MATERIAL SCIENCE LAB REPORT (EM204)

EXPERIMENT 5: PHASE DIAGRAM

TEOH YEE CIEN

(1001437330)

MECHANICAL DEPARTMENT

FACULTY OF ENGINEERING, TECHNOLOGY & BUILT ENVIRONMENT

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 TABLE OF CONTENT

CONTENTS

1. Introduction
a. Objective
b. Introduction
2. Material and Methodology
a. Materials & Apparatus
b. Procedure
3. Results
4. Discussion
5. Conclusion
6. Reference

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Learning Objectives:
 To provide a simple practical solidification process through solidifying Pb-Sn alloys of
four different compositions

 To obtain cooling curves during solidification

 To predict the microstructure development during slow cooling

 To understand how a phase diagram is constructed

Introduction

For a pure element, there exists a certain temperature at which the material changes from
a solid phase to a liquid phase (see Figure 1). This process called the solidification, freezing or
melting temperature. Alloys do not have a single melting temperature. Instead, there is a range of
temperatures over which the material is a mixture of both solid and liquid (see Figure 2). The
extent of this temperature range depends upon the alloy’s composition. The temperatures at
which the alloy is 100% liquid and 100% solid are used to define this range. These temperatures
are plotted against the alloy’s composition and are called the liquidus and solidus lines, which
form part of the phase diagram.
In this experiment, student will be able to construct the solidus and liquidus curves for a
binary alloy Pb-Sn. These curves will be found using a thermocouple to monitor the temperature
of specimens of various compositions during continuous cooling. By repeating this experiment
for a number of compositions, student will be able to outline the general shape of the phase
diagram.

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Figure 1: Near equilibrium cooling curve for a pure metal or a eutectic ally. Solidification takes
place at a single temperature.

Figure 2: The cooling curve characteristic of binary alloy where solidification takes place over a
range of temperature. Tb is the temperature at which solidification begins and Tc is the
temperature at which solidification is complete.

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 Figure 3: The Pb-Sn Equilibrium Phase Diagram

Materials, Apparatus and Methodology

Crucible, tongs, Bunsen burner, type-K thermocouple, cooling rack, weighing balance, tripod
stand

Reagent grade granulated lead and tin of the following compositions (in wt%): Sample 1 (0% Pb
– 100% Sn), Sample 2 (40% Sn – 60% Pb) and Sample 3 (40% Pb – 60% Sn)
Caution: Lead is toxic. Use gloves when handling the material. Do not inhale the fumes during
heating.

Procedure:

Heating of samples:
1. Sample 1 (0% Pb – 100% Sn) inside the crucible had put on the tripod stand with wire gauze
and heated by the Bunsen burner under the tripod stand.
2. The Bunsen burner had turned off after the sample has melted and allow the crucible slowly
cool down on a cooling rack.

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3. The thermocouple had inserted into the melt and chart the voltage output of the thermocouple
at the interval of every 5 seconds. The thermocouple had put in the middle of the molten
sample carefully.
4. The thermocouple has stopped measuring after the sample had cooled to the point not further
phase transformation.
5. The sample had remelted to easily remove the thermocouple.
6. The steps 1 to steps 5 had repeated for remaining samples, which is sample 2, and sample 3.

Result and Calculations

Sample 1 (60% Pb - 40% Sn):

Time (Second) EMF (mV) Time (Second) EMF (mV)

0 10 80 4.3
5 9 85 4.2
10 8.1 90 4
15 7.8 95 3.9
20 7.5 100 3.7
25 7.2
30 7
35 6.6
40 6.4
45 6.3
50 5.6
55 5.3
60 5
65 4.9
70 4.7
75 4.5
Table 1

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Sample 2 (40% Pb - 60% Sn):

Time (Second) EMF (mV) Time (Second) EMF (mV)

0 8.8 75 6.3
5 8.6 80 6.6
10 8.4 85 6.6
15 8.1 90 6.5
20 7.7 95 6.4
25 7.5 100 6.6
30 7.6 105 6.5
35 7.2 110 6.4
40 6.7
45 7.2
50 7
55 6.9
60 6.8
65 4.1
70 6.7
Table 2

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Sample 2 (100%Sn - 0%Pb):

Time (Second) EMF (mV) Time (Second) EMF (mV)

0 55
9.5 8.4
5 60
9.1 8.2
10 65
9 8
15 70
89 7.7
20
8.9
25
8.8
30
8.8
35
8.8
40
8.7
45
8.7
50
8.5
Table 3

From the experiment 4, student get the equation to use to determine the temperature of this
experiment 5 which is y = -100.2x6 + 557.1x5 - 1236.x4 + 1383.x3 - 802.5x2 + 241.9x + 4.444.
To determine the temperature in the experiment 5, We need to obtain the temperature linearly, so
the polynomial equation which is y = -100.2x6 + 557.1x5 - 1236.x4 + 1383.x3 - 802.5x2 + 241.9x
+ 4.444 had changed to linear equation which is y = 21.43x + 25.5 . Temperature can be
calculated by using the linear equation and the EMF value, the value had recorded below the
Table 4, Table 5 and Table 6.

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Sample 1 (60% Pb - 40% Sn):

EMF (mV) Temperature

10 239.8 4.2 115.5
9 218.4 4 111.2
8.1 199.1 3.9 109.1
7.8 192.6 3.7 104.8
7.5 186.2 4.2 115.5
7.2 179.8 4 111.2
7 175.5 3.9 109.1
6.6 166.9
6.4 162.6
6.3 160.5
5.6 145.5
5.3 139.1
5 132.6
4.9 130.5
4.7 126.2
4.5 121.9
4.3 117.6
Table 4

Sample 2 (40% Pb - 60% Sn):

EMF (mV) Temperature

8.8 214.1 6.8 171.2

8.6 209.8 4.1 113.4
8.4 205.5 6.7 169.1
8.1 199.1 6.3 160.5
7.7 190.5 6.6 166.9
7.5 186.2 6.6 166.9

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 7.6 188.4 6.5 164.8
7.2 179.8 6.4 162.6
6.7 169.1 6.6 166.9
7.2 179.8 6.5 164.8
7 175.5 6.4 162.6
6.9 173.4 6.8 171.2

Table 5

Sample 3 (100%Sn - 0%Pb):

EMF (mV) Temperature

9.5 229.1 8.5 207.6

9.1 220.5 8.4 205.5

9 218.3 8.2 201.1

8.9 216.2 8 196.9

8.9 216.2 7.7 190.5

8.8 214.1

8.8 214.1

8.8 214.1

8.7 211.9

8.7 211.9
Table 6

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Graph:

Temperature against time(s)

300

250

200

sample1
150
sample2
sample3
100

50

110
100
105

115
120
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95

Sample 1 (60% Pb - 40% Sn):

Sample 2 (40% Pb - 60% Sn):

Sample 3 (100%Sn - 0%Pb):

Figure 4

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Figure 5: The Pb-Sn equilibrium Phase Diagram.

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Discussion and Question

In this experiment, student able to observe a solidification through solidifying lead(Pb)

and tin(Sn) alloys of four different composition. Which are sample 1 60% of Pb and 40% of
Sn. Sample 2 40% of Sn and 60% of Pb.Sample 3 100% of Sn.
The result recorded is calculated and tabulated. To find the value of temperature of eat
record by using the formula equation.

The results recorded is calculated and tabulated. To determine the temperature of each record,
the formula of 𝑦 = 21.43𝑥 + 25.5 is applied. For example, the value of 10mV is taken:

𝑦 = 𝑇𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒 = ?

𝑥 = 𝑒. 𝑚. 𝑓 = 10.0 𝑚𝑉

𝑦 = 21.43𝑥 + 25.5

𝑦 = 21.43(10.0) + 25.5

𝑦 = 214.3 + 25.5

𝑦 = 239.8°𝐶

By using the data, cooling curve of each sample is constructed. A few data is obtained
from the cooling curve.
Alloy Tb/ oC Tm/ oC
60%Pb-40%Sn 239.8 96.2
40%Pb-60%Sn 214.1 162.6

Pure metal Tm/ oC

100%Sn 214.1

Because the heating of the sample will stopped when it melts, so we assumed that the sample
started to solidify again as soon as we stopped burning when it completely turn solid. Where Tb

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is the temperature where solidification begins and Tc is the temperature at which solidification
completed. Tm is the melting temperature for pure metals.

Next, a phase diagram is constructed according to the melting point obtained. Liquidus
line, Solidus line, Solvus line, Eutectic point and Phase regions is labelled in the diagram

1. Compare your result with the phase diagram in Figure 5.3. If there are any differences ,
explain them.
The students are required to compare between experimental phase diagram with
theoretical phase diagram .As can be seen between the two graphs, there is a similarity in the
profile. Some of the values are not the same, which the temperature where the horizontal line
is represented, melting point of Tin (Sn), and composition to achieve eutectic point.
From the diagram, the lowest temperature at which liquid phase will exist at 200oC,
where as in the theoretical diagram the lowest temperature is about 183oC.That are 2 reason
that will cause the different, which is temperature equation error and procedural error. For the
equation error, the difference is caused by the equation not being able to give result to
accurate temperatures. By giving non-precise values of temperature, it affects the diagram as
well. The problem can be solved by calibrating the thermocouple to be a more linear equation.
Another reason is procedural error, which means that the students do not follow the procedure
accordingly, which gives incorrect reading of EMF. Incorrect EMF readings will affect the
equation and consequently give incorrect results. This problem can be solved by reading the
manual lab before conducting the experiment.
Another problem is the difference of melting point of tin. Theoretically, the melting point
of Sn is 232oC, but the students obtained the value of 296oC, which has 64oC difference. This
difference is quite big of a value to be ignored. This difference is likely to be caused by the
same problems mentioned before: equation and procedural error.
Lastly is the composition percentage to achieve eutectic point. This point is used to
represent the lowest temperature at which a liquid phase may exist for any lead-tin
equilibrium. The difference is caused by the problems mentioned. By solving the problems,
the eutectic point will surely change.

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2. The cooling curves for some of the mixtures may show a dip in temperature as shown in
Figure 5.1.Explain why this occurs.

As can be seen in figure 7, there is a dip at the mixture’s freezing point. This happened
because of supercooling. Supercooling is a phenomenon where a material will begin to have
appreciable nucleation rate after the temperature has been lowered to below equilibrium
solidification temperature. This occurs because of the activation free energy become lower
when the temperature is decrease, so the forming unstable nucleus which cause the increasing
of nucleation rate. This phenomenon can happen to homogeneous nucleation and also
heterogeneous solution. Some homogeneous nucleation may need significant value of degree
to achieve supercooling compared heterogeneous solution.

3. Include sketches of the microstructures for each of the sample composition during
cooling.

4. Based on figure 5.3, determine the phases and amount of phases present in 60%Pb-
40%Sn and 40%Pb-60%Sn and eutectic composition using the Lever Rule.

In 60%Pb-40%Sn. It has three phase which are liquid, Pb +liquid and Pb+ Sn
a) Amount of liquid phase=100%
b) Amount of liquid in Pb + Liquid phase=[(40-18.3)/(61.9-18.3)]X100%=49.77%
liquid
Amount of Pb in Pb +Liquid phase=[(61.9-40)/(61.9-18.3)]X100%=50.23% Pb
c) Amount of Pb in Pb +Sn phase=[(97.8-40)/(97.8-18.3)]X100%=72.7% Pb
Amount of Sn in Pb +Sn phase=[(40-18.3)/(97.8-18.3)]X100%=23.3%Sn

In 40%Pb-60%Sn, it has three phase which are liquid , Pb+liquid and Pb+Sn

a) Amount of liquid phase=100%

b) Amount of liquid in Pb + Liquid phase=[(60-18.3)/(61.9-18.3)]X100%=95.64%
liquid
Amount of Pb in Pb +Liquid phase=[(61.9-60)/(61.9-18.3)]X100%=4.36% Pb

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 c) Amount of Pb in Pb +Sn phase=[(97.8-60)/(97.8-18.3)]X100%=47.55% Pb
Amount of Sn in Pb +Sn phase=[(60-18.3)/(97.8-18.3)]X100%=52.45%Sn

5. Comment the significance of the solvus lines

Conclusions

In conclusion, the results of the experiment was not as expected. From the results obtained,
it can be seen that the experimental diagram does not resemble the theoretical one in case of
value. This resulted incorrect diagram. However, the experimental diagram has quite similar
profile with the theoretical one. This suggests that only the measurements are incorrect. Other
than that, the students were able to plot the cooling curves of the three samples. The curves did
not fully resemble the figures given in the lab manual, however it has a similarity, which is
having a decreasing temperature as the time extends. By doing this experiment, the students were
able to obtain the cooling curves of the three materials, understand the concept of the
microstructure phases in cooling process and to plot the phase diagram and able to compare with
theoretical one.

References

1. Answers 2014, The Supercooling Process and Its Uses, retrieved 24 July 2014, <
http://chem.answers.com/chemistry-basics/the-supercooling-process-and-its-uses>
2. JW 2000, Chapter 9: Phase Diagrams, retrieved 24 July 2014, <
http://web.eng.fiu.edu/wangc/EGN3365-9.pdf>
3. http://chemed.chem.purdue.edu/genchem/topicreview/bp/ch14/phase.php
4. http://userwww.sfsu.edu/ozer/Phase%20Diagrams.pdf
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