 62 pump oil). To pump higher
corrosion must therefore be exposed to an active atom of the oxidation molecular weight alcohols (e.g. butanol) the gas ballast valve will have to
agent. be opened or other protective measures will have to be implemented to
This makes clear how the oil-sealed pump is protected against corrosion; prevent condensation.
the concentration of the oxidation agent in the oil is negligible and thus the
opportunity for the metal to release electrons is equally small. This also g) Solvents
makes it clear that the use of so-called Ònon-rustingÓ or ÒstainlessÓ steels Acetone: Can be extracted without difficulty; wait until normal operating
does not make sense since oxidation is necessary for the passivation of temperature is reached.
these steels, in order to reach the so-called passive region for these steel
Benzene: Caution Ð vapors are highly flammable. Ultimate pressure is
compounds. The critical passivation current density will normally not appear
degraded by dilution of the pump oil. Mixtures of air and benzene are
in oil-sealed pumps.
explosive and flammable. Work without a gas ballast! Inert gases may
possibly be used as ballast gas.
a) Acids
Our pumps are fundamentally suited to pumping acids. In special situations Carbon tetrachloride and trichlorethylene: Amenable to pumping; non-
problems with the oil and with auxiliary equipment attached at the intake flammable and non-explosive but will be dissolved in oil and thus increase
and/or discharge end may occur. Our engineers in Cologne are available to the ultimate pressure; wait until normal operating temperature is achieved.
141
Instructions for equipment operation
Keep the gas ballast open when pumping carbon tet and other non- strip; a motor protection switch (overload/ overheating) shall be provided as
flammable solvents. Use N 62 pump oil. required by local codes.
Toluene: Pump through the low-temperature baffle and without gas ballast. The direction of motor rotation shall be checked with the intake and outlet
Use inert gas, not air, as the gas ballast. ports open prior to installing the pump. The drive shaft, seen from the motor
end, must rotate counter-clockwise. Note the arrow on the motor indicating
the direction of rotation! If the roots pump runs in the wrong direction, then
8.3.1.4 Operating defects while pumping with gas it is reversed by interchanging two of the phases at the motor connection
ballast – Potential sources of error where cord.
the required ultimate pressure is not The roots pump may be switched on only after the roughing pump has
achieved evacuated the vacuum vessel down to the cut-in pressure.
a) The pump oil is contaminated (particularly with dissolved vapors). Check Permissible cut-in pressure PE will depend on the reduction ratios of the
the color and properties. Remedy: Allow the pump to run for an roots pump as against the roughing pump and is calculated by dividing the
extended period of time with the vacuum vessel isolated and the gas permissible pressure differential Æpmax by the compression ratio, reduced
ballast valve open. In case of heavy contamination an oil change is by the value of 1:
advisable. The pump should never be allowed to stand for a longer
∆pmax
period of time when it contains contaminated oil. p = where
E k th – 1
b) The sliding components in the pump are worn or damaged. Under clean
conditions our pumps can run for many years without any particular Theoretical pumping speed for the roots pump
k th =
Nominal pumping speed for the roughing pump
mainte-nance effort. Where the pump has been allowed to run for a
longer period of time with dirty oil, however, the bearings and the gate
valves may exhibit mechanical damage. This must always be assumed If the pump is protected using a diaphragm-type pressure switch, then the
when the pump no longer achieves the ultimate pressure specified in pump will be switched on automatically. If a combination of roots pump and
the catalog even though the oil has been changed. In this case the roughing pump is to convey highly volatile substances such as liquids with
pump should be sent in for repair or our customer service department a low boiling point, then it is advisable to use a roots pump which is
should be contacted. equipped with an integral bypass line and a valve which will respond to a
pre-set pressure. Example: Roots vacuum pumps RUVAC WAU / WSU.
c) The measurement instrument is soiled (see Section 8.4.2).
Roots pumps from the RUVAC-WAU/WSU series, being equipped with
bypass lines, can generally be switched on together with the forepump. The
Potential sources of error when the pump no longer turns
bypass protects these roots pumps against overloading.
• Check the pump electrical supply.
• The pump has stood for a long time containing contaminated or
resinous oil.
• The pump is colder than 10¡C and the oil is stiff. Heat the pump. 8.3.2.2 Oil change, maintenance work
• There is a mechanical error. Please contact our customer service Under clean operating conditions the oil in the roots pump will be loaded
department. only as a result of the natural wear in the bearings and in the gearing. We
nevertheless recommend making the first oil change after about 500 hours
Oil exits at the shaft
in service in order to remove any metal particles which might have been
If oil is discharged at the shaft, then the Seeger rotary shaft circlip in the
created by abrasion during the run-in period. Otherwise it will be sufficient
drive bearing will have to be inspected and possibly replaced. The design
to change the oil every 3000 hours in operation. When extracting gases
of the pumps makes it possible to replace this ring easily, following the
containing dust or where other contaminants are present, it will be
operating instructions provided with the unit.
necessary to change the oil more frequently. If the pumps have to run at
high ambient temperatures, then the oil in the sealing ring chamber shall
also be replaced at each oil change.
8.3.2 Roots pumps
We recommend using our specially formulated N 62 oil.
8.3.2.1 General operating instructions, installation Under ÒdirtyÓ operating conditions it is possible for dust deposits to form a
and commissioning ÒcrustÓ in the pump chamber. These contaminants will deposit in part in the
pumping chamber and in part on the pumpÕs impellers. They may be
Roots pumps must be exactly level. When attaching the pump it is
removed, once the two connection lines have been detached, either by
necessary to ensure that the pump is not under any tension or strain
blowing out the system with dry compressed air or by rinsing with a suitable
whatsoever. Any strains in the pump casing caused by the connection lines
cleaning agent, such as petroleum ether (naphtha).
shall be avoided. Any strain to which the pump is subjected will endanger
the pump since the clearances inside the roots pump are very small. The oil in the roots pump will then have to be changed. The rotor may be
turned only by hand during cleaning since, due to the high speed when the
Roots pumps are connected to the line power supply via the motor terminal
142
Instructions for equipment operation
motor is running, the deposits could damage the pump as they dislodge 8.3.3 Turbomolecular pumps
from the surfaces.
Grime which cannot be eliminated by washing can be removed 8.3.3.1 General operating instructions
mechanically using a wire brush, metallic scrubber or scraper.
In spite of the relatively large gap between the pump rotor and the stator,
the turbomolecular pumps should be protected against foreign objects
Important! entering through the intake port. It is for this reason that the pump should
The dislodged residues may not remain in the pump chamber. After never be operated without the supplied wire-mesh splinter guard. In
cleaning is completed check the pump for operability by slowly turning the addition, sharp shock to the pump when running and sudden changes in
impellers by hand. There may be no resistance to rotation. It is generally attitude are to be avoided.
not necessary to dismantle the roots pump. If this should nevertheless be
required due to heavy soiling, then it is highly advisable to have this done Over and above this, and particularly for the larger types with long rotor
by the manufacturer. blades, airing the pump to atmospheric pressure while the impellers are
rotating may be done only when observing exactly the rules given in the
operating instructions. Under certain circumstances it is possible to operate
turbomolecular pumps under exceptional conditions.
8.3.2.3 Actions in case of operational disturbances
The turbomolecular pump may, for example, be used unprotected inside
1. Pump becomes too warm: (maximum operating temperature
magnetic fields if the magnetic induction at the surface of the pump casing
100 to 115 ¡C)
does not exceed B = 3 á 10-3 T when radially impinging and B = 15 á 10-3 T
Possible causes: at axial impingement.
• Overloading: Excessive heat of compression due to an excessively In a radioactive environment standard turbomolecular pumps can be used
high pressure ratio. Check the pressure value adjustments and the without hazard at dose rates of from 104 to 105 rad. If higher dose rates are
tightness of the vacuum chamber! encountered, then certain materials in the pump can be modified in order to
• Incorrect clearances: The distances between the rotors and the withstand the greater loading. The electronic frequency converters in such
housings have been narrowed due to dirt or mechanical strain. cases are to be set up outside the radioactive areas since the semicon-
• Soiled bearings: Excessive friction in the bearings ductors used inside them can tolerate a dose rate of only about 103 rad.
• Improper oil level: If the oil level is too high, the gears will touch the oil, The use of motor-driven frequency converters which can withstand up to
causing friction resistance. Where the oil level is too low the system will 108 rad represents another option.
not be lubricated.
Roughing (backing) pumps are required for the operation of turbomolecular
• Incorrect oil type: An SAE 30 grade oil must be used for the pump.
pumps. Depending on the size of the vessel to be evacuated, the
2. Excessive power consumption: All the factors which can lead to turbomolecular pumps and forepumps may be switched on simultaneously.
elevated temperatures can also cause excessisve amounts of power to If the time required to pump the vessel down to about 1 mbar using the
be drawn. The motor is defective if excessive power requirements are particular fore-pump is longer than the run-up time for the pump (see
not accompanied by a rise in the temperature at the pump. operating instructions), then it is advisable to delay switching on the
turbomolecular pump. Bypass lines are advisable when using
3. Oiling at the pump chamber: turbomolecular pumps in systems set up for batch (cyclical) operations in
order to save the run-up time for the pump. Opening the high vacuum valve
Possible causes: is not dangerous at pressures of about 10-1 mbar.
• Oil level too high: Oil is subjected to excessive thermal loading. Oil
foam is swept along.
• Oil mixed with the product: Azeotropic degasification of the oil. 8.3.3.2 Maintenance
• Pump leaking: Air ingress through the oil drain or filler screw will cause Turbomolecular pumps and frequency converters are nearly maintenance-
a large stream of air and conveyance of oil into the pumping chamber. free. In the case of oil-lubricated pumps it is necessary to replace the
4. Abnormal running noises: bearing lubricant at certain intervals (between 1500 and 2500 hours in
operation, depending on the type). This is not required in the case of
Possible causes: grease-lubricated pumps (lifetime lubrication). If it should become
• Grime at the impeller necessary to clean the pumpÕs turbine unit, then this can easily be done by
• Bearing or gearing damage the customer, observing the procedures described in the operating
• Impellers are touching the housing instructions.
In the case of bearing or gearing damage or where the impeller scrapes the
housing the pump should be repaired only by the manufacturer.
143
Instructions for equipment operation
8.3.4 Diffusion and vapor-jet vacuum to protect the pump from damage. Remedy: Measure the exit
pumps temperature of the coolant water (it should not exceed 30 ¡C). Increase
the coolant flow-through rate. The cooling coils at the pump may have to
be decalcified.
8.3.4.1 Changing the pump fluid and cleaning the • Forevacuum pressure too high: This is possible particularly where
pump vapors which are either evacuated from the vessel or are created as
Changing the pump fluid is always necessary whenever the pump no longer cracking products from the driving medium (e.g. following air ingress)
achieves the required ultimate vacuum or when its pumping speed falls off. get into the roughing pump. Check the forevacuum pressure with the oil
The service life of the pump fluid will as a rule come to several weeks or diffusion pump disconnected. Remedy: Run the forevacuum pump for an
months Ð or even years Ð and will depend largely on the operating extended period of time with gas ballast. If this is not sufficient, then the
conditions for the pump. It is reduced by frequent pumping at high oil in the forepump will have to be changed.
pressures, by exposure to aggressive vapors and by air ingress of longer • Pump fluid at the diffusion pump spent or unserviceable: Replace the
duration (this does not apply to silicone oil and mercury). driving medium.
• Heating is incorrect: Check the heating output and check for good
In the case of oil diffusion and vapor-jet pumps the danger presented to the thermal contact between the heating plate and the bottom of the boiler
pump fluid where there is air ingress with the pump hot is often section. Replace the heating unit if necessary.
overestimated. Where air ingress (up to atmospheric pressure) is • Leaks, contamination:
encountered only occasionally and for short periods of time then silicone oil Remedy: if the pump has been contaminated by vapors it may help to
will not be attacked at all and the DIFFELEN pump fluid will only barely be use a metering valve to pass air through the apparatus for some period
affected. The products with considerably higher vapor pressures which can of time; here the pressure should not exceed 10-2 mbar when
be created through oxidation are removed again in a short period of time by DIFFELEN is being used.
the fractionation and degassing equipment in the pump (see Section • Measurement system old or soiled (see Section 8.4.2).
2.1.6.1). Even though the pump fluid which was originally light in color has
been turned brown by air ingress, this need not necessarily mean that the Potential sources of error where there is insufficient pumping speed:
medium has become unusable. If, on the other hand, the pump fluid has • Forevacuum pressure is too high: Check the forevacuum; allow the gas
turned cloudy and has become more viscous, as well (which may be the ballast pump to run for a longer period of time with the gas ballast valve
case following periods of air ingress lasting for several minutes) then the open. It may be necessary to change the oil in the forepump.
medium will have to be replaced. It is possible that under certain • The pump fluid in the diffusion pump has become unserviceable: Driving
circumstances cracking products from the pump fluid may make the oil in medium will have to be replaced.
the forepump unserviceable so that here, too, an oil change will have to be • Nozzles at the diffusion pump are clogged: Clean the diffusion pump.
made. • Heating is too weak: Check heating output; examine heating plate for
good thermal contact with the bottom of the boiler chamber.
Mercury diffusion and vapor-jet pumps are less sensitive to air ingress than
• Substances are present in the vacuum vessel which have a higher
oil diffusion pumps. The oxidation of the hot mercury caused by the air
vapor pressure than the driving medium being used: among these are,
ingress is negligible in regard to the operating characteristics of the pump
for example, mercury, which is particularly hazardous because the
when compared with the mercury loss in the forepump line.
mercury vapors will form amalgams with the nonferrous metals in the oil
Changing the pump fluid: The interior section will be extracted from the diffusion pump and thus make it impossible to achieve perfect vacuums.
pump and the contaminated pump fluid poured out. The interior section and
the pump body are then cleaned with pure petroleum ether (naphtha). The
interior section and pump body of mercury pumps should have been 8.3.5 Adsorption pumps
cleaned beforehand with a clean brush; use a bottle brush for the nozzle
bores. Ensure that all the nozzle orifices are properly cleaned. It is 8.3.5.1 Reduction of adsorption capacity
advantageous to evaporate all solvent residues in a drying kiln. Then the
A considerable reduction in pumping speed and failure to reach the ultimate
inside section is inserted once again and the fresh pump fluid is installed
pressure which is normally attainable in spite of thermal regeneration
through the forevacuum port. It is necessary to ensure that the upper
having been carried out indicates that the zeolite being used has become
nozzle cover is not moistened with pump fluid! Do not install too much
contaminated by outside substances. It does not make good sense to
pump fluid!
attempt to rejuvenate the contaminated zeolite with special thermal
processes. The zeolite should simply be replaced.
144
Instructions for equipment operation
element associated with the pump, for a period of several hours so that pumps manufactured by LEYBOLD are so good that no problems will be
contaminants which might have collected during the storage period can encountered when returning the units to service, even after a longer period
dissipate. in storage.
When the sputter-ion pumps are installed one should ensure that the
magnetic fields will not interfere with the operation of other devices
8.3.6 Titanium sublimation pumps (ionization vacuum gauges, partial pressure measurement units, etc.).
Each of the turns in the titanium sublimation pump contains approximately Mounting devices for the sputter-ion pumps may not short circuit the
1.2 g of useable titanium supply. At a heating current of 50 A the surface inductance flow and thus weaken the air gap inductance and pumping
temperature comes to about 1850 K, the sublimation rate approximately speed.
0.12 g/h, i.e. a turn can be operated continuously for about 10 hours. Since If the ultimate pressure which can be attained is not satisfactory even
at pressures below 1 á 10-6 mbar sublimation is not continuous but rather though the apparatus is properly sealed, then it will usually be sufficient to
only at intervals which Ð at low pressures (below 5 á 10-8 mbar) and low gas bake out the attached equipment at about 200 to 250 ¡C. If the pressure
volumes Ð are already more than ten times the actual sublimation period, here rises to about 1 á 10-5 mbar when this is done, then the sputter ion
one may assume a pumping period of almost one month at a working pump will become so hot after evacuating the gases for two hours that it will
pressure of 10-10 mbar per turn. not be necessary to heat it any further in addition. It is also possible to heat
The effective pumping speed of a titanium sublimation pump will depend on the pump by allowing air to enter for 2 hours at 10-5 mbar before the other
the getter screen surface and the geometry of the suction opening. The apparatus is then subsequently baked out. If the ultimate pressure is still
pumping speed, referenced to the surface area of the getter surface, will be not satisfactory, then the pump itself will have to be baked out for a few
dependent on the type of gas and the getter screen temperature. Since hours at 250 to 300¡C (but not higher than 350 ¡C!). The pump should
inert gases, for example, cannot be pumped at all, titanium sublimation without fail remain in operation throughout this period! If the pressure rises
pumps should always be used only with an auxiliary pump (sputter-ion above 5 á 10-5 mbar it will be necessary either to heat more slowly or to
pump, turbomolecular pump) used to pump these gas components. The connect an auxiliary pump. Before airing one should allow the hot sputter-
supplementary pump can be much smaller than the titanium sublimation ion pump enough time to cool down at least to 150 ¡C.
pump. Only in a few special cases can one do without the additional pump.
The selection of the coolant is dictated by the working conditions and the
requirements in terms of ultimate pressure. At high pressures, above
1 á 10-6 mbar, more thermal energy is applied to the getter screen by 8.4 Information on working with
frequent sublimation cycles. It is for this reason that cooling with liquid vacuum gauges
nitrogen is more favorable. At low pressures water cooling may be
sufficient. The getter screen should if at all possible be heated to room
temperature before airing the pump as otherwise the humidity in the air
8.4.1 Information on installing vacuum
would condense out on the surface. sensors
Here both the external situation in the immediate vicinity of the vacuum
apparatus and the operating conditions within the apparatus (e.g. working
8.3.7 Sputter-ion pumps pressure, composition of the gas content) will be important. It is initially
necessary to ascertain whether the measurement system being installed is
Sputter-ion pumps use high-voltage current. Installation and connection
sensitive in regard to its physical attitude. Sensors should only be installed
should be carried out only under the supervision of a qualified specialist.
vertically with the vacuum flange at the bottom to keep condensates, metal
The operating instructions shall be observed!
flakes and filings from collecting in the sensor or even small components
The service life of sputter-ion pumps depends linearly on the pumpÕs such as tiny screws and the like from falling into the sensorand the
operating pressure. In the case of pumps manufactured by LEYBOLD, the measurement system. The hot incandescent filaments could also bend and
following applies: deform improperly and cause electrical shorts inside the measurement
system. This is the reason behind the following general rule: If at all
p á T = 45 á 10-3 mbar á h
possible, install sensors vertically and open to the bottom. It is also
(p = operating pressure, T = service life) very important to install measurement systems if at all possible at those
points in the vacuum system which will remain free of vibration during
This means that for operating pressure of
operation.
10-3 mbar the service life is 45 hours
10-6 mbar the service life is 45,000 hours The outside temperature must be taken into account and above all it is
10-9 mbar the service life is 45,000,000 hours necessary to avoid hot kilns, furnaces or stoves or other sources of intense
radiation which generate an ambient temperature around the measurement
If a triode pump is not needed over an extended period of time it can either
system which lies above the specific acceptable value. Excessive ambient
be operated continuously at low pressure Ð with practically no influence on
temperatures will result in false pressure indications in thermal conductivity
the service life Ð or it can be aired, removed from the pump and packed in
vacuum sensors.
a dust-tight container. The starting properties of the sputter-ion (triode)
145
Instructions for equipment operation
8.4.2 Contamination at the measurement is necessary to ensure in particular that the required high insulation values
system and its removal for the high-voltage electrodes and ion traps also be maintained during
operation and sometimes even during bake-out procedures. Insulation
defects may occur both in the external feed line and inside the
The vacuum gauges used in vacuum technology for pressure measurement measurement system itself. Insufficient insulation at the trap (detector) lead
will certainly work under ÒdirtyÓ conditions. This is quite understandable may allow creep currents Ð at low pressures Ð to stimulate overly high
since a vacuum device or system does not serve simply to produce low pressure value readings. The very low ion trap currents make it necessary
pressures but rather and primarily have to run processes in chemistry, for this lead to be particularly well insulated. Inside the measurement
metallurgy or nuclear physics at low pressures. Here, depending on the sensors, too, creep currents can occur if the trap is not effectively shielded
nature of the process, considerable quantities of gases or vapors will be against the other electrodes.
liberated either continuously or intermittently; these can pass into the
measurement systems provided for pressure measurement and installed in An error frequently made when connecting measurement sensors to the
the vacuum system and Ð due to surface reactions or through simple vacuum system is the use of connector piping which is unacceptably long
deposits Ð can falsify the pressure measurements considerably. This is true and narrow. The conductance value must in all cases be kept as large as
for all types of vacuum gauges whereby, of course, high-sensitivity, high- possible. The most favorable solution is to use integrated measurement
accuracy measurement systems are particularly susceptible to soiling systems. Whenever connector lines of lower conductance values are used
resulting from the causes named. One can attempt to protect the the pressure indication, depending on the cleanliness of the measurement
measurement systems against contamination by providing suitable sensors and the connector line, may be either too high or too low. Here
shielding. This, however, will often lead to the pressure registered by the measurement errors by more than one complete order of magnitude are
measurement system Ð which is indeed clean Ð deviating considerably possible! Where systems can be baked out it is necessary to ensure that
from the pressure actually prevailing in the system. the connector line can also be heated.
146
Tables, Formulas, Diagrams
1 ↓ = ... → mbar Pa dyn á cmÐ2 atm Torr inch Micron cm kp á cmÐ2 lb á inÐ2 lb á ftÐ2
(N/m3) (µbar) (phys.) (mm Hg) Hg (µ) H2O (at tech.) (psi)
mbar 1 102 103 9.87 á 10Ð4 0.75 2.953 á 10Ð2 7.5 á 102 1.02 1.02 á 10Ð3 1.45 á 10Ð2 2.089
Pa 10Ð2 1 10 9.87 á 10Ð6 7.5 á 10Ð3 2.953 á 10Ð4 7.5 1.02 á 10Ð2 1.02 á 10Ð5 1.45 á 10Ð4 2.089 á 10Ð2
µbar 10Ð3 0.1 1 9.87 á 10Ð7 7.5 á 10Ð4 2.953 á 10Ð5 7.5 á 10Ð1 1.02 á 10Ð3 1.02 á 10Ð6 1.45 á 10Ð5 2.089 á 10Ð3
atm 1013 1.01 á 105 1.01 á 106 1 760 29.92 7.6 á 105 1.03 á 103 1.033 14.697 2116.4
Torr 1.33 1.33 á 102 1.33 á 103 1.316 á 10Ð3 1 3.937 á 10Ð2 103 1.3595 1.36 á 10Ð3 1.934 á 10Ð2 2.7847
in Hg 33.86 33.9 á 102 33.9 á 103 3.342 á 10Ð2 25.4 1 2.54 á 104 34.53 3.453 á 10Ð2 0.48115 70.731
µ 1.33 á 10Ð3 1.33 á 10Ð1 1.333 1.316 á 10Ð6 10Ð3 3.937 á 10Ð5 1 1.36 á 10Ð3 1.36 á 10Ð6 1.934 á 10Ð5 2.785 á 10Ð3
cm H2O 0.9807 98.07 980.7 9.678 á 10Ð4 0.7356 2.896 á 10Ð2 7.36 á 102 1 10Ð3 1.422 á 10Ð2 2.0483
at 9.81 á 102 9.81 á 104 9.81 á 105 0.968 7.36 á 102 28.96 7.36 á 105 103 1 14.22 2048.3
psi 68.95 68.95 á 102 68.95 á 103 6.804 á 10Ð2 51.71 2.036 51.71 á 103 70.31 7.03 á 10Ð2 1 1.44 á 102
lb á ftÐ2 0.4788 47.88 478.8 4.725 á 10Ð4 0. 3591 1.414 á 10Ð2 359.1 0.488 4.88 á 10Ð4 6.94 á 10Ð3 1
Normal conditions: 0 ¡C and sea level, i.e. p = 1013 mbar = 760 mm Hg = 760 torr = 1 atm
in Hg = inches of mercury; 1 mtorr (millitorr) = 10-3 torr = 1 µ (micron É µm Hg column)
Pounds per square inch = lb á in-2 = lb / sqin = psi (psig = psi gauge É pressure above atmospheric, pressure gauge reading; psia = psi absolute É absolute pressure)
Pounds per square foot = lb / sqft = lb / ft2; kgf/sqcm2 = kg force per square cm = kp / cm2 = at; analogously also: lbf / squin = psi
1 dyn á cm-2 (cgs) = 1 µbar (microbar) = 1 barye; 1 bar = 0.1 Mpa; 1 cm water column (cm water column = g / cm2 at 4 ¡C) = 1 Ger (Geryk)
atm É physical atmosphere Ð at É technical atmosphere; 100 - (x mbar / 10.13) = y % vacuum
147
Tables, Formulas, Diagrams
Variable General formula For easy calculation Value for air at 20¡C
Most probable speed
of particles cw ABBBB
cw =
2⋅R⋅T
M
cw = 1.29 ⋅ 104AB [ ]
M
T cm
s
cw = 410 [m/s]
Mean velocity
of particles c– ABBBB
–c = 8 ⋅ R ⋅ T
π⋅M
–c = 1.46 ⋅ 10 AB
4
[ ]
T
M
cm
s
–c = 464 [m/s]
–2 3 ⋅ R ⋅ T 2 cm2
M [ s ] [s ]
Mean square of velocity – T cm –2
– c = c = 2.49 ⋅ 10
2 8
2 c = 25.16 ⋅ 104 2
of particles c2 M
Gas pressure p of particles p=n⋅k⋅T p = 13.80 ⋅ 10–20 ⋅ n ⋅ T [mbar] p = 4.04 ⋅ 10–17 ⋅ n [mbar] (applies to all gases)
1 –
p = ⋅ n ⋅ m T ⋅ c2
3
1 –
p = ⋅ ̺ ⋅ c2
3
Number density of particles n p
n = p/kT n = 7.25 ⋅ 1018 ⋅ [cm–3] p = 2.5 ⋅ 1016 ⋅ p [cm–3] (applies to all gases)
T
Area-related impingement ZA
ZA =
1
· n · –c ZA = 2.63 · 1022 ·
p
· p [cm–2 s–1] ZA = 2.85 ⋅ 1020 ⋅ p [cm–2 s–1] (see Fig. 78.2)
4 ABB
M BB
·T
ZA = ABBBB
N
·p
2⋅π⋅M⋅k⋅T
A
Volume collision rate ZV 1 n ⋅ –c p2 ZV = 8.6 ⋅ 1022 ⋅ p2 [cm–3 s–1] (see Fig. 78.2)
ZV = ⋅ ZV = 5.27 · 1022 · [cm–3 s–1]
2 λ c* · ABB
BBBB
M ·T
ZA =
1
c* ABBBB2 ⋅ NA
π⋅M⋅k⋅T
⋅p2
Equation of state of ideal gas p⋅V=ν⋅R⋅T p ⋅ V = 83.14 ⋅ ν ⋅ T [mbar ⋅ ℓ] p ⋅ V = 2.44 ⋅ 104 ν [mbar ⋅ ℓ] (for all gases)
Area-related mass flow rate qm, A
qm, A = ZA ⋅ mT = ABBBB
M ⋅p
2 ⋅ π ⋅ k ⋅ T ⋅ NA
Qm, A = 4.377 ⋅ 10–2 ABMT ⋅ p [g cm –2 s–1] qm, A = 1.38 ⋅ 10–2 ⋅ p g [cm–2 s–1]
c* =λ á p in cm á mbar λ mean free path in cm NA Avogadro constant in molÐ1 p gas pressure in mbar T thermodynamic temperature in K
(see Tab. III) M molar mass in g á molÐ1 n number density of particles in cmÐ3 R molar gas constant V volume in l
k Boltzmann constant in mbar á l á KÐ1 mT particle mass in g ν amount of substance in mol in mbar á l á molÐ1 KÐ1
Table IV: Compilation of important formulas pertaining to the kinetic theory of gases
148
Tables, Formulas, Diagrams
1↓ = ... → mbar á l/s kg á hÐ1 (20¡C) kg á hÐ1 (0¡C) cm3/h (NTP) cm3/s (NTP) Torr á l/s g/a (F12. 20 ¡C) g/a (F12. 25 ¡C) µ á cfm lusec Pa á l/s slpm
mbar á l/s 1 4.28 á 10Ð3 4.59 á 10Ð3 3554 0.987 0.75 1.56 á 105 1.54 á 105 1593 7.52 á 102 100 59.2 á 10Ð3
kg á hÐ1 (20 ¡C) 234 1 1.073 8.31 á 105 231 175 Ð Ð 37.2 á 104 1.75 á 105 23.4 á 103 13.86
kg á hÐ1 (0 ¡C) 218 0.932 1 7.74 á 105 215 163 Ð Ð 34.6 á 104 1.63 á 105 21.8 á 103 12.91
cm3/h (NTP) 2.81 á 10Ð4 1.20 á 10Ð6 1.29 á 10Ð6 1 2.78 á 10Ð4 2.11 á 10Ð4 44 Ð 44.7 á 10Ð2 2.11 á 10Ð1 2.81 á 10Ð2 1.66 á 10Ð5
cm3/s (NTP) 1.013 4.33 á 10Ð3 4.65 á 10Ð3 3600 1 0.760 1.58 á 105 Ð 1611 760 101 6 á 10Ð2
Torr á l/s 1.33 5.70 á 10Ð3 6.12 á 10Ð3 4727 1.32 1 2.08 á 105 2.05 á 105 2119 1 á 103 133 78.8 á 10Ð3
g/a (F12. 20 ¡C) 6.39 á 10Ð6 Ð Ð 2.27 á 10Ð2 6.31 á 10Ð6 4.80 á 10Ð6 1 Ð 10.2 á 10Ð3 4.8 á 10Ð3 6.39 á 10Ð4 37.9 á 10Ð8
g/a (F12. 25 ¡C) 6.50 á 10Ð6 Ð Ð Ð Ð 4.88 á 10Ð6 Ð 1 10.4 á 10Ð3 4.89 á 10Ð3 6.5 á 10Ð4 38.5 á 10Ð8
µ á cfm 6.28 á 10Ð4 2.69 á 10Ð6 2.89 á 10Ð6 2.24 6.21 á 10Ð4 4.72 á 10Ð4 98.16 96.58 1 0.472 6.28 á 10Ð2 37.2 á 10Ð6
lusec 1.33 á 10Ð3 5.70 á 10Ð6 6.12 á 10Ð6 4.737 1.32 á 10Ð3 1 á 10Ð3 208 205 2.12 1 13.3 á 10Ð2 78.8 á 10Ð6
Pa á l/s 1 á 10Ð2 4.28 á 10Ð5 4.59 á 10Ð5 35.54 9.87 á 10Ð3 7.5 á 10Ð3 1.56 á 103 1.54 á 103 15.93 7.50 1 59.2 á 10Ð5
slpm 16.88 72.15 á 10Ð3 77.45 á 10Ð3 60.08 á 103 16.67 12.69 2.64 á 106 2.60 á 106 26.9 á 103 12.7 á 103 16.9 á 102 1
1 cm3 (NTP) = 1 cm3 under normal conditions (T = 273.15 K; p = 1013.25 mbar) NTP = normal temperature and pressure (1 atm; 0 ¡C) R = 83.14 mbar á l á molÐ1 á KÐ1
1 cm3 (NTP) á hÐ1 = 1 atm á cm3 á hÐ1 = 1 Ncm3 á hÐ1 = 1 std cch SI coherent: 1 Pa á m3 á sÐ1 = 10 mbar á l á sÐ1; R = 8.314 Pa á m3 á molÐ1 á KÐ1; M in kg / mol
1 cm3 (NTP) á sÐ1 = 1 sccs = 60 cm3 (NTP) á minÐ1 60 sccm = 60 std ccm = 60 Ncm3 á minÐ1 1 lusec = 1 l á µ á sÐ1 1 á µ = 1 micron = 10Ð3 Torr 1 lusec = 10Ð3 Torr á l á sÐ1
Freon F 12 (CCl2F2) M = 120.92 g á molÐ1; air M = 28.96 g á molÐ1 1 sccm = 10Ð3 slpm = 10Ð3 N á l á minÐ1 = 60 sccs
Note: Anglo-American units are not abbreviated nonuniformly! Example: Standard cubic centimeter per minute → sccm = sccpm = std ccm = std ccpm
1↓= ... → mbar á l/s cm3/s **) Torr á l/s Pa á m3/s g/a *) oz/yr *) lb/yr *) atm á ft3/min µ á l/s µ á ft3/h µ á ft3/min
mbar á l/s 1 0.987 0.75 10Ð1 1.56 á 105 5.5 á 103 3.4 á 102 2.10 á 10Ð3 7.52 á 102 9.56 á 104 1593
cm3/s **) 1.013 1 0.76 1.01 á 10Ð1 1.58 á 105 5.6 á 103 3.44 á 102 2.12 á 10Ð3 760 96.6 á 103 1614
Torr á l/s 1.33 1.32 1 1.33 á 10Ð1 2.08 á 105 7.3 á 103 4.52 á 102 2.79 á 10Ð3 103 1.27 á 105 2119
Pa á m3/s 10 9.9 7.5 1 1.56 á 106 5.51 á 104 3.4 á 103 2.09 á 10Ð2 7.5 á 103 9.54 á 105 15.9 á 103
g/a *) 6.39 á 10Ð6 6.31 á 10Ð6 4.80 á 10Ð6 6.41 á 10Ð7 1 3.5 á 10Ð2 2.17 á 10Ð3 1.34 á 10Ð8 4.8 á 10Ð3 0.612 10.2 á 10Ð3
oz/yr *) 1.82 á 10Ð4 1.79 á 10Ð4 1.36 á 10Ð4 1.82 á 10Ð5 28.33 1 6.18 áá 10Ð2 3.80 á 10Ð7 0.136 17.34 0.289
lb/yr *) 2.94 á 10Ð3 2.86 á 10Ð3 2.17 á 10Ð3 2.94 á 10Ð4 4.57 á 102 16 1 6.17 á 10Ð6 2.18 280 4.68
atm á ft3/min 4.77 á 102 4.72 á 102 3.58 á 102 47.7 7.46 á 107 2.63 á 106 1.62 á 105 1 3.58 á 105 4.55 á 107 7.60 á 105
µ á l/s 1.33 á 10Ð3 1.32 á 10Ð3 10Ð3 1.33 á 10Ð4 208 7.34 4.52 á 10Ð1 2.79 á 10Ð6 1 127 2.12
µ á ft3/h 1.05 á 10Ð5 1.04 á 10Ð5 7.87 á 10Ð6 1.05 á 10Ð6 1.63 5.77 á 10Ð2 3.57 á 10Ð3 2.20 á 10Ð8 7.86 á 10Ð3 1 1.67 á 10Ð2
µ á ft3/min 6.28 á 10Ð4 6.20 á 10Ð4 4.72 á 10Ð4 6.28 á 10Ð5 98 3.46 2.14 á 10Ð1 1.32 á 10Ð6 0.472 60 1
1áµá ft3 á hÐ1 = 1.04 á 10Ð5 stsd cc per second 1 micron cubic foot per hour = 0.0079 micron liter per second 1 kg = 2.2046 pounds (lb)
1 cm3 á sÐ1 (NTP) = 1 atm á cm3 á sÐ1 = 1 scc á sÐ1 = 1 sccss 1 micron liter per second = 0.0013 std cc per second = 1 lusec 1 cubic foot (cfut. cf) = 28.3168 dm3
1 atm á ft3 á minÐ1 = 1 cfm (NTP) 1 micron cubic foot per minute = 1 µ á ft3 á minÐ1 = 1 µ á cuft á minÐ1 = 1µ á cfm 1 lb = 16 ounces (oz)
1 Pa á m3/s = 1 Pa á m3/s (anglo-am.) = 103 Pa á l/s 1 standard cc per second = 96.600 micron cubic feet per hour 1 lusec = 1 µ á l á sÐ1
1µálá sÐ1 = 127 µ á ft3 á hÐ1 = 0.0013 std cc per second = 1 lusec 1 std cc/sec = 760 µ á l á sÐ1
*) F12 (20 ¡C) C.Cl2F2 M = 120.92 h/mol **) (NTP) normal temperature and pressure 1 atm und 0 ¡C
149
Tables, Formulas, Diagrams
Other special features Convection dependent Significant change in Significant reduction- Particles on the
on pressure thermal conductivity in volume surfaces dominate
of a gas related collision rate to a great extend in
relation to particles in
gaseous space
Table IX: Pressure ranges used in vacuum technology and their characteristics (numbers rounded off to whole power of ten)
At room temperature
Standard values1 Metals Nonmetals
(mbar á l á sÐ1 á cmÐ2) 10Ð9 ... á 10Ð7 10Ð7 ... á 10Ð5
Outgassing rates (standard values) as a function of time
Examples: 1/2 hr. 1 hr. 3 hr. 5 hr. Examples: 1/2 hr. 1 hr. 3 hr. 5 hr.
Ag 1.5 á 10Ð8 1.1 á 10Ð8 2 á 10Ð9 Silicone 1.5 á 10Ð5 8 á 10Ð6 3.5 á 10Ð6 1.5 á 10Ð6
Al 2 á 10Ð8 6 á 10Ð9 NBR 4 á 10Ð6 3 á 10Ð6 1.5 á 10Ð6 1 á 10Ð6
Cu 4 á 10 Ð8 2 á 10Ð8 6 á 10Ð9 3.5 á 10Ð9 Acrylic glass 1.5 á 10Ð6 1.2 á 10Ð6 8 á 10Ð7 5 á 10Ð7
Stainless steel 9 á 10Ð8 3.5 á 10Ð8 2.5 á 10Ð8 FPM, FKM 7 á 10Ð7 4 á 10Ð7 2 á 10Ð7 1.5 á 10Ð7
1 All values depend largely on pretreatment!
150
Tables, Formulas, Diagrams
Table XI: Nominal internal diameters (DN) and internal diameters of tubes, pipes and apertures
with circular cross-section (according to PNEUROP).
Acetone 58 0.798 56
Benzene (solution) 78 0.8788 5.49 80.2 25
Petrol (light) 0.68 ... 0.72 > 100
Carbon tetrachloride 153.8 1.592 Ð 22.9 76.7 25
Chloroform 119.4 1.48 Ð 63.5 61 50
Diethyl ether 46 0.7967 Ð114.5 78 1000
Ethyl alcohol 74 0.713 Ð 116.4 34.6 400
Hexane 86 0.66 Ð 93.5 71 500
Isopropanol 60.1 0.785 Ð 89.5 82.4 400
Methanol 32 0.795 Ð 97.9 64.7 200 (toxic!)
Methylene chloride 85 1.328 41
Nitromethane 61 1.138 Ð 29.2 101.75 100
Petroleum ether mixture 0.64 Ð 40 ... 60
Trichlorethylene (ãTriÒ) 131.4 1.47 55
Water 18.02 0.998 0.00 100.0 Ð
151
Tables, Formulas, Diagrams
t ps ̺D t ps ̺D t ps ̺D t ps ̺D
¡C mbar g/m3 ¡C mbar g/m3 ¡C mbar g/m3 ¡C mbar g/m3
Ð 100 1.403 á 10Ð5 1.756 á 10Ð5 Ð 35 0.2233 0.2032 30 42.43 30.38 95 845.3 504.5
Ð 99 1.719 2.139 Ð 34 0.2488 0.2254 31 44.93 32.07 96 876.9 522.1
Ð 98 2.101 2.599 Ð 33 0.2769 0.2498 32 47.55 33.83 97 909.4 540.3
Ð 97 2.561 3.150 Ð 32 0.3079 0.2767 33 50.31 35.68 98 943.0 558.9
Ð 96 3.117 3.812 Ð 31 0.3421 0.3061 34 53.20 37.61 99 977.6 578.1
Ð 95 3.784 á 10Ð5 4.602 á 10Ð5 Ð 30 0.3798 0.3385 35 56.24 39.63 100 1013.2 597.8
Ð 94 4.584 5.544 Ð 29 0.4213 0.3739 36 59.42 41.75 101 1050 618.0
Ð 93 5.542 6.665 Ð 28 0.4669 0.4127 37 62.76 43.96 102 1088 638.8
Ð 92 6.685 7.996 Ð 27 0.5170 0.4551 38 66.26 46.26 103 1127 660.2
Ð 91 8.049 9.574 Ð 26 0.5720 0.5015 39 69.93 48.67 104 1167 682.2
Ð 90 9.672 á 10Ð5 11.44 á 10Ð5 Ð 25 0.6323 0.5521 40 73.78 51.19 105 1208 704.7
Ð 89 11.60 13.65 Ð 24 0.6985 0.6075 41 77.80 53.82 106 1250 727.8
Ð 88 13.88 16.24 Ð 23 0.7709 0.6678 42 82.02 56.56 107 1294 751.6
Ð 87 16.58 19.30 Ð 22 0.8502 0.7336 43 86.42 59.41 108 1339 776.0
Ð 86 19.77 22.89 Ð 21 0.9370 0.8053 44 91.03 62.39 109 1385 801.0
Ð 85 23.53 á 10Ð5 27.10 á 10Ð5 Ð 20 1.032 0.8835 45 95.86 65.50 110 1433 826.7
Ð 84 27.96 32.03 Ð 19 1.135 0.9678 46 100.9 68.73 111 1481 853.0
Ð 83 33.16 37.78 Ð 18 1.248 1.060 47 106.2 72.10 112 1532 880.0
Ð 82 39.25 44.49 Ð 17 1.371 1.160 48 111.7 75.61 113 1583 907.7
Ð 81 46.38 52.30 Ð 16 1.506 1.269 49 117.4 79.26 114 1636 936.1
Ð 80 0.5473 á 10Ð3 0.6138 á 10Ð3 Ð 15 1.652 1.387 50 123.4 83.06 115 1691 965.2
Ð 79 0.6444 0.7191 Ð 14 1.811 1.515 51 129.7 87.01 116 1746 995.0
Ð 78 0.7577 0.8413 Ð 13 1.984 1.653 52 136.2 91.12 117 1804 1026
Ð 77 0.8894 0.9824 Ð 12 2.172 1.803 53 143.0 95.39 118 1863 1057
Ð 76 1.042 1.145 Ð 11 2.376 1.964 54 150.1 99.83 119 1923 1089
Ð 75 1.220 á 10Ð3 1.334 á 10Ð3 Ð 10 2.597 2.139 55 157.5 104.4 120 1985 1122
Ð 74 1.425 1.550 Ð 9 2.837 2.328 56 165.2 109.2 121 2049 1156
Ð 73 1.662 1.799 Ð 8 3.097 2.532 57 173.2 114.2 122 2114 1190
Ð 72 1.936 2.085 Ð 7 3.379 2.752 58 181.5 119.4 123 2182 1225
Ð 71 2.252 2.414 Ð 6 3.685 2.990 59 190.2 124.7 124 2250 1262
Ð 70 2.615 á 10Ð3 2.789 á 10Ð3 Ð 5 4.015 3.246 60 199.2 130.2 125 2321 1299
Ð 69 3.032 3.218 Ð 4 4.372 3.521 61 208.6 135.9 126 2393 1337
Ð 68 3.511 3.708 Ð 3 4.757 3.817 62 218.4 141.9 127 2467 1375
Ð 67 4.060 4.267 Ð 2 5.173 4.136 63 228.5 148.1 128 2543 1415
Ð 66 4.688 4.903 Ð 1 5.623 4.479 64 293.1 154.5 129 2621 1456
Ð 65 5.406 á 10Ð3 5.627 á 10Ð3 0 6.108 4.847 65 250.1 161.2 130 2701 1497
Ð 64 6.225 6.449 1 6.566 5.192 66 261.5 168.1 131 2783 1540
Ð 63 7.159 7.381 2 7.055 5.559 67 273.3 175.2 132 2867 1583
Ð 62 8.223 8.438 3 7.575 5.947 68 285.6 182.6 133 2953 1627
Ð 61 9.432 9.633 4 8.129 6.360 69 298.4 190.2 134 3041 1673
Ð 60 10.80 á 10Ð3 10.98 á 10Ð3 5 8.719 6.797 70 311.6 198.1 135 3131 1719
Ð 59 12.36 12.51 6 9.347 7.260 71 325.3 206.3 136 3223 1767
Ð 58 14.13 14.23 7 10.01 7.750 72 339.6 214.7 137 3317 1815
Ð 57 16.12 16.16 8 10.72 8.270 73 354.3 223.5 138 3414 1865
Ð 56 18.38 18.34 9 11.47 8.819 74 369.6 232.5 139 3512 1915
Ð 55 20.92 á 10Ð3 20.78 á 10Ð3 10 12.27 9.399 75 385.5 241.8 140 3614 1967
Ð 54 23.80 23.53 11 13.12 10.01 76 401.9 251.5
Ð 53 27.03 26.60 12 14.02 10.66 77 418.9 261.4
Ð 52 30.67 30.05 13 14.97 11.35 78 436.5 271.7
Ð 51 34.76 33.90 14 15.98 12.07 79 454.7 282.3
Ð 50 39.35 á 10Ð3 38.21 á 10Ð3 15 17.04 12.83 80 473.6 293.3
Ð 49 44.49 43.01 16 18.17 13.63 81 493.1 304.6
Ð 48 50.26 48.37 17 19.37 14.48 82 513.3 316.3
Ð 47 56.71 54.33 18 20.63 15.37 83 534.2 328.3
Ð 46 63.93 60.98 19 21.96 16.31 84 555.7 340.7
Ð 45 71.98 á 10Ð3 68.36 á 10Ð3 20 23.37 17.30 85 578.0 353.5
Ð 44 80.97 76.56 21 24.86 18.34 86 601.0 366.6
Ð 43 90.98 85.65 22 26.43 19.43 87 624.9 380.2
Ð 42 102.1 95.70 23 28.09 20.58 88 649.5 394.2
Ð 41 114.5 á 10Ð3 106.9 á 10Ð3 24 29.83 21.78 89 674.9 408.6
Ð 40 0.1283 0.1192 25 31.67 23.05 90 701.1 423.5
Ð 39 0.1436 0.1329 26 33.61 24.38 91 728.2 438.8
Ð 38 0.1606 0.1480 27 35.65 25.78 92 756.1 454.5
Ð 37 0.1794 0.1646 28 37.80 27.24 93 784.9 470.7
Ð 36 0.2002 0.1829 29 40.06 28.78 94 814.6 487.4
1 Sources: Smithsonian Meteorological Tables 6th. ed. (1971) and VDI vapor tables 6th ed (1963).
Table XIII: Saturation pressure ps and vapor density ̺D of water in a temperature range from Ð100¡C to +140¡C1
152
Tables, Formulas, Diagrams
Octane a Tetrahydrofuran a
Cyclohexane c Tetrafluoroethylene a
Propylene (propene) a
Styrene (s) b
Benzene (s) c
Toluene (s) Ð
Methanol (s) c MIC2 ratio > 0.8 mm 0.45 ... 0.8 mm < 0.45 mm
Ethanol (s) c
1 Minimum Electrical Spark Gap
Propyl alcohol (propanol) c 2 Minimum Ignition Current
The ratio is based on the MIC value for laboratory methane
Butyl alcohol (butanol) a 3 Group allocation:
Phenol Ð a Ð according to MESG value
b Ð according to MIC ratio
Acetaldehyde (ethanal) a c Ð according to both MESG value and MIC ratio
(s) Ð solvent
Acetone (s) (propanone) c
Ethyl methacrylate Ð
Ammonia a
acetonitrile a
Aniline Ð
Pyridine Ð
Table XIV: Hazard classification of fluids according to their MESG1 and/or MIC2 values.
(Extract from European Standard EN 50.014)
153
Tables, Formulas, Diagrams
x = resistant x = resistant
Ð = conditionally resistant Ð = conditionally resistant
Silicone rubber
o = not resistant
Silicone rubber
o = not resistant
Teflon (PTFE)
Teflon (PTFE)
EPDM
EPDM
Acetaldehyde o o o o x x Carbon dioxide, dry x x x x x
Acetic acid (crystalline), pure Ð o Ð o x Ð Carbon dioxide, wet x x x x
Acetic acid, industrial x x Carbon tetrachloride o o o x x o
Acetic acid vapors x x Ð x Chloracetic acid o o o x x
Acetic acid, 20 % x x x Chlorinated solvents o x
Acetophenone o x x Chloroform o o x x o
Acetylene x Ð x x Chloromethyl o Ð x x o
Acrylnitrile Ð o x Citrus oils o o x
Air, clean x x x x x x Coke furnace gas o o x o
Air, oily x x x x x o Copra oil acid Ð o Ð x
Benzene o o x x o Dichlorethylene x
Benzene bromide o o x o Dichlorethane x x x o
Benzoic acid x x Diethylamine Ð o x x
Bitumen x Diethylene glycol x x x x
Blast furnace gas x x x x Ð Diethyl ether o Ð o x o
Table XV: Chemical resistance of commonly used elastomer gaskets and sealing materials
154
Tables, Formulas, Diagrams
x = resistant x = resistant
Ð = conditionally resistant Ð = conditionally resistant
Silicone rubber
Silicone rubber
o = not resistant o = not resistant
Teflon (PTFE)
Teflon (PTFE)
EPDM
EPDM
Dioxan o o x Ð Heating fuel oil (coal base) o o x x
Diphenyl o o Ð x x o Heating fuel oil (petroleum crude base) x Ð x x o
Diphenyloxyd o x x Heptane x Ð o x x o
Edenol 888 x x Hexaldehyde o o x x
Essential oils o o Ð x o Hexane x Ð o x x o
Formaldehyde x Ð x x x Methane x Ð x Ð
Formalin, 55 % x x x x Methane (pit gas) x x x x Ð
Formic acid Ð Ð x Ð Methylene chloride o o o x o
Formic acid methyl ester o Ð Ð x Methyl acrylate o x o
Freon 11 x x o x Methyl alcohol (methanol) Ð Ð x o x x
Table XV: Chemical resistance of commonly used elastomer gaskets and sealing materials
155
Tables, Formulas, Diagrams
x = resistant x = resistant
Ð = conditionally resistant Ð = conditionally resistant
Silicone rubber
Silicone rubber
o = not resistant o = not resistant
Teflon (PTFE)
Teflon (PTFE)
EPDM
EPDM
Oxygen x x x x Tar oil o x o
Ozone o Ð x x x x Tetrachlorethylene x x o
Palmitic acid x x x o Tetrahydrofurane o o x o
Palm oil acid Ð o x x Tetraline o o o x o
Paraffin x x x x o Toluene o o o x x o
Pydraul A 200 o x x x
Pyridine o x Ð
Salicylic acid x x x x
Skydrol 500 x o x x
Skydrol 7000 x x x
Stearic acid Ð x x
Styrene o o x x o
Sulfur Ð x x x x x
Sulfur dioxide o o x x x
Sulfur trioxide, dry o Ð x x Ð
Table XV: Chemical resistance of commonly used elastomer gaskets and sealing materials
156
Tables, Formulas, Diagrams
Vacuum symbols
All symbols wit the exception of those marked with**) do not depend on the
position.
**) These symbols may only be used in the position shown here (tip of the
angle pointing down)
The symbols for vacuum pumps should always be arranged such that the
side with the constriction is allocated to the higher pressure
Vacuum pumps
Axial flow vacuum pump Condensate trap with heat exchanger (e.g. cooled)
Table XVI: Symbols used in vacuum technology (extract from DIN 28401)
157
Tables, Formulas, Diagrams
Sorption trap
Throttling
Modes of operation
Manual operation
Table XVI: Symbols used in vacuum technology (extract from DIN 28401) (continuation)
158
Tables, Formulas, Diagrams
Intersection of two lines without connection Vacuum gauge with analog measured-value display **)
Table XVI: Symbols used in vacuum technology (extract from DIN 28401) (continuation)
159
Tables, Formulas, Diagrams
Conversion in
K ¡C ¡R ¡F ¡R
Kelvin Celsius RŽaumur Fahrenheit Rankine
K 4 9 9
1 K Ð 273 (K Ð 273) (K Ð 273) + 32 K = 1,8 K
Kelvin 5 5 5
¡C 4 9 9
¡C + 273 1 á ¡C á ¡C + 32 (¡C + 273)
Celsius 5 5 5
¡C
RŽaumur
5
4
á ¡R + 273
5
4
á ¡R 1
9
4
á ¡R + 32
5
9 [ 54 (¡R + 273) ]
¡F 5 (¡F Ð 32) + 273 5 (¡F Ð 32) 4 (¡F Ð 32) 1 ¡F + 460
Fahrenheit 9 9 9
¡R
Rankine
5 (¡R)
9
5 (¡R Ð 273)
9
4
5 [ 59 (¡R Ð 273) ] ¡R Ð 460 1
Table XVII: Temperature comparison and conversion table (rounded off to whole degrees)
Ð p2
Mean free path λ [cm]
2
Z
Ðp
ZA
λ~ 1
p
Pressure p [mbar]
Pressure p [mbar]
λ : mean free path in cm (λ ~ 1/p)
n : particle number density in cmÐ3 (n ~ p)
ZA : area-related impingement rate in cmÐ3 á sÐ1 (ZA ~ p2)
ZV : volume-related collision rate in cmÐ3 á sÐ1 (ZV ~ p2)
Fig. 9.1: Variation of mean free path λ (cm) with pressure for various gases Fig. 9.2: Diagram of kinetics of gases for air at 20 ¡C
160
Tables, Formulas, Diagrams
106
105
104
Pressure [mbar]
Temperature (K)
conductance [l á cmÐ1]
103
102
1018
Altitude [km] 6
4
2
Fig. 9.3: Decrease in air pressure (1) and change in temperature (2) as a function of altitude
100 2 4 6 8102
101 103 104
Pipe length l [cm]
Fig. 9.5: Conductance values for piping of commonly used nominal width with circular cross-
section for laminar flow (p = 1 mbar) according to equation 53a. (Thick lines refer to
preferred DN) Flow medium: air (d, l in cm!)
conductance [l á sÐ1]
Altitude (km)
161
Tables, Formulas, Diagrams
pSTART Ð pend, P
R=
pEND Ð pend, P pEND – pend, p
mbar
Column ➀: Vessel volume V in liters Example 1 with regard to nomogram 9.7: Example 2 with regard to nomogram 9.7:
Column ➁: Maximum effective pumping speed Seff,max at the
vessel in (left) liters per second or (right) cubic A vessel with the volume V = 2000 l is to be pumped down A clean and dry vacuum system (qpV,in = 0) with V = 2000 l (as
meters per hour. from a pressure of pSTART = 1000 mbar (atmospheric in example 1) is to be pumped down to a pressure of
pressure) to a pressure of pEND = 10-2 mbar by means of a pEND = 10-2 mbar. Since this pressure is smaller than the
Column ➂: Pump-down time tp in (top right) seconds or
rotary plunger pump with an effective pumping speed at the ultimate pressure of the rotary piston pump (Seff,max = 60 m3/h
(center left) minutes or (bottom right) hours.
vessel of Seff,max = 60 m3/h = 16.7 l á s-1. The pump-down time = 16.7 l ( s-1 = 3 á 10-2 mbar), a Roots pump must be used in
Column ➃: Right: can be obtained from the nomogram in two steps: connection with a rotary piston pump. The former has a
Pressure pEND in millibar at the END of the pump- starting pressure of p1 = 20 mbar, a pumping speed of
down time if the atmospheric pressure 1) Determination of τ: A straight line is drawn through Seff,max = 200 m3/h Ð 55 l á s-1 as well as pult,p Ð 4 á 10-3 mbar.
pSTART ( pn = 1013 prevailed at the START of the V = 2000 l (column ➀) and Seff = 60 m3/h-1 = 16.7 l á s-1 From pstart = 1000 mbar to p = 20 mbar one works with the
pump-down time. The desired pressure pEND is to (column ➁) and the value t = 120 s = 2 min is read off at the rotary piston pump and then connects the Roots pump from
be reduced by the ultimate pressure of the pump intersection of these straight lines with column ➂ (note that p1 = 20 mbar to pEND = 10-2 mbar, where the rotary piston
pult,p and the differential value is to be used in the the uncertainty of this procedure is around ∆τ = ± 10 s so pump acts as a backing pump. For the first pumping step one
columns. If there is inflow qpV,in, the value that the relative uncertainty is about 10 %). obtains the time constant τ = 120 s = 2 min from the
pend Ð pult,p Ð qpV,in / Seff,max is to be used in the nomogram as in example 1 (straight line through V = 2000 l,
columns. 2) Determination of tp: The ultimate pressure of the rotary Seff = 16.7 l á s-1). If this point in column ➂ is connected with
Left: pump is pult,p = 3 á 10-2 mbar, the apparatus is clean and the point p1 - pult,p = 20 mbar Ð 3 á 10-2 mbar = 20 mbar (pult,p
Pressure reduction ratio R = (pSTART Ð pult,p Ð leakage negligible (set qpV,in = 0); this is pSTART Ð pult,p = is ignored here, i.e. the rotary piston pump has a constant
qpV,in / Seff,max)/(pend Ð pult,p Ð qpV,in / Seff,max), if 10-1 mbar Ð 3 á 10-2 mbar = 7 á 10-2 mbar. Now a straight line pumping speed over the entire range from 1000 mbar to 20
the pressure pSTART prevails at the beginning of is drawn through the point found under 1) τ = 120 s (column mbar) in column 5, one obtains tp,1 = 7.7 min. The Roots
the pumping operation and the pressure is to be ➂) and the point pEND Ð pult,p = 7 á 10-2 mbar (column ➄) and pump must reduce the pressure from p1 = 20 mbar to
lowered to pEND by pumping down. the intersection of these straight lines with column ➃ pEND = 10-2 mbar, i.e. the pressure reduction ratio
tp = 1100 s = 18.5 min is read off. (Again the relative R = (20 mbar Ð 4 á 10-3 mbar) / (10-2 mbar-4 á 10-3) =
The pressure dependence of the pumping speed uncertainty of the procedure is around 10 % so that the 20/6 á 10-3 mbar = 3300.
is taken into account in the nomogram and is relative uncertainty of tp is about 15 %.) Taking into account
expressed in column ➄ by pult,p. If the pump an additional safety factor of 20 %, one can assume a pump- The time constant is obtained (straight line V = 2000 l in
pressure pult,p is small in relation to the pressure down time of column ➀, Seff = 55 l á sÐ1 in column ➁) at = 37 s (in column
pend which is desired at the end of the pump- tp = 18.5 min á (1 + 15 % + 20 %) = 18.5 min á 1.35 = 25 min. ➂). If this point in column ➂ is connected to R = 3300 in
down operation, this corresponds to a constant column ➄, then one obtains in column ➃ tp, 2 = 290 s =
pumping speed S or Seff during the entire 4.8 min. If one takes into account tu = 1 minfor the changeover
pumping process. time, this results in a pump-down time of tp = tp1 + tu + tp2 =
7.7 min + 1 min + 4.8 min = 13.5 min.
Fig. 9.7: Nomogram for determination of pump-down time tp of a vessel in the rough vacuum pressure range
162
Tables, Formulas, Diagrams
Tube diameter
Example: What diameter d must a 1.5-m-long pipe have so example d/l = 0.16 and α = 0.83 (intersection point of the
that it has a conductance of about C = 1000 l / sec in the straight line with the a scale). Hence, the effective
region of molecular flow? The points l = 1.5 m and conductance of the pipeline is reduced to
C = 1000 l/sec are joined by a straight line which is extended C á α = 1000 á 0.83 = 830 l/sec. If d is increased to 25 cm,
to intersect the scale for the diameter d. The value d = 24 cm one obtains a conductance of 1200 á 0.82 = 985 l / sec
is obtained. The input conductance of the tube, which depends (dashed straight line).
on the ratio d / l and must not be neglected in the case of
short tubes, is taken into account by means of a correction
factor α. For d / l < 0.1, α can be set equal to 1. In our
Fig. 9.8: Nomogram for determination of the conductance of tubes with a circular cross-section for air at 20 ¡C in the region of molecular flow (according to J. DELAFOSSE and G. MONGODIN: Les
calculs de la Technique du Vide, special issue ÒLe VideÓ, 1961).
163
Tables, Formulas, Diagrams
C
Air 20 ¡C
Pressure [mbar]
Tube length [meters]
conductance [ l á sÐ1]
Laminar flow
Procedure: For a given length (l) and internal diameter (d), Example: A tube with a length of 1 m and an internal diameter In a tube with a length of 1 m and an internal diameter of 5 cm
the conductance Cm, which is independent of pressure, must of 5 cm has an (uncorrected) conductance C of around 17 l/s a molecular flow prevails if the mean pressure p in the tube is
be determined in the molecular flow region. To find the in the molecular flow region, as determined using the < 2.7 á 10-3 mbar.
conductance C* in the laminar flow or Knudsen flow region appropriate connecting lines between the ÒlÓ scale and the ÒdÓ To determine the conductance C* at higher pressures than
with a given mean pressure of p in the tube, the conductance scale. The conductance C found in this manner must be 2.7 á 10-3 mbar, at 8 á 10-2 mbar (= 6 á 10-2 torr), for example,
value previously calculated for Cm has to be multiplied by the multiplied by the clausing factor γ = 0.963 (intersection of the corresponding point on the p scale is connected with the
correction factor a determined in the nomogram: C* = Cm á α. connecting line with the γ scale) to obtain the true point d = 5 cm on the ÒdÓ scale. This connecting line intersects
conductance Cm in the molecular flow region: the ÒαÒ scale at the point α = 5.5. The conductance C* at
Cm á γ = 17 á 0.963 = 16.37 l/s. p = 8 á 10-2 mbar is: C* = Cm á α = 16.37 á 5.5 = 90 l/s.
Fig. 9.9: Nomogram for determination of conductance of tubes (air, 20 ¡C) in the entire pressure range.
164
Tables, Formulas, Diagrams
Example 2
ple 1
Exam
Gas evolution [mbar á l á sÐ1 á mÐ2]
weak
normal
strong
Area F [m2]
The nomogram indicates the relationship between the nominal connected via a vertical line to the curve that is based on the 8 á 10-5 mbar á l á s-1 á m-2 is to be evacuated from 10 mbar to
pumping speed of the pump, the chamber volume, size and pumping speed of the pump of 1300 m3/h (D). If the projection 10-3 mbar within a time of 10 min. The nomogram shows that
nature of the inner surface as well as the time required to to the curve is within the marked curve area (F), the pumping in this case a pump with a nominal pumping speed of
reduce the pressure from 10 mbar to 10-3 mbar. speed of the pump is adequate for gas evolution. The relevant 150 m3/h is appropriate.
pump-down time (reduction of pressure from 10 mbar to
Example 1: A given chamber has a volume of 70 m3 and an 10-3 mbar) is then given as 30 min on the basis of the line
inner surface area of 100 m2; a substantial gas evolution of connecting the point 1300 m3/h on the pumping speed scale
2 á 10-3 mbar á l á s-1 á m-2 is assumed. The first question is to to the point 70 m3 (C) on the volume scale: the extension
decide whether a pump with a nominal pumping speed of results in the intersection point at 30 min (E) on the time scale.
1300 m3/h is generally suitable in this case. The coordinates
for the surface area concerned of 100 m2 and a gas evolution In example 2 one has to determine what pumping speed the
of 2 á 10-3 mbar á l á s-1 á m-2 result in an intersection point A, pump must have if the vessel (volume = approx. 3 m3) with a
which is joined to point B by an upward sloping line and then surface area of 16 m2 and a low gas evolution of
Fig. 9.10: Determination of pump-down time in the medium vacuum range taking into account the outgasing from the walls
165
Tables, Formulas, Diagrams
1000
1,00E+03
Mercury
100
1,00E+02
Halocarbon 11
10
1,00E+01
Halocarbon 12
Vapor pressure [mbar]
Halocarbon 13 1,00E+00 1
Santovac 5
(similar to Ultralen)
Halocarbon 22 10-1
1,00E-01
Aziepon 201
Trichorethylene
10-3
Acetone 1,00E-03
DC 704 Diffelen ultr a
10-4
1,00E-04
10-5
1,00E-05
1,00E-06 -6
10 DC 705
1,00E-07-7
10
Diffelen
light
Temperature [¡C] 1,00E-08-8
10
Diffelen
normal
1,00E-09-9
10
Fig. 9.11: Saturation vapor pressure of various substances
10 -10
1,00E-10
10-11
1,00E-11
10-12
1,00E-12
Fig. 9.12: Saturation vapor pressure of pump fluids for oil and mercury fluid entrainment pumps
Temperature [¡C]
Temperature [K]
Vapor pressure
Fig. 9.13: Saturation vapor pressure of major metals used in vacuum technology
166
Tables, Formulas, Diagrams
Vapor pressure [mbar]
p critical point
P melting point
Temperature [¡C]
Fig. 9.14: Vapor pressure of nonmetallic sealing materials (the vapor pressure curve for fluoro Fig. 9.15: Saturation vapor pressure ps of various substances relevant for cryogenic technology in
rubber lies between the curves for silicone rubber and Teflon). a temperaturerange of T = 2 Ð 80 K.
Turbomolecular pump
Diffusion pump
Adsorption pump
submilation pump
Sputter-ion pump
Cryopump
10Ð14 10Ð13 10Ð12 10Ð11 10Ð10 10Ð9 10Ð8 10Ð7 10Ð6 10Ð5 10Ð4 10Ð3 10Ð2 10Ð1 100 101 102 103
p in mbar →
Working range for special model or special operating data Normal working range
167
Tables, Formulas, Diagrams
Pressure balance
Magnetron gauge
10Ð14 10Ð13 10Ð12 10Ð11 10Ð10 10Ð9 10Ð8 10Ð7 10Ð6 10Ð5 10Ð4 10Ð3 10Ð2 10Ð1 100 101 102 103
p in mbar →
The customary limits are indicated in the diagram.
168
Tables, Formulas, Diagrams
Saturated vapor
Fig. 9.17: Specific volume Vsp of saturated water vapor in m3/kg within a range of 0.013 to 133 mbar.
Fig. 9.18: Breakdown voltage U between parallel electrodes in a homogeneous electrical field as
a function of gas pressure p distance between electrodes d (in mm) (Paschen curve),
for air.
169
Tables, Formulas, Diagrams
SOLID LIQUID
Evaporation
Melting
Triple point
(0.01¡C, 6.09 mbar)
Water vapor pressure [mbar]
Sublimation
GASEOUS
Temperature [¡C]
170
Statutory units
171
Statutory units
172
Statutory units
173
Statutory units
174
Statutory units
3/10: Force
Conversions The dyne, the CGS unit for force, is no longer used.
1 kg á cm-2 = 980.665 mbar = 981 mbar
1 dyne = 10-5 N
1 at (technical atmosphere) = 980.665 mbar = 981 mbar
175
Statutory units
3/26: Angle
3/16: Standard volume
1 radian (rad) is equal to the plane angle which, as the central angle of a
DIN 1343 must be complied with.
circle, cuts out an arc having a length of 1 m from the circle. See also DIN
The designation m3 (NTP) or m3 (pn, Tn) is proposed, though the 1315 (8/82).
expression in parentheses does not belong to the unit symbol m3 but points
π
out that it refers to the volume of a gas in its normal state 1¡ = ÐÐÐÐÐ rad: 1Õ = 1¡/60; 1ÕÕ = 1Õ/60.
(Tn = 273 K, pn = 1013 mbar). 180
360¡
1 rad = ÐÐÐÐÐ á 60¡
3/17: Partial pressure 2π
The index ÒiÓ indicates that it is the partial pressure of the Òi-thÓ gas that is
contained in a gas mixture.
176
Statutory units
10.4.2 Derived coherent1 SI units with 10.4.4 Derived noncoherent SI units with
special names and symbols special names and symbols
(alphabetical)
Basic unit Symbol Definition
Name of unit Symbol Variable Relationship ÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑ
ÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑÑ
Day d 1 d = 86.400 s
coulomb C quantity of electricity 1C=1Aás
or electric charge Hour h 1 h = 3.600 s
Electron eV energy
volt
177
Vacuum technology standards
For around 20 years now, numerous standards and recommendations have 1304 General symbols
been drawn up at national and international level and revised, whenever Part 1 Ð General symbols 3/94
necessary, in accordance with the state of the art. These standards and Part 2 Ð Symbols for meteorology and geophysics 9/89
recommendations must be observed whenever use is made of vacuum Part 3 Ð Symbols for electrical energy supply 3/89
equipment (pumps, gauges, valves, etc.) and vacuum apparatus, systems Part 5 Ð Symbols for flow mechanics 9/89
and plants are assembled. They not only contain specifications applying Part 6 Ð Symbols for electrical
specially to vacuum technology, but also go beyond this specific field and communications technology 5/92
involve, for example, physical units, formulas, noise protection regulations, Part 7 Ð Symbols for meteorology and geophysics
etc. Part 7 Ð Symbols for electric machines 1/91
National standards are primarily DIN standards, particularly those relating 1305 Mass; weighed value, force, weight force, weight 1/88
to the area of vacuum technology in the DIN Standards Committee on load, definitions
Mechanical Engineering (NAM). International standards and
1306 Density; definitions 6/84
recommendations are drawn up and issued
1313 Physical variables and equations,
a) by the International Standardization Organization (ISO), in particular by
definitions, spelling 4/78
ISO Committee TC 112 (vacuum technology)
1314 Pressure; basic definitions, units 2/77
b) by the European Committee of Manufacturers of Compressors, vacuum
pumps and compressed air tools (PNEUROP), in particular by 1319 Basic definitions for measurement technology
PNEUROP Subcommittee C5 (vacuum technology) Part 1 Ð Basic definitions 1/95
Part 2 Ð Definitions for the use of gauges 1/80
c) by the European Committee for Standardization (CEN), in particular by
Part 3 Ð Definitions for measurement
Technical Committee TC 138 (nondestructive testing) and Technical
uncertainty and evaluation of gauges
Committee TC 318.
and measuring equipment 8/83
The content of the documents drawn up by the international organizations Part 4 Ð Treatment of uncertainty in the
in a) to c), with German participation (also by LEYBOLD), has been use of measurements 12/85
extensively incorporated into DIN standards, as reflected in designations
such as DIN / ISO or DIN / EN.
The most important standards to be complied with are listed in Table 11.1
below. A) National agreements, Part 1: DIN (cont.)
DIN Title Issue
178
Vacuum technology standards
8964 Circuit parts for refrigeration systems with 28410 Vacuum technology; mass spectrometer partial
hermetic and semi-hermetic compressors pressure gauges, definitions, characteristic
Part 1: Tests 3/96 variables, operating conditions 11/86
Part 2: Requirements 9/86
28411 Vacuum technology; acceptance specifications
(E 12/95)
for mass spectrometer leak detection devices,
16005 Overpressure gauges with elastic measuring definitions 3/76
element for general use Requirements
28416 Vacuum technology; calibration of vacuum
and testing 2/87
gauges in a range from 10-3 to 10-7 mbar.
16006 Overpressure gauges with Bourdon tube General methods; pressure reduction
Safety-related requirements and testing 2/87 through constant flow 3/76
19226 Ð 1 Control and instrumentation technology; 28417 Vacuum technology; measuring pV mass flow
control and regulation technology; according to volumetric method at constant
definitions Ð general principles 2/94 pressure 3/76
Ð 4 Control and instrumentation technology;
28418 Vacuum technology; standard method for
control and regulation technology;
calibrating vacuum gauges through direct
definitions for control and regulation
comparison with a reference device
systems 2/94
Part 1 Ð General principles 5/76
Ð 5 Control and instrumentation technology;
Part 2 Ð Ionization vacuum gauges 9/78
control and regulation technology;
Part 3 Ð Thermal conductivity vacuum gauges 8/80
functional definitions 2/94
28426 Vacuum technology; acceptance specifications
25436 Integral leak rate test of safety vessel with
for rotary piston vacuum pumps
absolute pressure method 7/80
Part 1 Ð Rotary piston and vane type rotary
28090 Static seals for flange connections vacuum pumps in rough and medium vacuum range
Part 1 - Characteristic values for seals and Part 2 Ð Roots vacuum pumps in medium
testing methods 9/95 vacuum range
Part 2 - Seals made of sealing plate; special
28427 Vacuum technology; acceptance specifications
testing methods for quality assurance 9/95
for diffusion pumps and ejector vacuum pumps for
28400 Vacuum technology; designations and definitions pump fluid vapor pressures of less than 1 mbar 2/83
Part 1 - Basic definitions, units, ranges,
28428 Vacuum technology; acceptance specifications
characteristic variables and basic principles 5/90
for turbo-molecular pumps 11/78
Part 2 - Vacuum pumps 10/80
Part 3 - Vacuum plants; characteristic 28429 Vacuum technology; acceptance
variables and gauges 6/92 specifications for getter-ion pumps 8/85
Part 4 - Vacuum coating technology 3/76
28430 Vacuum technology; measuring specifications for
Part 5 - Vacuum drying and vacuum
ejector vacuum pumps and ejector compressors.
freeze-drying 3/81
Pump fluid: water vapor 11/84
Part 6 - Analytical techniques for surface
technology 10/80 28431 Acceptance specifications for liquid
Part 7 - Vacuum metallurgy 7/78 ring vacuum pumps 1/87
Part 8 - Vacuum systems, components and
28432 Acceptance specifications for diaphragm
accessories 10/80
vacuum pumps E 5/95
(E 7/91)
53380 Testing of plastic foils, determination of gas
28401 Vacuum technology; symbols Ð overview 11/76
permeability 6/69
28402 Vacuum technology: variables, symbols, (E 10/83)
units - overview 12/76
45635 Noise measurement at machines: measurement
28403 Vacuum technology; quick connections, of airborne noise, enveloping surface methods.
small flange connections 9/86 Part 13 Ð Compressors, including vacuum pumps,
positive displacement, turbo and steam
28404 Vacuum technology: flanges, dimensions 10/86
ejectors 2/77
179
Vacuum technology standards
55350 Definitions of quality assurance and statistics 1607 / 2 Positive displacement vacuum pumps.
Part 11 Ð Basic definitions of quality assurance 8/95 Measurement of performance characteristics. 11/89
Part 18 Ð Definitions regarding certification of Part 2 - Measurement of ultimate pressure
results of quality tests/quality test certificates 7/87
1608 / 1 Vapor vacuum pumps.
66038 Torr Ð millibar; millibar Ð torr conversion tables 4/71 Part 1: Measurement ofvolume rate of flow 12/93
1593 E Nondestructive testing Ð bubble type testing method 12/94 3669 Vacuum Technology. Bakable flanges, dimensions. 2/86
Part 1: Clamped Type
NMP 826 Calibration of gaseous reference leaks, CD 9/95
Nr. 09Ð95 EN/ISO Rubber and plastic hoses and hose
4080 lines Ð determination of gas permeability 4/95
180
Vacuum technology standards
C) PNEUROP/C5 (6.93)
Number Title/remark identical Issue
to DIN
181
References
182
References
H. Adam F. Fauser
Vakuum-Technik in der Zeit nach Gaede (1945 to the present); Charakteristik von Pumpsystemen fŸr grš§ere Wasserdampfmengen unter
Pages 146-147 Vakuum und unter Anwendung von Kondensation und Kompression des
Wasserdampfes
G. Reich 1965 Transactions of the Third International Vacuum Congress, Stuttgart,
Die Entwicklung der Gasreibungspumpen von Gaede, Ÿber Holweck, Bd. 2/II, 393-395, Pergamon Press, Oxford 1966
Siegbahn bis zu Pfleiderer und Becker (mit zahlreichen Literaturangaben)
Vakuum-Technik in der Praxis, Vol. 4, 1992, 206-213 M. Wutz
Das Abpumpen von DŠmpfen mit gekŸhlten Kondensatoren
G. Reich Vakuum-Technik, 16, 1967, 53-56
Carl Hoffman (1844-1910), der Erfinder der Drehschieberpumpe
Vakuum in der Praxis, 1994, 205-208 H. Hamacher
Kennfeldberechnung fŸr Rootspumpen
Th. Mulder DLR FB 69-88, 1969
Blaise Pascal und der Puy de D™me Ð Gro§e MŠnner der Vakuum-Technik
Vakuum in der Praxis, 1994, 283-289 H. Hamacher
Beitrag zur Berechnung des Saugvermšgens von Rootspumpen
W. Pupp und H. K. Hartmann Vakuum-Technik, 19, 1970, 215-221
Vakuum-Technik, Grundlagen und Anwendungen
C. Hanser, MŸnchen, 1991, Wien, H. Hamacher
Experimentelle Untersuchungen an NachkŸhlern von Rootspumpen
Vakuum-Technik, 23, 1974, 129-135
M. Rannow
2. Vacuum pumps …lgedichtete Vakuumpumpen in der Chemie
Chemie-Technik, No. 7, 1978, 39-41
183
References
184
References
185
References
H. G. Nšller G. Kienel
Theory of Vacuum Diffusion Pumps Vakuumerzeugung durch Kondensation und durch Sorption
Handbook of Physics, Vol.1, Part 6, (pp. 323...419) Ed. A. H. Beck, Chemikerzeitung / Chem. Apparatur 91, 1967, 83-89 und 155-161
Pergamon Press Ltd., London, W.I. (1966)
H. Hoch
G. Herklotz Erzeugung von kohlenwasserstoffreiem Ultrahochvakuum
Enddruckversuche mit Diffusionspumpen hohen Saugvermšgens und Vakuum-Technik, 16, 1967, 156-158
Restgasspektren
Vakuum-Technik, 20, 1971, 11 Ð 14 W. BŠchler und H. Henning
Neuere Untersuchungen Ÿber den Edelgas-Pumpmechnismus von
H. G. Nšller IonenzerstŠuberpumpen des Diodentyps
Die Bedeutung von Knudsenzahlen und €hnlichkeitsgesetzen in Diffusions- Proc. of the Forth Intern. Vacuum Congress 1968, I. 365-368,
und Dampfstrahlpumpen Inst. of Physics, Conference Series No. 5, London
Vakuum-Technik, 26, 1977, 72-78
H. Henning
R. Gšsling Der Erinnerungseffekt fŸr Argon bei Trioden-IonenzerstŠuberpumpen
Treibmittelpumpen Vakuum-Technik, 24, 1975, 37-43
Vakuum-Technik, 1980, 163-168
M. Wutz
Grundlagen zur Bestimmung der charakteristischen Daten von 2.5 Cryopumps and cryoengineering
Dampfstrahl-Ejektorpumpen
Vakuum-Technik, 1982, 146-153 R. A. Haefer
Cryo-Pumping
H. Bayer 456 pages, 1989 Oxford University Press, Oxford
Dampfstrahlpumpen
Vakuum-Technik, 1980, 169-178 H. Frey und R-A. Haefer
Tieftemperaturtechnologie, 560 pages, VDI-Verlag, DŸsseldorf, 1981
H. Bayer
Vakuumerzeugung durch Dampfstrahl-Vakuumpumpen G. Klipping und W. Mascher
Vakuum in der Praxis, 1989, 127-135 Vakuumerzeugung durch Kondensation an tiefgekŸhlten FlŠchen, I.
Kryopumpen
Vakuum-Technik, 11, 1962, 81-85
186
References
187
References
M. H. Hablanian F. GrotelŸschen
Backstreaming Measurements above Liquid-Nitrogen Traps Das UHV-System bei DESY. 1. Teil
Vac. Sci. Tech., Vol. 6, 265-268, 1969 Vakuum in der Praxis, 4, 1991, 266-273
G. Kienel
4. Conductances, flanges,
Probleme und neuere Entwicklungen auf dem Ultrahochvakuum-Gebiet
VDI-Zeitschrift, 106, 1964, 777-786
valves, etc.
M. Knudsen
G. Kienel und E. Wanetzky
Gesetze der Molekularstršmung und der inneren Reibungsstršmung der
Eine mehrmals verwendbare Metalldichtung fŸr ausheizbare
Gase durch Ršhren
Uktrahochvakuum-Ventile und Flanschdichtungen
Annalen der Physik, 4th issue, 28, 1909, 75-130
Vakuum-Technik, 15, 1966, 59-61
P. Clausing
H. G. Nšller
†ber die Stršmung sehr verdŸnnter Gase durch Ršhren von beliebiger
Physikalische und technische Voraussetzungen fŸr die Herstellung und
LŠnge
Anwendung von UHV-GerŠten.
Annalen der Physik, 5th issue, 12, 1932, 961-989
ãErgebnisse europŠischer Ultrahochvakuum ForschungÒ
LEYBOLD-HERAEUS GmbH u. Co., in its own publishing house, Cologne
W. Ršllinger
1968, 49-58
Die Verwendung von Klammerflanschen in der Vakuumtechnik
Vakuum-Technik, 13, 1964, 42-45
W. BŠchler
Probleme bei der Erzeugung von Ultrahochvakuum mit modernen Vakuum-
H. Hoch
pumpen. ãErgebnisse europŠischer Ultrahochvakuum ForschungÒ
Ausheizbare Verbindungen an Hochvakuum-Apparaturen
Vakuum-Technik, 10, 1961, 235-238
Leybold-Heraeus GmbH u. Co., in its own publishing house, Cologne 1968,
139-148
W. BŠchler und I. Wikberg
Dual Seal Bakable Section Valves of the CERN Intersection Storage Ring
P. Readhead, J. P. Hobson und E. V. Kornelsen
Vacuum, 21, 1971, 457-459
The Physical Basis of Ultrahigh Vacuum
Chapman and Hall, London, 1968
K. Teutenberg
UHV-Ganzmetallventile gro§er Nennweite
E. Bergandt und H. Henning
Vakuum-Technik, 21, 1972, 169-174
Methoden zur Erzeugung von Ultrahochvakuum
Vakuum-Technik, 25,1970, 131-140
H. Henning
The approximate calculation of transmission probabilities
H. Wahl
Vacuum, 28, 1978, No. 3, Seite 151
Das Hochvakuumsystem der CERN am 450 GeV Supersynchrotron und
Speichering (SPS)
G. KŸhn
Vakuum in der Praxis, 1989, 43-51
Gasstršme durch Spalte im Grobvakuum
Vakuum-Technik, 33, 1984, 171-175
188
References
189
References
A. J. B. Robertson
6. Pressure monitoring, Mass Spectrometry
control and regulation Methuen & Co, Ltd., London, 1954
H. Dohmen J. Backus
Vakuumdruckmessung und -Regelung in der chemischen Chap. 11 in ãCharacteristics of Electrical Discharges in Magnetic FieldsÒ
Verfahrenstechnik National Nuclear Energy Series, Div. I, Vol. 5, McGraw-Hill Book Company
Vakuum in der Praxis, 6,1994, 113-115 Inc., New York, 1949
N. Pšchheim J. Backus
Druckregelung in Vakuumsystemen University of California Radiation Laboratory Report, RL 20.6.36, Mar. 1945.
Vakuum in Forschung und Praxis, 7, 1995, 39-46
190
References
191
References
192
References
S. Sotier M. MŸhlloff
Schwingquarz-Schichtdickenmessung Vakuumgerechte Werkstoffe und Verbindungstechnik, Part 3
Vakuum in der Praxis 1992, 182-188 Vakuum in der Praxis, 2, 1990, 179-184
W. Espe
Synthetische Zeolithe und ihre Verwendung in der Hochvakuumtechnik
Experimentelle Technik der Physik, XII, 1964, 293-308
H. Adam
Allgemeiner †berblick Ÿber die Werkstoffe der Vakuumtechnik und deren
Auswahl
Haus der Technik Vortragsveršffentlichungen ãWerkstoffe und
Werkstoffverbindungen in der VakuumtechnikÒ H. 172, Vulkan-Verlag, Dr.
W. Classen, Essen, 1968, 4 Ð 13
K. Verfu§
Bessere OberflŠchenvergŸtung durch Elektropolieren Ð am Beispiel der
Vakuum-Technik
VDI-Berichte, 183, 1972, 29-34
K. Verfu§
Schwei§en und Hartlšten
Haus der Technik, Vortragsveršffentlichungen ãWerkstoffe und Werkstoffver-
bindungen in der Vakuumtechnik, H. 172
Vulkan-Verlag Dr. W. Classen, Essen, 1968, Seiten 39 -49
Chr. Edelmann
Gasabgabe von Festkšrpern im Vakuum
Vakuum-Technik, 38, 1989, 223-243
R. Fritsch
Besonderheiten vakuumdichrter Schwei§verbindungen
Vakuum-Technik, 38, 1989, 94-102
H. Henning
Vakuumgerechte Werkstoffe und Verbindungstechnik, Part 1
Vakuum in der Praxis, 2, 1990, 30-34
R. Fritsch
Vakuumgerechte Werkstoffe und Verbindungstechnik, Part 2
Vakuum in der Praxis, 2, 1990, 104-112
193
Index
194
Index
Derived coherent and not coherent SI units with special Gas dependent pressure reading, vacuum gauges with . . . . . . . . . . . . .81
names and symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .177 Gas discharge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .51, 83
Detection limit (leak detectors) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .117 Gas independent pressure reading, vacuum gauges with . . . . . . . . . . . .77
Determination of a suitable backing pump . . . . . . . . . . . . . . . . . . . . . . .69 Gas laws . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .13
Determination of pump down time from Nomograms . . . . . . . . . . . . . . . .70 Gas locks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .75
Determination of pump sizes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .66 Gas sorption (pumping) of vacuum gauges . . . . . . . . . . . . . . . . . . . .83, 84
DI series diffusion pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42 Gas storage in the oil of rotary vane pumps . . . . . . . . . . . . . . . . . . . . .117
Diaphragm contoller, examples of application . . . . . . . . . . . . . . . . . .91, 92 Gaskets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .73, 154, 155, 156
Diaphragm vacuum gauges . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .77 Gay-Lussac's law . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .13
Diaphragm vacuum pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .20 General gas constant (Molar gas constant) . . . . . . . . . . . . . . . . .9, 14, 148
DIAVAC diaphragm vacuum gauge . . . . . . . . . . . . . . . . . . . . . . . . . . . . .77 Getter pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50
DIFFELEN, light, normal, ultra . . . . . . . . . . . . . . . . . . . . . . . . . . . .44, 166 Glass coating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .137
Diffusion / vapor-jet pumps, Instructions for operation . . . . . . . . . . . . . .144 Halogen leak detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .116, 191
Diffusion pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .41 Helium leak detectors with 180¡ sector mass spectrometer . . . . . .114, 115
Diode-type sputter ion pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .52 Helium spray equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .122
Direct-flow leak detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .120 Helium standard leak rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .112
Discharge filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .38 High frequency vacuum test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .115
Displacement pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19, 20, 182 High pressure ionization vacuum gauge . . . . . . . . . . . . . . . . . . . . . . . . .86
DIVAC vacuum pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .20 High vacuum range . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .67, 68
DKD (Deutscher Kalibrierdienst) German calibration service . . . . . . . . . .87 HLD 4000 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .116
Dry compressing rotary displacement pumps . . . . . . . . . . . . . . . . . . . . .27 HO-factor (diffusion pumps) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42
Dry processes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .62 Hot cathode ionization vacuum gauge . . . . . . . . . . . . . . . . . . . . . . . . . .84
Drying of paper . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .72 HY.CONE pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .49
Drying processes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .64 Hybrid ball bearings (Ceramic ball bearings) . . . . . . . . . . . . . . . . . . . . .47
Drying processes, selection of pumps for . . . . . . . . . . . . . . . . . . . . . . . .71 Hydrocarbon-free vacuum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .44, 65
DRYVAC-Pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33 IC 5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131
D-Tek . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .116 Ideal gas law . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9, 13
Duo seal (sealing passage) . . . . . . . . . . . . . . . . . . . . . . . . . . . .20, 21, 22 Impingement rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .12
Dust separator (dust filter) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .38 Industrial leak testing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .124
Dynamic expansion method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .88 Influence of magnetic / electrical fields . . . . . . . . . . . . . . . . . . . . . . . . .146
ECOTEC II . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .119 Internal compression (claw pumps) . . . . . . . . . . . . . . . . . . . . . . . . . . . .32
Effective pumping speed . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .38, 67 Inside-out leak . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .112
Elastomer gaskets . . . . . . . . . . . . . . . . . . . . . . . . . . . . .74, 154, 155, 156 Integral leak rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .113
Electrical break down voltage(Paschen curve air) . . . . . . . . . . . . . . . . .169 Internal reflow (roots pumps) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28
Electron beam evaporators (electron guns) . . . . . . . . . . . . . . . . . . . . . .134 Ion desorption effect . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .85
Envelope test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .122, 123 Ion sputter pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50, 51
Envelope test (concentration measurement) . . . . . . . . . . . . . . . . . . . . .123 Ionization vacuum gauge for higher pressures up to 1 mbar . . . . . . . . . .85
Evacuation in the rough / medium / high vacuum region . . . . . . .66, 67, 68 Ionization vacuum gauges . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .83
Evacuation of gases / vapors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .71 Ionization, specific (gas analysis) . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103
Evaluating spectra . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .102 Isotopes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .102
Expansion method static / dynamic . . . . . . . . . . . . . . . . . . . . . . . . . .87, 88 Kammerer compression vacuum gauge . . . . . . . . . . . . . . . . . . . . . . . . .79
Extractor ionization vacuum gauge . . . . . . . . . . . . . . . . . . . . . . . . . . . . .86 Kinetic gas theory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .13
Fast regeneration (partial regeneration) . . . . . . . . . . . . . . . . . . . . . . . . .58 Kinetic of gases, diagram of . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .160
Fingerprint . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103 Kinetic of gases, formulas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .148
Flanges and their seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .73, 187 Knudsen flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .15
Floating zero-point suppression . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .117 Krypton 85 test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .115
Fluid entrainment pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .40, 185 Laminar flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .15
Foam spray leak test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .115 Langmuir-Taylor-effect . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .117
Fractionation of pump fluids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42 Laval nozzle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .43
Fragment distribution pattern . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103 Leak detection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .110, 190
Fundamental pressure measurement methods . . . . . . . . . . . . . . . . . . . .87 Leak detection using Helium leak detectors . . . . . . . . . . . . . . . . . . . . .122
Gas analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .95, 106, 107, 190 Leak detection without leak detector . . . . . . . . . . . . . . . . . . . . . . . . . . .113
Gas ballast . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .24, 25, 117 Leak detection, leak test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .110
Gas composition as a function of altitude . . . . . . . . . . . . . . . . . . . . . . .161 Leak detectors with 180¡ sector mass spectrometer . . . . . . . . . . . . . . .119
Gas constant, general (molar) . . . . . . . . . . . . . . . . . . . . . . . . . . .9, 14, 149 Leak detectors with mass spectrometer . . . . . . . . . . . . . . . . . . . .116, 190
Gas density . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9 Leak detectors with quadrupole mass spectrometer . . . . . . . . . . . . . . .119
195
Index
196
Index
197
Index
198