Laboratory 5 MAEN 1000

ENGINEERING MATERIALS (MAEN1000)

Metallography and Heat Treatment

October 2015
Brendan Jones
Laboratory 5: Metallography and Heat Treatment, October 2015

ABSTRACT

The aim of this report is to outline the aspects of and discuss the advantages and disadvantages of
metallography of alloys, precipitation hardening in aluminium and hardness and hardenability of steels. In
metallography the objective is to observe the physical structure of metals and alloys and analyse the effects
of wrought, cast and multiphase structures. The aim of the solid solution hardening and the precipitation
hardening of aluminium alloys, was to find the hardness values after a certain periods of time. The purpose
of the aluminium alloy after being heated and then quenched on one end was to measure the hardenability at
different length intervals from the quenched end. The hardness measurements were taken at various distances
on the metal from the quenched end which were then plotted against the distance to find the hardenability
curve. Hardenability is measured in terms of the severity (speed) of cooling that is necessary to prevent the
formation of pearlite or bainite.
Laboratory 5: Metallography and Heat Treatment, October 2015

TABLE OF CONTENTS
1.  INTRODUCTION ..................................................................................................................... 1 
2.  BACKGROUND ........................................................................................................................ 1 
2.1  Metallography of Cast and Wrought Alloys ............................................................................1 
2.2  Precipitation Hardening in Aluminium ...................................................................................1 
2.3  Hardness and Hardenability of Steels ...................................................................................2 
3.  EXPERIMENTAL PROCEDURE ................................................................................................. 2 
3.1  Metallography Procedure .....................................................................................................2 
3.2  Heat Treatment Technique ..................................................................................................2 
3.3  Hardness of Plain Carbon and Alloys Steels ...........................................................................2 
4.  RESULTS ................................................................................................................................. 3 
4.1  Metallography ....................................................................................................................3 
4.2  Solid Solution Hardening and Precipitation Hardening ............................................................4 
4.3  Effect of Rate of Cooling on the Hardness of Plain Carbon and Alloy Steels ..............................5 
5.  DISCUSSION .......................................................................................................................... 7 
6.  CONCLUSION ......................................................................................................................... 9 
7.  REFERENCES ........................................................................................................................ 10 
APPENDIX A:  ROCKWELL SCALES AND THEIR APPLICATIONS .............................................. 11 

LIST OF FIGURES
Figure 1. Pure Copper at 200x Magnification............................................................................................3 
Figure 2. 60/40 Brass (Cu-Zn Alloy) at 200x Magnification. .......................................................................3 
Figure 3. Rapid Cooled Pure Aluminium Microstructure at 1x Magnification.................................................3 
Figure 4. Slow Cooled Pure Aluminium Microstructure at 1x Magnification ..................................................3 
Figure 5. Hardness Values Measured from the non-ferrous Al-4%Cu Metal Alloy System .............................5 
Figure 6. ASIS 1040 (Plain Carbon Steel)/ASIS 4340 (Alloy Steel) Hardness Testing Measured against the
Distance from the Quenched end of the Jominy Bar ...................................................................6 
Figure 7. 60/40 Brass (Cu-Zn Alloy) at 200x Magnification ........................................................................7 
Figure 8. Grain Image of Pure Copper (200x Magnification) ......................................................................7 
Figure 9. SSS and ISS Diagrams Demonstrating how such Lattices are Structured (Materials Development I:
Metals and Alloys, 2015) ..........................................................................................................8 
Figure 10. Microstructural Development of Al2Cu showing the Depletion in the Strength of the Alloy as the
Incoherent Precipitates Grow (Materials Development II: Precipitation Hardening, 2015) ..............8 
Figure 11. Jominy curve Obtained by Plotting Hardness Values against the Distance from the Quenched End
(Physical Metallurgy) ...............................................................................................................9 
Figure 12. Separation of Austenite, Ferrite and Cementite in a Eutectoid Transformation.............................9 

LIST OF TABLES
Table 1. Hardness Testing of Aluminium Alloy (4.0% Cu) .........................................................................4 
Table 2. Jominy Bar Hardness Testing ....................................................................................................5 
Laboratory 5: Metallography and Heat Treatment, October 2015

1. INTRODUCTION

The purpose of this laboratory session is to introduce the concepts of metallography, heat treatment and the
application of phase equilibrium diagrams. Brass is a copper-based alloy with zinc as the main alloying element,
at anything between 0 – 50%. Brass is widely used in marine duties, where its resistance to atmospheric
corrosion is reasonable, provided that tarnishing is either accepted or taken care of by regular polishing.
However, for underwater use the unmodified alloy is not acceptable. The most commonly used alloys are
70/30 (70% copper, 30% zinc) which is ductile and 60/40 (60% copper, 40% zinc) which is rather more brittle
(Brass and Bronze, 2015). Typical duties for 70/30 brass are forgings, sheet, tubes and wires, whereas 60/40
is normally cast, for plumbing fittings and similar products (Brass and Bronze, 2015).

Precipitation Hardening (or Age Hardening) is commonly used to process aluminium alloys and other
nonferrous metals for commercial use. The examples are aluminium-copper, copper-beryllium, copper-tin,
magnesium-aluminium, and some ferrous alloys1 (Khaira, 2013).

2. BACKGROUND

2.1 Metallography of Cast and Wrought Alloys

Metallography is the application of appropriate surface preparation and visual microscopic inspection to
determine the physical structure of metals and alloys (Metallography and Heat Treatment, 2015). Most
commercially available metals have polycrystalline grains, randomly orientated with a common grain
boundary as the structure type.

Metals that have smaller grains are relatively strong and tough at low temperatures compared to metals
that have large grains which have good creep resistance at relatively high temperatures. A fine-grained
material is stronger and harder because it has a greater total grain boundary area to discourage
dislocation motion. In a longer time frame, the average grain size will increase in a metal, this
phenomenon occurs when the small grains shrink and hypothetically “disappear” while the large grains
continue to grow larger. Usually the temperature that the metal cools at will affect the grain size, if the
metal is cooled quickly then the grain size will be smaller than if the metal was cooled slowly. A wrought
substance will have larger grain sizes as it has a very slow cooling period, which allows for the small
grains to shrink and larger grains to grow.

2.2 Precipitation Hardening in Aluminium

Precipitation hardening (or age hardening) begins with the development of intermediate phase
precipitates within a crystal lattice. The precipitates act as sites to pin and block the movement of
dislocations in the lattice. The precipitates that are formed are extremely small and the particles are
uniformly dispersed through phase transformations induced by appropriate heat treatments. These
precipitates are present as a second phase within the original phase matrix. Examples include of
precipitation hardening include Al‐Cu, Cu‐Be and Cu‐Tin (Materials Development II: Precipitation
Hardening, 2015).

Annealing is the process of heat treatment where a material is exposed to a raised temperature for an
extended time period and then slowly cooled so that a few qualities change in the alloys. Some of these
are that there is an increase in ductility, toughness and softness. It reduces hardness, relieves stresses
and produces a specific microstructure that can be observed. Annealing of metal following cold working
allows grains to grow in the metal, it is similar to hot working in its end result. In the heat treatment
process, it first recovers then recrystallization. Which entitles new grains forming that has low dislocation
densities, small in size and consumes and replaces parent cold worked grains. Eventually all cold worked
grains are replaced then after a long time, average grain size increases. Small grains will shrink and

1
Ferrous alloys generally refer to iron-based alloys, or iron and steel.

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Laboratory 5: Metallography and Heat Treatment, October 2015

large grains will grow. Precipitation hardening in increases the strength of the metal/alloy by making
dislocation motion more difficult.

2.3 Hardness and Hardenability of Steels

If a piece of steel containing relatively high percentage of carbon is cooled rapidly it becomes harder
but more brittle. The degree of hardness produced is dependent on the percentage of carbon present
but this varies on the initial quenching temperature, size of the work piece, type of quenching medium,
its temperature and the amount of agitation. The rate of quenching doesn’t allow enough time for the
carbon to diffuse out of the structure FCC to form the BCC structure. The carbon is stuck in the solid
solution and the lattice is inaccurate which is known as martensite.

3. EXPERIMENTAL PROCEDURE

3.1 Metallography Procedure

1. A piece of metal was placed under the microscope for analysis at a particular magnification

2. The observed visual image was recorded in pencil

3. Magnification, properties of the alloys and any distinctive features were recorded for reference

4. These steps were repeated for four different metal formations

3.2 Heat Treatment Technique

1. The Rockwell test uses a pre-load to cancel out error

2. Aluminium alloy was solution treated at 525°C and subsequently aged at 180°C

3. Hardness was measured at various times, up to 240 minutes

4. Results were recorded and then plotted into a graph through an excel spreadsheet

3.3 Hardness of Plain Carbon and Alloys Steels

1. Observed the demonstration of the Jominy Bar test procedure

2. The plain carbon steel (AISI 1040) Jominy Bar was subjected to hardness testing

3. Results were recorded and subsequently a hardenability curve was plotted and graphed in an excel
spreadsheet

4. The alloy steel (AISI 4340) Jominy Bar was subjected to hardness testing

5. Results were recorded and subsequently a hardenability curve was plotted and graphed in an excel
spreadsheet

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Laboratory 5: Metallography and Heat Treatment, October 2015

4. RESULTS

4.1 Metallography

Figure 1. Pure Copper at 200x Figure 2. 60/40 Brass (Cu-Zn Alloy) at 200x
Magnification. Magnification.

Figure 3. Rapid Cooled Pure Aluminium Microstructure at 1x Magnification

Figure 4. Slow Cooled Pure Aluminium Microstructure at 1x Magnification

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Laboratory 5: Metallography and Heat Treatment, October 2015

4.2 Solid Solution Hardening and Precipitation Hardening

Table 1. Hardness Testing of Aluminium Alloy (4.0% Cu)

Hardness Values (HRa)

Aging Time
(Minutes)
1 2 3 Average

0 30 34 26 30.0

4 29 24 29 27.3

8 29 31 32 30.67

12 33 35 32 33.33

16 32 33 33 32.67

20 35 33 34 34

24 36 38 37 37

28 37 38.5 41 38.83

32 37 38.5 41 38.83

36 34 33 36 34.33

44 35 36 35 35.33

52 32 36 33 33.67

60 34 36 36 35.33

80 34 34 35 34.33

240 37 34 37 36

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Laboratory 5: Metallography and Heat Treatment, October 2015

Hardness Values of Al-4%Cu Alloy vs. Aging Time

45

40
Aging Time (Minutes)

35

30

25

20
0 50 100 150 200 250
Hardness Values (HRa)

Average Linear (Average)

Figure 5. Hardness Values Measured from the non-ferrous Al-4%Cu Metal Alloy System

4.3 Effect of Rate of Cooling on the Hardness of Plain Carbon and Alloy Steels

Table 2. Jominy Bar Hardness Testing

Hardness Values (HRc)

Distance (mm)
AISI 1040 AISI 4340

1.5 59 57

3 55.5 59

5 42 60

7 32 59

9 31 56

11 30 59

13 28 56

15 27 57

20 25 57

25 24 57

30 24 57

35 22 57

40 20.5 56.5

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Laboratory 5: Metallography and Heat Treatment, October 2015

45 19.5 56

50 18 56

55 15 55.5

60 14.5 57

65 13.5 56

70 10 57

AISI Hardness (HRc) vs. Distance (mm)

70

60

50
Hardness HRc

40

30

20

10

0
0 10 20 30 40 50 60 70
Distance from Quenched End (mm)

AISI 1040 AISI 4340

Figure 6. ASIS 1040 (Plain Carbon Steel)/ASIS 4340 (Alloy Steel) Hardness Testing Measured against the Distance
from the Quenched end of the Jominy Bar

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Laboratory 5: Metallography and Heat Treatment, October 2015

5. DISCUSSION

In the metallography analysis experiment samples, (a) Aluminium (slow cooled), (b) Aluminium (rapid cooled),
(c) Pure Copper and (d) 60/40 Brass were all analysed under a microscope. Figure 1 shows the pure copper
at 200x magnification clearly demonstrates a wrought copper structure when compared to Figure 8. The grains
in Figure 8 are consistent with that of Figure 1 as the grains resemble the grain boundaries which dictate the
hardness of the material. Figure 2 is the sketch of the 60/40 Brass alloy which is demonstrated below in colour
to distinguish between the zinc with dissolved copper (gold/yellow) and the copper saturated with zinc ~35%
(pink) (see Figure 7). As shown in Figure 8 the areas in pink is the alpha phase in which the copper saturated
with 35% zinc is a FCC structure while the beta phase (gold), zinc with dissolved copper is a BCC structure.

Pink - α (Alpha Phase)

Gold - β (Beta Phase)

Figure 7. 60/40 Brass (Cu-Zn Alloy) Figure 8. Grain Image of Pure

at 200x Magnification Copper (200x Magnification)

A rapid cooling rate (as seen in Figure 3) prevents the formation of grain boundary precipitates which rob the
alloy of solute, thus reducing precipitates available after ageing. As a result this decreases the strength and
hardness of the aluminium as there is less grain boundary area to oppose dislocation motion. On the other
hand the slow cooled aluminium (see Figure 4) is allowed to from grain barriers which increase the strength
and hardness of the metal and the ability to undergo aging.

Considering that the specimen used in the solid solution hardening experiment is an alloy of aluminium (Al-
4%Cu) it would more appropriate to use Rockwell B testing rather than Rockwell A testing as directed in the
lab sheet. According to Appendix A, the Rockwell Datasheet stipulates that for copper alloys, soft steels and
aluminium alloys the hardness is measured by Rockwell B (indenter is a steel ball – diameter of ~1.588mm).

Even so, as it so happens, copper (Cu) in aluminium (Al) does not precipitate according to its phase diagram,
but rather forms a metastable2 (state) precipitate phase before finally precipitating and forming the equilibrium
phase such as Al2Cu. If we consider an Al-Cu system, the first phase to form is a precipitate known as a Guinier
Preston (GP) zone3. This is followed by an intermediate phase before a stable (Al2Cu precipitate) phase forms.
As these reactions occur the hardness changes, increasing gradually as the precipitates grow (or age) and
change from a strong coherent phase eventually to a weak incoherent4 phase as the incoherent4 precipitates
grow in size but decrease in number (Materials Development II: Precipitation Hardening, 2015), (see Figure
9). During solution heat treatment all solute atoms are dissolved to form a single-phase solid solution
Quenching or rapid cooling to room temperature to form a no equilibrium supersaturated solid solution (to
prevent diffusion and the accompanying formation of any second phase). The supersaturated solid solution is
heated to an intermediate temperature within the two-phase region. At this temperature diffusion rates
become appreciable. The precipitates of the second phase form as finely dispersed particles. By quenching
and then reheating an Al-Cu (4.0 wt%) alloy, a fine dispersion of precipitates form within the grains. These

2
Metastable state refers to an excited state of a system which exceeds the lifetime of the ordinary excited
state and generally has a shorter lifetime than the lowest, often stable, energy state, called the ground
state (Metastable State, 2015).
3
Solute enriched regions of the material, which offer physical obstructions to the motion of dislocations (The
Strengthening Of Metals, 2005).
4
Coherent precipitate is a precipitate whose crystal structure and atomic arrangement have a continuous
relationship with the surrounding matrix from which the precipitate is formed (Khaira, 2013). An in
incoherent precipitate forms no relationship with the surrounding matrix crystal lattice structure.

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Laboratory 5: Metallography and Heat Treatment, October 2015

precipitates are effective in hindering dislocation motion and consequently, increasing alloy hardness and
strength (see Figure 5).

A solid solution forms when metals dissolve in all ratios one into the other. A solid state phase is when the
primary element has incorporated atoms of the secondary element(s) into the primary lattice. Sites for the
secondary element atoms can be:

 normal primary element sites: substitutional solid solution (SSS) (Figure 9.a)
 Between primary element sites: interstitial solid solution (ISS) (Figure 9.b)

Figure 9. SSS and ISS Diagrams Demonstrating how such Lattices are
Structured (Materials Development I: Metals and Alloys, 2015)

Figure 10. Microstructural Development of Al2Cu showing the

Depletion in the Strength of the Alloy as the Incoherent
Precipitates Grow (Materials Development II: Precipitation
Hardening, 2015)

Greater hardenability relates to a greater depth of hardening (e.g. the alloy steel 4340 has a higher
hardenability than the plain carbon steel 1040). This is largely due to the production of martensite in the AISI
1040 which decreases through the Jominy Bar because the quenched end is cooled faster than the opposite
end. The rate of quenching does not provide sufficient time for the carbon to diffuse out of the austenitic
structure (F.C.C.) to form the ferritic structure (B.C.C.). The carbon is trapped in this solid solution resulting
in the lattice structure becoming distorted. This phase is known as martensite. Due to the extreme distortion,
dislocation movement is virtually prevented with the result that the phase martensite is one of the hardest
produced in steels but extremely brittle. The results plotted on the graph in Figure 6 reflect the theoretical
analysis of the 1040 carbon steel sample as the trend shows the hardness decreasing as the distance from
the quenched end increases. A diagrammatically representation of this effect is shown in Figure 11 with the
curve decreasing the further the distance from the quenched end becomes.

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Laboratory 5: Metallography and Heat Treatment, October 2015

Figure 11. Jominy curve Obtained by Plotting Hardness Values against the
Distance from the Quenched End (Physical Metallurgy)

In some systems, particularly the iron carbon system, a solid solution stable at a higher temperature
decomposes into a two‐phase structure on cooling below a critical temperature. This is known as a eutectoid
transformation (Materials Development I: Metals and Alloys, 2015) (see Figure 12). Alternatively the sample
AISI 4043 alloy steel has a relatively consistent hardness from end to end of the Jominy Bar (see Figure 6).
This is due to the composition of the steel (Fe-C) alloy which contains nickel. The addition of certain alloying
elements such as nickel or magnesium generally stabilize the austenite structure whilst elements such as
silicon and chromium tend to destabilize the austenite. Austenite only exists in a stable state above 910°C but
a much higher alloy content can allow this structure to remain stable at room temperature. As mentioned
previously the graph in Figure 6 correlates with the theoretical properties of austenite and supports the trend
in the graph. The trend follows very little change in hardness from the quenched end of the sample to the
non-quenched end.

Figure 12. Separation of Austenite, Ferrite and Cementite in a

Eutectoid Transformation

6. CONCLUSION

In summary the theoretical analysis of the different experiments correlated with the data collected during
the laboratory. Besides using the incorrect method of Rockwell testing there seems to be little discrepancies
between the theory and the graphs plotted and analysis of the data. For more accurate results, more data
could have been collected from different specimens of the same alloy or metal, providing a larger range for
the data and producing more accurate results.

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Laboratory 5: Metallography and Heat Treatment, October 2015

7. REFERENCES

Brass and Bronze. (2015). Retrieved October 28, 2015, from Coxengineering.sharepoint.com:
http://coxengineering.sharepoint.com/pages/brassandbronze.aspx

Chegg.com. (2015). Retrieved October 28, 2015, from Chegg.com: http://www.chegg.com/homework-

help/questions-and-answers/3-shown-portion-al-cu-phase-diagram-heated-alloy-containing-8-wt-cu-
700oc-30-points-total--q2443155

Equilibrium Diagrams II – Applications. (2015). Perth, Western Australia, Australia. Retrieved October 28,
2015, from https://lms.curtin.edu.au/bbcswebdav/pid-2320888-dt-content-rid-
4957897_1/courses/307533-CU-061-01-Sxx-x2/Week%2010-
%20Materials%20Development%20II%2012.pdf

Hardness Testing. (2015). Retrieved October 29, 2015, from learneasy.info:

http://www.learneasy.info/MDME/MEMmods/MEM23061A/Hardness/Hardness.html

Khaira, D. H. (2013, November 18). Precipitation Hardening. Retrieved October 28, 2015, from
Slideshare.net: http://www.slideshare.net/RakeshSingh125/f-precipitation-hardening

Materials Development I: Metals and Alloys. (2015). Perth, Western Australia, Australia. Retrieved October
29, 2015, from https://lms.curtin.edu.au/bbcswebdav/pid-2320877-dt-content-rid-
21632773_1/courses/307533-CU-061-01-Sxx-x2/Metals%20and%20Alloys%282a%29.pdf

Materials Development II: Precipitation Hardening. (2015). Perth, Western Australia, Australia. Retrieved
October 28, 2015, from https://lms.curtin.edu.au/bbcswebdav/pid-2320888-dt-content-rid-
20192235_1/courses/307533-CU-061-01-Sxx-x2/Equilibrium%20Diagrams%20II%282%29.pdf

Metallography and Heat Treatment. (2015). Perth, Western Australia, Australia. Retrieved October 28, 2015

Metastable State. (2015, October 29). Retrieved October 29, 2015, from Encyclopedia Britannica:
http://www.britannica.com/science/metastable-state

Physical Metallurgy. (n.d.). Retrieved October 29, 2015, from http://www.iitk.ac.in/mme/test/MME415.pdf

The Strengthening Of Metals. (2005, August). Retrieved October 29, 2015, from Total Materia:
http://www.totalmateria.com/Article128.htm

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Laboratory 5: Metallography and Heat Treatment, October 2015

APPENDIX A: ROCKWELL SCALES AND THEIR APPLICATIONS

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