Experiment 2.

Phase Diagram

Dona Katalina S. Valin
Department of Mining, Metallurgical, and Materials Engineering, College of Engineering
University of the Philippines, Diliman, Quezon City, Philippines
Date Submitted: February 6, 2014
I. Results and Discussion
Phase diagram shows the phase at equilibrium for specific temperature, pressure, composition, or
other variables. This is classified by numbers of components in the system: unary, binary, tertiary,
and quarter phase diagrams. For this paper, lead-tin (Pb-Sn), a binary diagram, is discussed.
In this experiment, 10-g of Pb-Sn mixture of different compositions was prepared. The time
and temperature was monitored using thermocouple as the mixture was cooled to 150
o
C. These
data were used to plot the cooling curves of each mixture (see Appendix I).
Cooling curves shows the relationship between the temperature and time as the mixture
cools down. This gives a negative slope since temperature decreases with time. But notice in the
graph below that some parts of the line are horizontal. This is where the phase change occurs.

Figure 1 Cooling Curve of 80% Pb- 20% Sn
The constant temperature is the freezing temperature when the motion of the individual
atoms stabilizes and the attractive forces among them are increased. For this transition to take
place, energy is released. This is the latent heat
[1]
. This energy prevented the temperature to
decrease, which offsets the cooling
[2]
. The temperature remains constant because the amount of
heat that is released by the system is equal to the amount of heat absorbed by the surroundings.
Before the phase change, the slope of the cooling curves (negatively) increases or less steep.
The liquid is starting to solidify, leading to the evolution of latent heat, which affect the
temperature. And after each phase change, the cooling and drop of temperature resumes.
Separately, lead and tin freezes at 327C and 232C, respectively. However, making them
solid solution changes the freezing temperature. This is shown in the difference with every cooling
curves (refer to Appendix I). They produced same shape, but differ in change in slope. Thus, the
proportion of tin and lead affects the temperature when lead starts to solidify. Increasing tin lowers
the freezing point when starts to crystallise, but the final temperature for both to solidify is
constant.
Compared to the other four graphs with two/three horizontal part, it is only the mixture of
40% Pb and 60% Sn that forms one plateau in its cooling curve, where the whole solidifies. This
mixture is called the eutectic. Eutectic reaction is the transition between liquid and two solids. The
final temperature is called eutectic temperature
[3]
.
Combining the data from the cooling curves of the mixtures, phase diagram is made, as
shown in Figure 2. Phase transformation can be predicted for change in any of the factors. In this
experiment, the pressure is assumed to be constant
[3]
.

Figure 2. Phase Diagram Pb-Sn: (a) Eutectic point; (b) Eutectic Isotherm; (c) Liquidus; (d) Solidus; (e) Solvus
The lines in the diagram are the phase boundaries. The phases can be composed of one or
two components. For binary eutectic systems, like Pb-Sn, there are three single phases regions:
=solid solution of Pb in Sn matrix, =solid solution of Sn in Pb matrix, and L=liquid, with three two-
phase regions. Solvus line separates the solid from solid solutions. Liquidus line separates liquid from
liquid plus solid, while solidus separates solid from liquid plus solid. The horizontal solidus at eutectic
temp is called the eutectic isotherm. While at eutectic or invariant point, liquid and two solid phases
co-exist
[3]
.
Aside from the phases that can be shown in the diagram, the composition and the relative
fraction of the phases can also be obtained.
From this experiment, the eutectic point is at 60% Sn and 188
o
C. Comparing it with the
theoretical values
[4]
of 61.9 % Sn and 183
o
C, the experimental values for eutectic points composition
and temperature has deviation of 3% and 1.63%, respectively. This error is expected since the
system is open. During heating/mixing of the metals, and cooling, the set-up is exposed to
contaminations, which may affect the composition and data. Another source can be from the
thermocouple and overheating of the sample.


References

[1] Latent Heat, Access through http://physics.info/heat-latent/ on February 6, 2014
[2]How does Freezing Release Heat Energy? Accessed through
http://theweatherprediction.com/habyhints2/468/ on February 6, 2014
[3] Phase Diagrams, Accessed through
http://web.utk.edu/~prack/mse201/Chapter%209%20%20Total.pdf on February 6, 2014
[4]Sn-Pb Phase Diagram, Accessed through
http://www.physicsforums.com/showthread.php?t=281790 on February 6, 2014
[5] Latent Heat, Accessed through http://global.britannica.com/EBchecked/topic/331406/latent-
heat on February 6, 2014



Appendix
I. Cooling Curves

A. 20% Pb 80% Sn



B. 40% Pb 60% Sn



C. 60% Pb 40% Sn


0
100
200
300
400
500
0 100 200 300 400 500
T
e
m
p
e
r
a
t
u
r
e

time (s)
0
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400
500
0 100 200 300 400 500
T
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p
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time (s)
0
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500
0 100 200 300 400
T
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time (s)
D. 80% Pb 20% Sn



E. 90% Pb 10% Sn




0
100
200
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400
500
0 100 200 300 400 500 600
T
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m
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time (s)
0
50
100
150
200
250
300
350
400
450
1
0
4
0
7
0
1
0
0
1
3
0
1
6
0
1
9
0
2
2
0
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5
0
2
8
0
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1
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0
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7
0
4
0
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6
0
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time (s)
II. Data