Furnace handbook

General information
The tube furnace of the MMS laboratory facility is located near the cleanroom pass
thru, directly in front of the hallway window and chase door. It is a resistive heating
quartz tube furnace and is approximately 6.5 feet tall, excepting exhaust ducts, 5 feet
wide and 10 feet long. There are two exhaust ducts, one toward the rear of the furnace
over the attached gas cabinet, and a second at the front-end skimmer, which exhausts
process gases from a flue at the mouth of each tube.
Both 120 VAC and 240 VAC power is supplied to the tube furnace. The former
supplies power to the controllers, cooling fans and exhaust fans. The latter supplies the
power to the heaters.
The wall facing the chase door behind the furnace contains a large gas panel,
which supplies process gases to the tubes. The 5th tubes gas panel is inside the
cabinet. All tube furnace gases are provided through the bulkhead panel below the
main gas panel, as is the furnace cooling water.
Temperature control is achieved by operation of the Proportional-IntegratingDifferentiating (PID) controllers along the length of the tube furnace. Each set of four
controllers operates a single tube.
Although the tube furnace has spaces allotted for six tubes, only 5 of them are
operational. Each tube has an exclusive operation and is named accordingly: anneal
tube, phosphorus tube, dirty tube, oxidation tube, and boron tube. The dirty tube is
intended for a wide range of processes involving materials that would otherwise
contaminate the other tubes, such as organic materials and low melting point metals.
Looking at the front of the furnace, in clockwise direction starting from the upper right
the tubes are as follows: oxidation, boron, dead, dirty, phosphorus, anneal.

Anneal
Phosphorus
Dirty

Oxidation
Boron
Dead

The furnaces tubes are kept at standby temperatures and N 2 flow when they are not
in use. The standby temperature is 400oC. N2 flow is at 37 (6L/Min) read by the black
ball.
Utilization of higher standby temperatures decreases the life of the furnace heater
core windings. Do not completely shut off the heaters when the tubes are not in use.
Cycling of temperature from below 275C to above 1100C devitrifies (crystallizes) the
quartz tubes. Diffusion furnace tubes are manufactured using ultra-high purity and
totally amorphous SiO2. This material allows the furnace tubes to withstand extreme
temperatures and thermal gradients. They also provide a barrier to contaminants and
are considered "clean." Exercise extreme caution when working with the tubes and the
loading rods because they are very expensive.
The temperature read by digital temperature controllers is measured on the outside
of the tubes; the temperature inside the tubes may be different. A thermocouple in front
of the furnace tube may be used to calibrate the readers if necessary. All thermocouples
are of R type configuration.
The temperature controllers for the 1st, 2nd, 3rd are on the left side, and the 4th,
5th are on the right side. The 6th is not working and has no label on the controller. All
the others are labeled. The temperature controller has 3 control meters and 1 over heat
meter. The middle one is for control the temperature of the tube in its middle part, and
the left and right control meters are used to control the temperature difference on front
(mouth) and back of the tube compared with the middle part. The digital controller gives
both set temperature and measured temperature simultaneously. The over heat meter is
set to 1180oC. The controller will give an alarm and shut off the power of the tube if the
temperature of the tube is over it.
Do not operate the furnace at temperature over 1150 oC. If you really need a
temperature over 1150oC, talk to Michael R. Hansen. The tube will begin sagging if it is
operated above 1150oC (If it was not strengthened by rotating tube at install). The tube
will begin sagging above 1250oC even though being strengthened.
The quartz can get hot enough to severely burn even though it does not appear to
look any different than cool quartz. Quartz is also extremely expensive and can be
ruined by contamination. The worst thing is to spread contamination from, say a small
piece of burned glove on a boat, to the other quartzware, touch the loading rod in the
front side of the mark line and, consequently, to the wafers of other users.
The cooling water flowmeter and the gas flowmeter for all the five tubes are on the
right side at the back of the furnace bank. All the gas flowmeters except N 2 should be
turned completely off by turning the line valves beside or underneath the flowmeter; it is
not enough to adjust the flowmeters to no flow. The N 2 should be always on at 37
(6L/Min) read by the black ball when stand by.

The boron source wafers, actually boron nitride, are oxidized to form a B 2O3 layer
prior the doping run. It is this oxide that has a significant vapor pressure at the diffusion
temperatures. B2O3 reacts with silicon to form SiO2 with an extremely high concentration
of boron.
The wafers used for phosphorus doping are made with SiP 2O7 on a fine SiO2 matrix.
The SiP2O7 decomposes at diffusion temperatures to form P2O5 that vaporizes and
reacts with silicon.
There are 4 gases used in the furnace and each gas uses different flowmeter. The
gas flow rate is listed as following when the flowmeters is at full scale (150):
N2
O2
Ar-H2
HCl

24.145 L/Min read by black ball, 45.994 L/Min read by the white ball
7.59 L/Min
14.131 L/Min
17.59 L/Min

Operation Instruction
1. Verify that the specific tube you plan to use is at the proper temperature. The
temperature set and the temperature measured are different.
2. Check the cooling water flowmeter. It should be around 2.2.
3. Check that nitrogen is flowing into the tube and that the remaining gases are in
the correct conditions.
4. Put on the high temperature gloves over your gloves.
5. Open the door of the tube if it is closed.
6. Take off the cap of the tube and put it on the table.
7. Hook the boat in the tube to the mouth of the tube with the loading rod; never
touch the loading rod before the mark line on it. Using 30 second slowly pull the
boat in the condition that there are wafer on it. Every tube has its rod beside it in
the quartz storage tube, and do not change them. Allow the loading rod to cool
for several seconds before returning it to the quartz storage tube. It also helps to
use the end of the furnace tube as a fulcrum and pivot the hook upward as you
hook the boat. Avoid touching the wafers with the rod. Pulling too fast will result
in an abnormally high sheet resistance because a significant number of atoms
will be frozen off lattice sites, making them inactive.

Steps 8 to 15 are for the 3 wafer tubes.

8. Install the loading shelf on front of the furnace face according the marks on it.
9. Put the elephant on the shelf and enclose the tube inside it until the two legs of
the elephant set on the table of the tubes.
10. Hook boat from the mouth of the tube to the elephant.
11. Carefully unload the elephant and put it on the table of the furnace.
12. Unloading the boat using the rods and clamps.
13. Remove the high temperature gloves.
14. Do the load or unload work you needed. Hold the wafers in air for 10 seconds or
so to cool before placing them into the plastic wafer carriers. Although wafers

cool very fast, the quartz boat will retain heat and keep wafers hot for a relatively
long time.
15. Working at reversed steps and action from 14 to 4. When you push the boat into
the furnace tube, just push it as far as the mark line in the loading rod near the
mouth of the tube, not too far in, not too far out. The boat will be in the center of
the tube.

Steps 16 to 20 are for the 4 wafer tubes.

16. Insert the fingers of the fork into the holes on the boat.
17. Take the boat out of the tube by the fork and put it on the table.
18. Take the fork off the boat
19. Load or unload your samples
20. Load the boat back into the tube.
21. Put the cap on

Upon completion of your work, return the furnace to the standby

condition.

Gas Supply and Control

Nitrogen is supplied to every tube and is the gas to be flowed when the tube is idle.
The anneal tube can flow the following gases: nitrogen, argon-hydrogen, argon. The
phosphorus and dirty tubes both can flow nitrogen and oxygen. The oxidation and
boron tubes can both supply the following gases: nitrogen, argon-hydrogen, and
oxygen.
Gases supplied during processing and idle mode are controlled by use of the gas
panels at the back of the furnace. Each gas is fed from the bulkhead panel to a quarter
turn on/off valve and a rotometer. The rotometers should solely be used for metering
the flow, not for shutting down the flow; the quarter turn valves are intended for this
purpose. Gases for each tube are segregated on the panel by a vertical offset.
Each gas has a different type of rotometer on it and different maximum flow rates.
Each gas on the panel is labeled with the full-scale flow rate associated with its
rotometer. The flow rate is read from the center of the float. These full-scale flows
occur when the center of the metering float is positioned at the top of the rotometer
tube: the 150 mm line. There is no way of knowing the flow rate if the float is outside
the range of the tube markings. The oxygen gases all have maximum flow rates of 6.99
L/min at standard temperature and pressure (STP). The argon-hydrogen rotometers, as
well as the argon line, have maximum flow rates of 14.1 L/min STP. Finally, the nitrogen
lines have a maximum flow rate of 46.3 L/min STP. Appendix A contains copies of the
calibration sheets associated with the rotometers used in this system.
The nitrogen rotometers have two floats in a single tube. The black float is made of
glass and the metal float is stainless steel. Each float has an associated full scale flow
rate. The glass floats full-scale flow is 24.3 L/min and the stainless steel ball is 46.3
L/min at STP. This is done so that at low flow rates, the glass ball may be used to more
accurately meter the flow. The stainless steel ball float has the ability to run at flow rates
beyond the glass float flow range.

In order to prevent tube contamination, gases must always be flowing through the
system. When a process is not being run, nitrogen should be flowing through every
tube. The recommended flow rate is 6 L/min. This corresponds to a glass float value at
45 mm.

Temperature Control and Operation

The tube temperatures are controlled by a set of digital controllers located along the
sides of the tube furnace. Each set is contained in its own panel next to the breaker
switch that powers the tube. The set consists of three 2416 Eurotherm controllers and
one 2132 Eurotherm alarm controller. There is a green power indicator light next to the
tube breaker switch and a red alarm indicator light located below the 2132 Eurotherm
controller.
Tube temperature is controlled solely by the center 2416 Eurotherm controller. The
controller displays the set point value and the present value of the system by default. It
can be cycled to display the output percentage being called for by the controllers by
pressing the circle-arrow key. The current set point can be altered by pressing and
holding the up or down arrows until the desired set point is reached.
The left and right zones of the tube furnace are set to maintain a temperature
difference of 1 C from the center zone. These controllers are slaved off the center
zone and require no intervention from the user. They only serve as a means for the
user to determine if the tube has reached equilibrium and is stable across the three
zones.
The 2132 Eurotherm high temp alarm reads the temperature at the left and right
zones of the tube. If the temperature at either end exceeds the alarm temperature
setpoint, the alarm will trip and open the relay supplying power to the tube. The alarm
state is indicated by a flashing controller display and the red light will be lit. The alarm
cannot be acknowledged and power restored until after the tube has fallen below the
alarm set point. Once the temperature has fallen, the alarm may be acknowledged by
pressing the page and circle-arrow keys at the same time. Once the alarm has been
acknowledged, the breaker must be reset (toggled off if still in the on position, then
switched to on) in order to restore the power to the tube.
Currently, the alarm set point is 1180 C. This is set to ensure that the system is not
damaged in the event of a controller malfunction and to account for any discrepancies
between measured and actual temperature values. If higher process temperatures are
desired, contact the MMS Cleanroom Lab Specialist for more information.

Flowmeter Calibration Tables

Argon and oxygen supplied by manufacturer specs. Nitrogen flows calculated
based on air/nitrogen ratios and air data supplied by manufacturer.
Scale
Readings
150
140
130
120
110
100
90
80
70
60
50
40
30
20
10

Nitrogen
Flow [mL/min]
Glass / Stainless
24279 / 46250
22627 / 42917
20846 / 39182
19073 / 35968
17369 / 32371
15417 / 28884
13848 / 25730
12232 / 22701
10484 / 19488
8832 / 16369
6938 / 13282
5217 / 10267
3785 / 7420
2299 / 4774
809 / 2231

Argon
Flow [mL/min]

Oxygen
Flow [mL/min]

14131
13307
12375
11480
10581
9634
8643
7764
6805
5896
4886
3855
2940
1926
826

6992
6561
6131
5624
5168
4712
4231
3724
3268
2787
2280
1773
1267
735
228

Useful website
Dry oxidation calculator:
http://www.lelandstanfordjunior.com/dealgrove.html
Doping wafer
http://www.bn.saint-gobain.com