MARMARA UNIVERSITY

FACULTY OF
ENGINEERING
DEPARTMENT OF METALLURGICAL AND
MATERIALS ENGINEERING
MSE 2106

MATERIALS LABORATORY

EXPERIMENT 3 - Determination of The Lead-Tin Phase Diagram By

Thermal Analysis

By

Muhammed Utku Acu

150523042

To

Asst. Prof. Mehmet Masum TÜNÇAY

Res. Asst. Özgür ÇINAR

10.04.2025
Contents
1 Introduction 2

2 Background 2
2.1 Phase Diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2.1.1 Unary Phase Diagram (Single Component) . . . . . . . . . . . . . . . 2
2.1.2 Binary Phase Diagram (Two Components) . . . . . . . . . . . . . . . 2
2.1.3 Ternary Phase Diagram (Three Components) . . . . . . . . . . . . . 3
2.2 Cooling Curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

3 Procedure 5

4 Results 6

5 Discussion of Results 7

6 Conclusion 8

References 9

A Cooling Curves of Pb-Sn 10

1
1 Introduction
The purpose of this experiment is to demonstrate the process of constructing a phase diagram
from cooling curves. This highlights the meaning and importance of some critical points in
phase diagrams.

2 Background
2.1 Phase Diagram
Phase diagram is a type of chart used to show conditions (pressure, temperature, etc.) at
which thermodynamically distinct phases (solid, liquid or gaseous) occur and coexist at
equilibrium. [4]
Phase diagrams mainly split into three kinds that are being: Unary phase diagrams (sin-
gle component), binary phase diagrams (two components), ternary phase diagram (three
component).

2.1.1 Unary Phase Diagram (Single Component)

The water phase diagram is a typical example of a unary phase diagram. Axis of this diagram
is temperature vs. pressure.

-100 °C -50 °C 0 °C 50 °C 100 °C 150 °C 200 °C 250 °C 300 °C 350 °C 400 °C

100 MPa 1 kbar

10 MPa 100 bar

1 MPa 10 bar

Water
100 kPa 1 bar
Pressure

Ice
10 kPa 100 mbar

Vapor
1 kPa 10 mbar

100 Pa 1 mbar

10 Pa 100 µbar

1 Pa 10 µbar
150 K 200 K 250 K 300 K 350 K 400 K 450 K 500 K 550 K 600 K 650 K 700 K

Temperature

Figure 1: Water phase diagram

2.1.2 Binary Phase Diagram (Two Components)

A binary system in the context of phase diagrams refers to a system made up of two com-
ponents (elements or compounds) that can form mixtures or alloys. Binary phase diagrams
help visualize how these two components behave together across varying temperatures and
compositions, at constant pressure (usually 1 atm). Axis of this diagram is composition vs.
temperature. This is the type of diagram that this experiment aims to construct.

2
 660
647

T (°C)
600 Liquid

550
NaI + L L + RbI
505 NaIss RbIss
18 82

450

NaI + RbI
400

350
0 20 40 50 60 80 100
NaI Mol% RbI RbI

Figure 2: NaI-PbI phase diagram

2.1.3 Ternary Phase Diagram (Three Components)

A ternary phase diagram represents the phase behavior of a system containing three com-
ponents. These diagrams are essential when dealing with more complex mixtures, such as
alloys, ceramics, and chemical solutions. Unlike binary diagrams, which are plotted on a 2D
graph (temperature vs. composition), ternary diagrams use a triangular composition plot to
show the relative proportions of the three components with constant temperature or pressure.
Phase diagrams can be constructed by [2]

ˆ Thermodynamic modeling

ˆ Measure/analyze cooling curves at each composition (Thermal analysis)

ˆ Evaluate phases present at each composition by x-ray diffraction (XRD)

ˆ Evaluate microstructure by light (Micrograph analysis)

ˆ Determine composition and microstructure by scanning electron microscope (SEM)

In this experiment thermal analysis method used for constructing phase diagram.

2.2 Cooling Curve

Cooling curve is a line graph that represents the change of phase of matter typically from a
a gas to a solid or a liquid to a solid. The x-axis is time and the y-axis is temperature. The
initial point of the graph is named as pouring temperature. When the phase change occurs
there is a thermal arrest (temperature stays constant). Cause of this arrest is latent heat. [3]

3
Latent heat is energy released or absorbed, by a body or a thermodynamic system. Latent
heat arises due to the energy needed to overcome or form molecular bonds. [1] From the
cooling curve at choosen composition you can transform this data into phase diagram.

POURING TEMPERATURE

SUPERHEAT
T/t = COOLING RATE

TEMPERATURE [T]
EQUILIBRIUM FREEZING
TEMPERATURE

THERMAL ARREST

LOCAL SOLIDIFICATION TIME

TOTAL SOLIDIFICATION TIME

TIME (t)

Figure 3: Examplary cooling curve

LIQUID
LIQUIDUS
TEMPERATURE [T]

SOLIDUS
FREEZING RANGE
LIQUID &
SOLID

SOLID

Cu % Ni Ni TIME (t)
PHASE DIAGRAM COOLING CURVE

Figure 4: Transition from cooling curve to phase diagram

4
3 Procedure
1. The furnace is heated up tp range of 450-500 C way above freezing point for the
observing the thermal arrest.

2. A sample of 90 wt% Sn-10% Pb alloy placed into crucible.

3. crucible placed into the furnace and waited until it is completely melted.

4. Melted solution removed from the furnace and put into 21 C room.

5. Right after the removing from the furnace thermocouple inserted into the solution.

6. temperature data recorded until a satisfactory cooling curve obtained.

5
4 Results
From the data recorded from experiment cooling curves constructed as given in Appendix A.
By using this cooling curves critical points extracted as given in Table 1.

Table 1: Critical points of Pb-Sn cooling curves.

Composition (wt % Sn) Temperature (°C)

100 210
97 251,208
75 194,182
62 241,188
50 223,185
30 250,182
19 256,249,160
10 207,184

By using this critical points estimation of Pb-Sn phase diagram is given in Figure 5.

Figure 5: Phase diagram of Pb-Sn from the experimental data.

6
5 Discussion of Results
As experimental phase diagram compared with standard Pb-Sn phase diagram (given in
Figure 6) differences can be seen.

Figure 6: Standard Pb-Sn phase diagram

Cause of this disturbances can be human error (researchers comment on the cooling curves)
or faulty laboratory equipment or the compositions of the alloy could be faulty.

7
6 Conclusion
This experiment successfully demonstrated the methodology for constructing a binary phase
diagram through the thermal analysis of cooling curves, specifically for the Pb-Sn alloy sys-
tem. By systematically recording temperature variations during the solidification process
across a range of alloy compositions, key thermal arrest points indicative of phase transfor-
mations were identified. These critical temperatures were employed to estimate the corre-
sponding phase diagram. While the resulting experimental phase diagram exhibited some
deviations from the standard Pb-Sn reference diagram, these discrepancies are attributable to
potential sources of error, including compositional inaccuracies, instrumental limitations, or
subjective interpretation of cooling curves. Notwithstanding these deviations, the experiment
effectively illustrated the principles underlying phase diagram construction and emphasized
the utility of cooling curves as a fundamental tool in materials science for analyzing phase
behavior in binary systems.

8
References
[1] The Editors of Encyclopaedia Britannica. latent heat, 2025. [Accessed 8 April 2025].

[2] Tünçay, Mehmet Masum. Experiment 3 - Determination of The Lead-Tin Phase Diagram
By Thermal Analysis. 2025.

[3] Wikipedia contributors. Cooling curve — Wikipedia, the free encyclopedia, 2025. [Online;
accessed 8-April-2025].

[4] Wikipedia contributors. Phase diagram — Wikipedia, the free encyclopedia, 2025. [On-
line; accessed 8-April-2025].

9
A Cooling Curves of Pb-Sn

(a) 100 wt % Sn (b) 97 wt % Sn

Figure 7: Cooling curve of Pb-Sn.

(a) 90 wt % Sn (b) 75 wt % Sn

Figure 8: Cooling curve of Pb-Sn.

10
(a) 62 wt % Sn (b) 50 wt % Sn

Figure 9: Cooling curve of Pb-Sn.

(a) 19 wt % Sn (b) 10 wt % Sn

Figure 10: Cooling curve of Pb-Sn.

11