EXPERIMENT NO.

01

OBJECTIVE: TO DETERMINE THE CURIE TEMPERATURE (TC) OF THE GIVEN

FERRITE SAMPLE AND STUDY THE PERMEABILITY VARIATION IN THE VICINITY
OF CURIE TEMPERATURE.

INTRODUCTION:

Curie temperature is the temperature at which the ferromagnetic materials become

paramagnetic.

E.M.F. induced in secondary coils of a transformer is given, as per Faraday‟s Law, as

dB
VS  K (1)
dt
Where,
K: Constant dependent upon the geometrical factors and the turn ratio of the transformer.
B: The flux density depends on magnetizing field (H), which in turn is proportional to the
primary voltage (Vp) and permeability of the core (µ).

In the ferromagnetic state, the temperature dependence of Vs thus directly gives us the
temperature dependence of permeability. At Curie temperature (Tc) there would be a sudden
drop in the permeability of the material and hence a corresponding drop in Vs. So, the point at
which Vs starts decreasing defines the Curie temperature.

Figure 1: Schematic of the Curie Temperature setup.

At temperature exceeding Tc the materials is in the paramagnetic state where magnetic

susceptibility m (= µ-1) follows the Curie-Weiss Law:
 C
 m (T )  (2)
T  Tc

Where,
T is a temperature close to Curie temperature.

Equation (1) in the paramagnetic state can be rewritten as:

dH
VS  K 0  m
dt
dH
 K 0 (  m  1)
dt

For a sinusoidal magnetising current

VS  K 0H (1   m ) (3)

Where  is the angular frequency of magnetizing current.

Incorporating equation (2) in equation (3)
C
VS  K 0H (1  ) (4)
T  Tc

Thus a plot of Vs vs 1/T-Tc should be a straight line with µ0K H as intercept and µ0KHC as
slope.
Thus ratio of slope to intercept gives C. This fully characterizes the equation (2) which gives the
temperature dependence of permeability in the paramagnetic state.

EXPERIMENTAL PROCEDURE:

1. Connect the primary turns of the coil over a ferrite core (figure 1) to an oscillator output.
2. Read the induced e.m.f in the secondary turns with the help of an ac millivoltmeter.
3. Heat up the sample in an oil bath and note secondary output as temperature increases.
4. At curie temperature the output will show a sudden drop. Once the secondary coil output
starts to drop note the output for every 10C rise in temperature.
5. Repeat the observation of Tc during the cooling (after completing the observations of Vs
vs T and shutting off the heater power).
6. To note temperature accurately locate the bulb of the thermometer in the vicinity of the
sample. While reading V at varying temperature monitor current in primary turns and see
that it remains constant. If needed, keep adjusting it to a constant (preset) value.
CALCULATIONS AND RESULTS:

1. Plot Vs vs. temperature and deduce Tc.

2. Plot Vs vs. 1/T-Tc plot (for T > Tc) and determine its slope, intercept and their ratio C.

TABLE:

S. NO Temperature (◦c) Vs (mV)

Conclude your report by answering the following questions:

1. If the same experiment was to be performed employing a ferromagnetic core would any
modifications be required in terms of experimental procedure theory and results deduced.

2. Equation (3) suggests that secondary output would be higher for higher frequency of
magnetizing current. In this should we perform the experiment at very high frequencies
(say RF)? Are there any difficulties in doing so?

3. What does parameter C in equation (2) signify?

4. Did you observe Tc to be different between the heating and cooling process? If so, how
do you explain this difference?

5. Ask your instructor about the ferrite materials used in the experiment and write a
paragraph on it after studying reference materials.
 EXPERIMENT NO. 02

OBJECTIVE: TO STUDY THE COOLING CURVE OF A GIVEN Pb-Sn ALLOY AND

DETREMINE ITS COMPOSITION.

INTRODUCTION:

The knowledge of phase diagrams and accompanying solid state transformations is essential to
synthesize alloys of variable compositions and desired properties. A simple technique of
understanding phase diagrams is to study time vs. temperature curve of an alloy undergoing
cooling with a uniform rate. The resulting thermal curve reveals internal energy changes during
cooling.

Due to the release of internal energy difference of two phases (latent heat), the temperature does
not fall during solidification and a horizontal part in the thermal curve is obtained. When one of
the constituents of the alloy undergoes a first order thermodynamic transition (namely freezing)
and the other constituent remains as such, the temperature of the alloy will exhibit a change from
original slope depending on the relative percentage of the two constituents. Below is graph in
temperature (°C) and time (sec).

Figure 1: Cooling curve for a 2-phase alloy.

When temperature of the alloy falls to a value at which second constituent is also undergoing
first order changes, then thermal curve will again exhibit horizontal slope, or change in slope
depending upon whether in the meanwhile first component has, or, has not transformed its
structure completely. Hence study of thermal curve will reflect the phase transformations of
different constituents.

All phase transformations in alloys follows Gibbs phase rule.

For a binary alloy: degree of freedom = 4 – p. Where „p‟ denotes the number of phases. Degree
of freedom is equal to the number of variable parameters externally controllable – temperature,
pressure and composition. Usually one degree of freedom namely pressure, is fixed during
cooling as expt. is done at atmospheric pressure. The balance of degree of freedom are 3-p, thus
at point in phase diagram where three phases coexist the degree of freedom is zero (i.e. unique
composition and temperature). Two phases coexist over a range of temperatures.

The temperatures corresponding to points where changes in slope occur in the cooling curve (e.g.
points b,c in Fig. 1) depend on the composition of the alloy. Given a known phase diagram and
an experimentally obtained cooling curve these arrest points can be used to find composition of
the alloy.

Temperature of the alloy is measured using a potentiometer attached to a Copper-constantin

thermocouple which must be kept embedded in the alloy.

EXPERIMENTAL PROCEDURE:

1. The unknown alloy is put in an alumina or porcelain crucible and placed into the center
of the heating unit.
2. Before staring the heating run (temp) please ensure that the set temperature is set above
2500C.
3. After the set temperature is reached (Alloy is melted), switch off the heating.
4. The temperature readings are taken every 15-20 seconds.

CALCULATIONS AND RESULTS:

1. Plot the direct cooling curve and note the arrest points (temperature at which changes in
slope occur).
2. From the Pb-Sn phase diagram provided, estimate the composition of your sample.

TABLE:
Time interval: ______sec

S. No. EMF (mV)

Conclude your report by answering the following questions:

1. Did you get sharp arrest points? If not, explain the reason(s). Did you observe any dips in
the curve before the beginning of a horizontal portion of the curve? If so, why? What
phenomenon does it represent?

2. Under what conditions one may prefer to employ a heating curve rather than a cooling
curve to study an alloy.

3. Pb-Sn is used as a solder material. From the phase diagram can you infer what
composition would be optimal for soldering?

4. Inspect the Pb-Sn phase diagram and infer arrest points in cooling curves at various
compositions. At what composition the numbers of arrest points are minimum.

5. Do you expect a similar cooling curve for an alloy in vapor form undergoing
liquefaction?

6. Which thermocouple should be most suitable for the purpose of this experiment? Explain.
 EXPERIMENT NO. 3

OBJECTIVE: TO DETERMIE YOUNG‟S MODULUS, YIELD STRENGTH AND THE

ULTIMATE STRENGTH OF THE GIVEN STRAND OF FIBER.

INTRODUCTION:

This experiment employs Hook‟s Law to determine Young‟s Modulus of a thin fiber. Hook‟s
law states that when a body is subjected to a stress a corresponding strain is produced such that
the ratio between the stress and the strain is constant as long as the elastic limit is not exceeded.
For the determination of Young‟s modulus of high modulus fiber (e.g. glass fiber) filament, its
small cross section (less than mm) and the small change in length is required to be measured
precisely. This is accomplished in this experiment by employing a high magnification travelling
microscope with ability to measure fiber diameter up to 0.01 mm and fiber length up to 0.01 mm.

Figure1: Schematic of the experimental setup

EXPERIMENTAL PROCEDURE:

A) PREPARATION OF THE SAMPLE:

1. One end of the fiber to be used is glued to the lower part of a screw; other end is fixed to
metal strip attached to a weighing pan (see fig.).
 2. The sealing at the two ends can be affected by employing Araldite/Super Glue. If
applying Araldite it should be allowed to be cured for about 24 hours.
3. Mount the sample on the stand such that the screw holder is held tightly in the clamp.
4. Carefully level the sample so that fiber hangs vertically.
5. Focus the cross-wires of the microscope at the fiber. Now, the set up is ready to note
down the initial length and diameter of the fiber.

B) MEASUREMENT OF THE DIAMETER:

1. Note the least count of the micrometer scale for up-down motion and the lateral
movement. The latter is to be employed for measuring diameter of the fiber.
2. Though the microscope, view the fiber along its length and also by rotating the screw (see
fig.). You should notice that diameter may not be equal along the length and/or at
different orientations in view. Therefore, you need to make a number of observations for
the diameter.
3. Moving vertical cross-wire across the thickness of the fiber and noting the horizontal
distance moved on micrometer/vernier combination would give diameter of the fiber.
4. An average value of observed thickness of fiber may be taken to represent the effective
value of its diameter assuming fiber to be cylindrical in shape.

C) MEASUREMENT OF STRAIN

1. Focus the microscope at the position from where the fiber comes out of Araldite (A) and
read the corresponding position on the vertical scale of microscope. Likewise the position
corresponding to point where the hook for the pan is attached (C) is read.
2. The difference AC, is a measure of the original length of the fiber.
3. Introduce a weighing pan (Weight of the pan: ____ g), this will be your first reading.
Now gradually add weight in the pan (10 g); each time noting the increased length by
reading lowered position corresponding to the end C of the fiber.
4. One can determine strain on the fiber for various loadings. As the fiber elongates, point C
lowers by an amount equal to extension in total length. Since the edge B, (i.e. edge of
strip next to the fiber end C) is close to the fiber end, the edge B would be lowered by
almost the same amount and therefore can served as proxy for C.
5. Noting the changes in position (lowering along vertical scale of edge B instead of point C
would thus give the extensions in fiber length corresponding to each loading. Edge B can
be more conveniently aligned with horizontal cross-wire instead of point C and thus
serves as a better bench-mark.
6. Record your observations relating the original length, diameter and changes in the length
corresponding to increasing loads and represent strain (l/l) against stress = (load/ A)
where, A = area of cross section of the fiber. Hence, compute the Young‟s modulus.
MEASUREMENT OF ULTIMATE STRENGTH:

1. The ultimate strength is related to the load at which fiber breaks. This can be done by
continuing to add weights in the pan and noting the load at which the fiber give in.
Corresponding stress gives ultimate strength.

CALCULATIONS AND RESULTS:

1. Plot the Stress-Strain curve.

2. From the graph calculate the Young‟s Modulus, Yield Strength and the Ultimate
Strength.

TABLES:

For Diameter:

S. No X◦ Xi ΔX(cm)

Diameter, d = _______ cm

Length, L= _______cm

For Young‟s Modulus:

S. No Weight (g) Force (N) Stress (N/m2) Δl (cm) Δl/l

Conclude your report by answering the following questions:

1. Compare your results for Young‟s modulus and ultimate strength against the
corresponding standard values (available from reference sources) and give your
inference.

2. List the significant sources of error in this experiment and estimate the overall percentage
error in the determination of Young‟s experiment.

3. Distinguish between engineering stress / strain and true stress / strain, which one was
employed in your data analysis?

4. The elongation noted in the experiment is not just the elongation in the fiber but also
includes elongation of the metallic support holding the fiber. In view of this suggests how
we may determine the true modulus of the fiber alone.

5. Young‟s modulus is one of a number of mechanical parameters characterizing a material.

What physical properties does Young‟s modulus measures?

6. From your determined values of Young‟s modulus(Y) and ultimate strength (S) calculate
the specific modulus (Y/density) and specific strength (S/density). What do these
numbers signify? Compare these numbers with corresponding numbers for a metal and
discuss.

7. Do you expect strength of a fiber to depend on its length? Explain your answer on the
basis of microstructure arguments.
 EXPERIMENT NO.: 04

OBJECTIVE: TO DETERMINE THE DIELECTRIC CONSTANT OF THE GIVEN PCB

LAMINATE.

INTRODUCTION:

Dielectric constant is one of the most basic electric parameters characterizing a dielectric
material. The experiment below describes the determination of the same for a parallel plate
capacitor by measurement of the discharge current of the capacitor.

The capacitance, C, of a parallel plate capacitor of plate area, A, and separation between the
electrodes, d, is given by:

C = 0r (A/d)
Where,
0: Permittivity of the free space = 8.85 x 10-12 F/m
r: Relative dielectric constant
Here the effect of fringing has been ignored.

If the capacitor is charged and discharged rapidly with a known frequency, n, the discharge
current measured by the ammeter is given by:

I = nQ = nCV
= n0rV (A/d)

It is assumed that capacitor is discharged completely each time.

Measurement of discharge current, I, and the dc charging voltage, V, allows us to calculate r .

r = (I/V)(d/An0)
EXPERIMENTAL SETUP:

In the present setup (Fig1) an inexpensive and commonly available electric buzzer working at
50Hz signalAmmeter
is employed for rapid charging and discharging of the capacitor. An ordinary low
resistance dc micro-ammeter reads the discharging current. A dc supply (0-30V) is used for
charging the capacitor. The vibrating hammer (made of iron) of the buzzer produces the buzzing
sound as it is attracted and repelled by the electromagnet at the input frequency. On both sides of
this hammer two screws are fixed so that it makes contact with the screws alternatively and as a
consequence the capacitor is charged and discharged continuously at the 50Hz.
EXPERIMENTAL PROCEDURE:

Note: Before switching on the power buttons make sure that the screws for charging and
discharging of the capacitor are not touching each other and the input of the dc power
supply is at zero.

1. Switch on the buzzer and the dc power supply.

2. Adjust the two screws such that the discharge current measured by the micro-ammeter is
stable for a constant charging voltage.
3. Note the value of discharge current (I) for various readings (at least 10) of charging
Voltage (V).

CALCULATIONS AND RESULTS:

1. Plot I vs V graph.
2. Using the best fit value from the graph find the value of r.

TABLE:

S. No. Charging voltage (V) Discharge current (A)

Conclude your report by answering the following questions:

1. How much error is being injected in the final result because of ignoring the fringing
effects?
2. Is it reasonable to assume that capacitor is discharged completely during the time of
circuit break-off.
3. Can we modify the set-up to compare dielectric constant of different solids? Can we
determine dielectric constant of liquids by this procedure? (In particular of water.)
4. Which is the prime source of error in this experiment? Which is the next important factor?
5. Which type of current measuring device would be an improvement over the moving coil
type ammeter employed here?
6. In case we want to investigate the degree to which the capacitor is discharged, how might
we go about it?
 EXPERIMENT NO.: 05

OBJECTIVE: TO CHECK THE LINEARITY OF UFD AND DETERMINE THE LOCATION

OF FLAWS IN THE GIVEN METALLIC SPECIMEN.

INTRODUCTION:

Nondestructive testing aims at testing/evaluating materials without impairing their service

ability. Obvious examples are the use of X-ray (transmission) and ultrasonic (reflection and/or
transmission) detection of cracks and voids within opaque bodies. Ultrasound is an ideal tool in
this regard because of the following reasons:

The acoustic impedance (v) of cracks is significantly different from that of the host material. Due
to impedance mismatch they strongly reflect ultrasonic waves (even extremely thin cracks are
very strong reflectors).

It is possible to generate short pulses (frequency 2-6 MHz) and narrow beams of ultrasound with
the help of piezoelectric transducers (PZT type).The reflected waves from echoes can be
received by the same transducer and detected. In flaw detection it is resolution rather than range
that is required and thus high frequencies are used.

Consider a specimen with two parallel plane surfaces with a probe mounted on one surface.
Suppose that the probe is connected via an amplifier, to the y-plates of an oscilloscope and that
the time-base of the oscilloscope is triggered at the moment when the probe launches a short
ultrasonic pulse in to the specimen. If the specimen contains no flaw, the pattern should appear
on the screen; the peak marked A corresponds to the original pulse while C corresponds to the
pulse reflected from the bottom of the specimen.

In order that the trace on the screen does not die away and to obtain a steady trace, the pulse will
have to be repeated at a rate greater than about 20Hz. However, the repetition rate must not be
too rapid, because it is desirable that the echo (or echoes) from any given pulse should be
received before the next pulse is emitted by the transducer.

The situation illustrated in the figure is rather an over simplification for in practice the echo C
will be followed by a train of further echoes corresponding to successive double transits of the
specimens thickness due to multiple reflections from top and bottom ends of the specimen. The
amplitude of these echoes will decay exponentially.

Let us suppose now that the specimen contains a flaw in the path of the beam. The will give
additional reflected pulse B which will be recorded on the screen between pulse A an C.

The whole specimen can be examined for further flaws by moving the probe all over the top
surface of the specimen and observing the echo pattern on the oscilloscope. From the trace on
CRO the location of defects (at depth d) in relation to the thickness of the test object can be
found by comparing time elapsed between return of reflected wave from flaw (t) and the bottom
(t`)

EXPERIMENTAL PROCEDURE:

1. In flaw detection it is necessary to maintain good acoustic contact between the probe and
the specimen. This is achieved by ensuring that the surface of the specimen is clean and
by maintaining a film of oil between the probe and the specimen; in addition to providing
good acoustic coupling, the film of liquid also act as a lubricant.
2. The location of a discontinuity can be easily determined with the help of echo, provided
previously a specific measuring range or, the testing range, has been displayed as
possible on the CRT screen.
3. The ultrasonic flaw detector 6255A generates short initiating pulses at regular intervals of
time. This output serves dual function: It first triggers the transmitter causing a larger part
of energy to excite the transducer at its natural frequency by virtue of its piezo-electric
properties. Secondly triggers the sweep circuit causing a spot on the CRT screen to move
from left to right with constant speed.
4. For a single transducer mode of operation, the transducer coaxial cable is connected to
connector marked T-R/T and the mode switch should be set at T-R. In this position, the
transducer not only gets exited by the electrical signal from the transmitter also converts
the reflected mechanical vibrations from the object. The surface of the object on which
the transducer is to be placed for inspection must not cause significant attenuation of the
sound waves transmitted from the transducer. Hence there should be a good acoustic
coupling between the probe face and test place surface. This achieved by smearing the
top surface of the test object with a high viscosity oil/ liquid.
5. A linearity check of the UFD should be made before proceeding with the testing. For this
purpose a flawless, 8 step standard steel samples is taken. Each step corresponds to 1 cm;
hence the last step is of 8 cm. A transducer is placed on the step block. The back (echo)
peak from the 8 cm step should be adjusted to coincide with 8 cm position of CRT
graticule. For this we make adjustments with the help of Mat. Cal coarse and Fine
 control. Now 8 cm of graticule corresponds to 8 cm of the step bloack. Hence the
corresponding steps should record the back echo at 7 cm, 6 cm, 5 cm, 4 cm, 3 cm, 2 cm
and 1 cm respectively. The positions of back peak for all steps should be noted and
compared with the expected positions. Next an aluminum block is taken, which has
certain known flaws in it. The back echo is adjusted such that it coincides the 10th cm
position on the graticule. The flaws will give rise to additional echoes in between the two
pulses i.e. starting peak at zero and back peak at 10th cm. Noting the echoes the
corresponding location (depth) of flaws can be noted. This can be verified against the
actual location (depth) of flaw can be noted. Tabulate the actual location Vs observed
location for each one flaw.

6. Now we are ready to try our hand at locating unknown flaws in a commercial
steel/aluminium sample. Here too the starting and back (echo) peak are aligned with 0th
and 10th cm location on graticule. We scan the surface of specimen with the probe and
see if there is any flaw peak. To ensure that no flaw is missed the appropriate Gain and
Attenuator is selected. The location of flaws so observed is noted as done in the earlier
aluminium block. Record the location (depth) of flaws observed and calculate the
percentage error.
TABLES:

Linearity (steel steps):

Scale:
8cm steel= ______cm on screen

1cm steel= ______cm on screen

S. No. Actual(cm) Observed

Flaw detection (For Al):

Scale: 20cm Al= ______cm on screen

1cm Al= ______cm on screen

S. No. Actual depth of Observed depth on Calculate depth % error

defect screen at defect
Complete your report by answering the following questions:

1. 20 KHz is the minimum frequency for ultrasonic. Is there any upper limit for frequency
of ultrasonic?
2. We are using 2 MHz transducer. What would be the benefit of using a transducer of
higher frequency?
3. What would happen if no coupling fluid is used? Are all coupling fluids equally
effective?
4. Under what conditions a normal probe is ineffective in locating flaws. What would be an
effective alternative in locating flaws?
5. Name other methods of finding flaws in opaque materials. State their principle(s) of
operation briefly.
 EXPERIMENT NO. 11

OBJECTIVE: TO DETERMINE FIBER AND VOID FRACTION OF A GLASS FIBER

REINFORCED COMPOSITE SPECIMEN.

Note: You would need refractory furnace operating at 800 0C in this experiment. Switch on the
furnace keeping temperature setting at 800 0C before beginning to read this write up. It may take
an hour before the furnace is ready to use.

Introduction : Fiber reinforced composites are a new class of engineering materials which offer
high specific strength, corrosion resistance and flexibility of design strength, corrosion resistance
and flexibility of design. They are made by mixing glass fiber strands with rosins and molding
the mixture to shape the composite. Molding is carried out under appropriate temperature and
pressure condition to effect proper curing. The fiber volume fraction plays a major role in
determining the engineering properties of fiber reinforced composites. Therefore it is important
to know the fiber fraction of a composite to characterize it. Some voids (unfilled spaces) in small
amounts inevitably remain in a composite. The voids tell on the mechanical and electrical
properties of a composite specimen.

One can relate volumes of fiber (Vf), resin or matrix (Vm) and voids (Vv) as:

Vf + Vm+ Vv = VT (1)

VT: total volume of the composite piece.

Also,

VT = l X b X h (2)

Where,
l, b and h is the dimension of the specimen.

We know,
WT = Wf + Wm (3)

Wf ,Wm and WT denote mass of fiber, mass of matrix and the total mass of composite specimen
respectively.

After burning at 800 ◦C

WB = Wf (4)
WB : weight of the specimen after burn.

So,
Wm = WT – WB (5)
The volume of the matrix and the fiber can calculate from:

Where:
M and F are the density of matrix and the density of the fiber respectively.

Densities of constituents are assumed to be known (As provided by manufacturers: f = 2.54

g/cc, m = 1.12 g/cc )

So the volume of the voids can be calculated from this equation:

Vv = VT – (Vf +Vm)

Void Fraction = (Vv/VT)

Fiber Fraction = (Vf/VT)

EXPERIMENTAL PROCEDURE:
Fiber and void fraction is determined most commonly by a burn out test:

1. In this a small specimen of composite known as (coupon) is cut and weighed.

2. Then its volume is determined by measuring its sides andthickness with an accurate
Vernier.

3. The specimen is then put in furnace (at about 800 0C) to combust and evaporate the
organic resin matrix leaving only the glass fiber component in it unaffected.

4. Weighing the fiber provides an estimate of mass of resin evaporated.

5. Equations (1) - (6) can now be employed to determine void and fiber fraction.

Note: The measurements of mass and volume are conceptually simple. However, the key to
accurate and reliable determination of Vv and Vf is correspondingly accurate
measurements of Vc, Wc, Wf .

The coupon usually weighs around one gram and has volume of less than 1ml. Fiber
mass in the coupon is quite clearly less than a gram. The mass of coupon and fibre
remaining after burn out should be measured using electrically operated alalytic balance
with the least count of 0.1 mg. Dimensions of coupon should be measured with
micrometer and venier with a least count of atleast 0.002 mm. A number of
measurements should be taken for thickness and each side of the coupon and average
taken to improve the accuracy of coupon volume. Show these observations and
calculation leading to the determination of Vv and Vf.
Conclude your report by answering the following questions:

1. Estimate the percentage accuracy in the measurement of thickness and volume of coupon,
mass of coupon and mass of fiber. Combine these to determine the uncertainty in
determination of Vv and Vf.

2. Can you suggest a substantially more accurate and sophisticated method of the
determination of coupon thickness.

3. Suggest how the method can be modified to determine Vv and Vf through the
measurement of density of coupon instead of measuring coupon volume.

4. Read reference material and write an outline of an alternative method to determine the
fiber and void fractions.
 EXPERIMENT NO.14

OBJECTIVE: TO INVESTIGATE CREEP OF A GIVEN WIRE AT ROOM

TEMPERATURE.

INTRODUCTION:
When a material is subjected to a load, deformation occurs leading to an increase in
length almost instantaneously. Under certain conditions, however, and particularly at high
temperature, if the applied load is retained for long periods, considerable additional deformation
may occur. The material may gradually deform plastically and ultimately even fracture at a stress
that is well below the ultimate tensile strength as determined by short time tensile testing. This
continuous slow extension under a constant stress is known as creep.

The standard creep test measures the strain or elongation of a loaded sample as a function
of time at a constant temperature. If a constant load is used, the stress will not, of course, remain
constant since the sample will undergo elongation. However, constant loading case merits
investigation as it is more representative of service conditions. Under optimum conditions, one
can observe three distinct stages of elongation during creep deformation in metals. These are
known as:

i) Primary Creep, ii) Secondary Creep and, iii) Tertiary Creep

At low temperatures and stress most metals show only primary creep. During the primary
creep period the rate of extension decreases with time. It remains steady during the secondary
creep stage. Tertiary creep is characterized by accelerating creep rate which eventually results in
fracture. The contribution of various stages to total creep deformation depends on the nature of
materials and the conditions of temperature and stress prevailing during the test. The creep
curves for any material are sensitive to both stress and temperature.
For metals the functional form of extension vs time for primary and secondary stages is

l  l0 (1  t 1 / 3 )e kt (1)

Where l is the length at any time t,

l0 is the length immediately after applying the load;
 and k are primary and secondary creep constants and are constant for any given stress
and temperature.

In order to verify equation (1); an experiment is to be performed for the determination of k. In

this experiment, we shall subject a thin Cu wire to a constant tensile load (≈10 N) and measure
time variation in extension with the help of a travelling microscope.

-
EXPERIMENTAL PROCEDURE:

1. Arrange the Cu wire provided to you, as per fig.2. Suspend a weight of about 2 Kg and
mark any point (at about 80 cm from the fixed end) on the wire.

2. Focus the cross wire of the microscope on the mark and note down the initial position on
 the horizontal vernier scale.

3. Now add a weight of about half Kg on the hook and start the stop watch. It is seen that
there is a measurable change in elongation.

4. Give support to the weight from below (by hand or jack) after about 10 seconds and note
down the change in the length on the horizontal scale.

5. Giving support to the load freezes extension enabling us to record the changes in the
length after small intervals of time of active load application.

6. Repeat the process after every ten seconds of the load application recording the
observations up to, say 60 seconds.

7. During this period, the elongation is considerable and represents the primary creep.
Beyond this region the elongation slows down.

8. Now take the observations of the extension after every 1 minute. Observe secondary
creep for 10-15 minutes.

9. Plot a graph between the elongation and time. The characteristics correspond to a general
equation. (Eq 1) which is the sum of the exponential curve (OA) and the linear one (AB).

DATA ANALYSIS

1. Determination of 

a. Slope in equation (1) is a constant and denotes transient flow.

b. In the primary creep region (OA), the variation of time is very small. Thus exp(kT)→1 in
equation (1).
c. So the equation (1) reduces to:

l  l0
 t 1 / 3
l0
d. Hence, Corresponding to each data point for the region OA compute (strain)3.
e. Plot it against time.
f. Slope of the curve would give 3.
g. Deretmine .

2. Determination of k

a. The constant k can be evaluated from the region AB, for which the product t1/3<<1.
b. Therefore, Eqn. (1) for region AB can be approximated as:

l = l0exp(kt)
 c. The plot between log(l) and time t is a linear one.
d. Determine the value of k from its slope. k is known as the rate of strain for the secondary
region.

3. Arrange your extension vs data systematically.

4. Show graphical plot mentioned before and give the resulting values of  and k (in proper
units).

l0 = _______ mm

S. No. time l (l-l0)/l

Conclude your report by answering the following questions:

1. What is the effect of prior deformation on creep strength of a material?

2. Discuss whether „freezing‟ creep at various intermediate times in the primary region (as
done in the experiments) affects the overall creep behavior?

3. How would creep strength change with the purity of the wire used?

4. Can we adopt this method to determine creep at higher temperatures?

5. Compare creep behavior in metals to corresponding behavior in ceramics and polymers.

 EXPERIMENT NO. 12

OBJECTIVE: TO ESTIMATE THE HALL COEFFICIENT, CARRIER CONCENTRATION

AND THEIR MOBILITY IN Ge CRYSTAL USING HALL EFFECT.

REQUIREMENTS: The Hall Effect set-up (digital) DHE-02, as shown giving block diagram in
fig. (2) Consist of the following components.

(i). (a) Hall probe (Ge crystal), (b) Hall probe (Indium Arsenide, for measuring magnetic field)

(ii). Digital millivoltmeter

(iii). Constant current power supply

(iv). Electromagnet, EMU-75

(v). Power supply, PS-75

(vi). Gauss meter, GM-101

INTRODUCTION:
The conductivity measurements cannot reveal whether one or both types of carriers in
semiconductors are present, nor can they distinguish between them. However, this information
can be obtained from Hall Effect measurement, which is basic tool for the determination of
mobilities. The effect was discovered by E.H. Hall in 1879.

THEORY:

A static magnetic field has no effect on charges unless they are in motion. When the charges
flow, a magnetic field directed perpendicular to the direction of flow produces a mutually
perpendicular force on the charges (Lorentz Force). When this happens, electrons and holes will
be separated by opposite forces. They will in turn produce an electric field known as Hall field
(EH).

In metals and heavily doped semiconductors where one type of carrier dominates, the force due
to Lorentz force is balanced by the force on the charge carriers due to Hall field.

qEH = q(v x H)

Where „v‟ is the drift velocity of the carriers.

Also,
J = qnv

Where q is the charge of each carrier and n is the carrier concentration.

So,

RH = EH(J X H) =1/nq (1)

Where RH is called the Hall coefficient and depends only on the free charge carrier density (n)
for a given material.

Let us consider a semiconductor material in the form of a bar having dimensions X, Y and Z. let
J is directed along X and H is along Z, and the Eh will be developed across Y, is shown in fig.2

R H = EH / J H

VH / Y

( I / YZ ) H

Therefore, on substitution in equation (2) we get,

RH = 1 / (n q) (3)

From this equation, it is clear that the sign of Hall coefficient depends upon the sign of the q.
This means, in a p-type specimen the RH would be positive and in a n-type it would be negative.

When one type of carrier dominates, the conductivity of the sample will be given by,

=nq (4)

Where  is the mobility of the charge carriers. Thus,

 =  RH (5)

RH is expressed in cm3/Coulomb.
 in -1cm-1,
Thus  is expressed in cm2V-1s-1.
And the carrier concentration is given by
n = 1/RH q

EXPERIMENTAL PROCEDURE:

1. Connect the widthwise contacts of the hall probe to the terminal marked „hall voltage‟ of
the set-up.
 2. Connect the lengthwise contacts of the hall probe to the current terminals

3. Pass a very small current through the crystal and measure the zero magnetic fields
potential. This should be made minimum possible by adjusting one of the hall probe
contacts.

4. Switch on electromagnet power supply and adjust to any desired value. Rotate the hall
probe till it becomes perpendicular to the magnetic field. Hall voltage will be maximum
in this adjustment.

5. Calibrate the apparatus by plotting the graph between current through electromagnet v/s
magnetic field in guassmeter. It is straight line.

6. Measure hall voltage for both the directions of the current and magnetic field.

7. Measure the hall voltage as the function of current keeping the magnetic field constant.
Plot a graph.

8. Measure the hall voltage as the function of magnetic field keeping a suitable value of
current, as constant. Plot a graph.

CALCULATIONS:

1. From both the graphs calculate separately the hall coefficient RH.

2. Calculate the carrier mobility, and the concentration of charge carriers using the specified
value of resistivity of sample.

3. Given = 8 -cm for Ge, obtained from four-probe method.

4. Z= 0.05 cm

Figure 1 showing the hall effect

 I. Calibration of magnet:

S. No. IM (A) H (gauss)

II. IM = ______ A

H = ______G

S. No. Is Vs

III. Is = _______ mA

S. No. Iμ H VH
 EXPERIMENT NO: 13

OBJECT: TO ESTIMATE THE BAND GAP ENERGY (EG) OF Ge CRYSTAL FROM

RESISTIVITY VERSES TEMPERATURE MEASUREMENTS USING FOUR PROBE
TECHNIQUE .

INTRODUCTION:
Many conventional methods for measuring resistivity are unsatisfactory for
semiconductors because metal-semiconductor contacts are usually rectifying in nature. Also,
there is generally some minority carrier injection by one of the current carrying contacts. An
excess concentration of minority carriers affects of potential of other contacts and modulates the
resistance of the material.
Four probe method overcomes the difficulties mentioned above and also offers several
other advantages. It permits measurements of resistivity in samples having a wide variety of
shapes. It is not always convenient to produce a specimen of known dimensions for a
conductivity measurement. This method is used to measure, conveniently and accurately, the
conductivity of ingots or slices, both thick and thin of semiconductor crystals.

THEORY:
The probe basically employs four spring loaded equi-spaced needles which make contact
with a plane shaped surface on the specimen as shown in figure (1). A stabilized current is
passed through the outer pair of probes, 1 and 4 and the voltage V, between the inner two, 2 and
3 is measured by a voltmeter which draws negligible current.

Figure (1): Schematic diagram of Four probe setup

We know that for the four probe setup at a given temperature T

o = 2s(V/I) (1)

Where “s” denotes inter probe spacing.

This equation (1) is valid only for materials whose dimensions are large compared with the probe
spacing S. If this is not the case, for example, when measurements are made on thin slices or
small disc of materials, then a correction factor G (b/s) is introduced.

Here:

s = distance between two probes = 0.233 cm

b = thickness of the crystal = 0.04 cm

So, the correction factor, G (b/s) = 8

And the resistivity will be given by

c = o/G(b/s)

For semiconductors the variation of high temperature (>room temperature) resistivity is inversely
proportional to the intrinsic charge carrier concentration variation. The intrinsic charge carrier
concentration varies with temperature as

ni α exp(-Eg/2kT)

And the measured resistivity at the given temperature is proportional to the voltage drop
developed.
α V
So,

V α exp(Eg /2kT)

ln V =(Eg /2kT) + A

From the graph ln V vs 1/T, Eg can be calculated.

EXPERIMENTAL PROCEDURE:
1. Take the four probe resistivity measurement of the Ge sample at the room temperature.
2. Now fix the value of the current through the probes and switch on the heater (keep the
setting as low).
3. Measure the variation in voltage as the function of increase temperature.
4. From a graph for 1/T vs ln V.
CALCULATION:
1. From the probe measurement graph measure the room temperature resistivity of Ge.
2. From the temperature variation graph calculate the Band gab of Ge (in eV).

NOTE:
1. K= Boltzmann‟s Constant
=1.3807 X 10-23J/K

Figure (2): Temperature variation of resistivity for semiconductor.

I. Resistivity determination:

S. No. I V

II. Temperature :
I= ______ mA

S. No. T V Ln V 1/T
 EXPERIMENT NO. 07

OBJECTIVE: TO PREPARE TWO METALLIC SPECIMENS FOR METALLOGRAPHIC

EXAMINATIONS AND MEASURE THEIR GRAIN SIZE.

REQUIREMENTS: Sample, grinder, emery paper of grit vary from 100 to 800, alumina
powder and diamond paste, ethyl alcohol, distilled water, dryer, mounting machine, metallurgical
/optical microscope, etc.

THEORY:
For polycrystalline materials many properties depend on grain size .The micro structural
study features observed through microscopes can provide information regarding grains, their
morphology and distribution and phases in the material. Some of the technique which have
developed for observing the features are optical microscopy, electron microscopy, field-ion
microscopy, field emission microscopy, X-ray microscopy, and electro-probe microanalysis. Of
these, optical microscopy is by far the most important, since the equipment is relatively
inexpensive and easy to handle.
In order to observe the structure in optical microscope, the specimen surface is polished
and subsequently etched with appropriate reagents before microscopic examination. In a polished
specimen, the etching not only delineates grain boundaries, but also allows the different phases
to be distinguished by difference in brightness of grains. Differences in contrast may result from
differences in light absorption characteristics of the different phases.

a) b)
Figure:
a) Section of a grain boundary and its surface groove produced by etching; the light reflection
characteristics in the vicinity of the groove are also shown.
b) Photomicrograph of the surface of a polished and etched polycrystalline specimen in which
the grain boundaries appear dark.
Etching results in preferential attack or preferential staining of the surface. The
preferential attack is electrochemical corrosion. Grain boundaries are often anodic to the bulk
metal in the interior of the grain and so are etched away preferentially and delineated staining is
produced by deposition of solid enchant product on the specimen surface. This is formed by
chemical reaction between enchant and the specimen. Under the favorable conditions the use of
proper enchant enables the identification of constituents. Micro structural examination can
provide quantitative information about the following parameters:

 The grain size of specimens

 The amount of interfacial area per unit volume

 The dimensions of constituent phases

For grain size measurement, the grains along a line, circle, or within a known area are counted.
From the study of actual grain shapes it has been found that, while grains do not actually posses
a regular or idealized forms, the truncated octahedron is a reasonable approximation for equaxed
grains. From the analysis of the distributions of sections in space occupied by truncated
octahedral, the ASTM system gives the following relationship:

n = 2N-1

Where, „n‟ is the number of grains per square inch at 100X and
„N‟ is the ASTM grain index number

In the ASTM method, the microstructure or the photomicrograph of a given polycrystalline

specimen at a magnification of 100X is compared with a set of standard micrographs or idealized
polygons as can be seen in the microscope. The charts are indexed for varying from 1 to 8.

Formula for grain size determination:

At 100X

So, Actual Grain size = (Diameter at 100X)/100

EXPERIMENTAL PROCEDURE:

Specimen preparation:
Grinding: An unprepared specimen may have sharp edges and many scratches. Any burn on the
edges of the specimen should be removed by means of a coarse grinding paper or a file. In order
to remove scratches, the specimen is rubbed on emery papers. Initially a coarse grade paper is
used for this purpose. The paper is placed on a smooth hard surface such as a glass sheet and
then specimen is gently rubbed backward and forward against it until only scratches due to the
particular paper can seen to cover the surface. Then the specimen is ground on the next finer
emery paper in such a direction that the new set of parallel scratches are at right angle to the
previous set, so that the removal of previous grinding marks is easily observed. This procedure is
repeated till the finest emery paper has been used.

Polishing: The specimen is polished by holding it against a horizontal rotating disk. The disk is
covered with a velvet cloth which has very fine particle such as alumina (Al2O3) or Fe2O3 (600
nm – 1 m size) embedded in it. During polishing the velvet cloth is supplied with these particles
in the form of an aqueous suspension at regular intervals. These abrasive particles rub against the
specimen and produce a very smooth surface. During this process the surface must attain such a
good polish as to resemble a mirror.

Etching: Before etching, the specimen should be thoroughly washed with water and dried with
alcohol. The specimen, with its polished side upwards should be immersed in the etching
solution contained in a small porcelain dish. The specimen surface should be examined from
time to time and the specimen is removed from the enchant when grain structure is visible to the
unaided eye. After etching, the specimen is thoroughly washed with water and then dried with
alcohol.

Microstructural Examination: Before placing he specimen on the microscope stage, fix the
specimen on a glass slide with plasticine and level the etched surface with the help of leveling
device

OBSERVATIONS:
i) Calculate the number of grains per square inch of each specimen.
ii) Measure the grain size of both specimens and report it.
Complete your report by answering the following questions:

1) What limits the resolution of an optical microscope? Is the minimum size of an object
which can be observed by an optical microscope, limited by magnification or resolution?

2) How can you improve the resolving power of your optical microscope?

3) How can you obtain better image contrast in an optical microscope?

4) How mechanical properties changes with grain size?