Eric Fitterling

Heat Treating of Aluminum

11/4/10
Dr. Amy Robinson
Abstract

In this laboratory, the effects of heat treatments on aluminum alloys were investigated. The aluminum
used was A356 which is approximately 7 wt% silicon and less than 0.3 wt% magnesium.1 Solution
treatments (S.T.) and age treatments were the two heat treatments studied. Each of these treatments
was applied to a normal A356 alloy and samples with titanium and boron grain refining additions. The
grain refined sample was harder after solution treatment. Upon age both samples increased in hardness
and both refined and unrefined samples yielded nearly the same hardness. Microstructure analysis
showed finer grains in the solution treated refined grain sample when compared to the unrefined
sample. After aging the microstructures were closer in grain size, but there were more fine particles of
silicon in the refined sample compared to larger particles in the unrefined sample.

Introduction

Heat treatment is defined as, “an operation or combination of operations involving the heating and
cooling of a metal or an alloy in the solid state for the purpose of obtaining certain desirable conditions
or properties.2” There are multiple types of heat treatments that all have different goals associated with
them. Annealing is a heat treatment that’s purpose is to create a uniform microstructure and relieve
stresses thus softening the material. A heat treatment leading to the hardening of an alloy is
precipitation hardening which creates precipitates that disrupt dislocation movement. Overall there are
many types of heat treatments many that are alloy specific. In general heat treatments are governed by
three different components: soak temperature, soaking time, and cooling rate.

The soak temperature dictates the amount of energy that is available. When referring to heat
treatment temperatures they are always below the liquidus line of an alloy. Heat treatments do not
include re-melting and casting of alloys. The energy that results from the soak temperature can cause
dissolution of soluble phases that are present in the alloy. When materials are cast different phases
precipitate out during cooling and the ones that are thermodynamically unstable at the soaking
temperature will dissolve into the solid solution. Thermal energy can also drive diffusion processes that
form precipitates, as is the case in age hardening. Heat treatment temperatures ultimately drive the
diffusion to thermodynamic equilibrium.

Equilibrium is dictated by the temperature, but all

diffusion processes take time. The amount of time that
the alloy is allowed to soak at affects the amount of
diffusion that occurs. If an alloy is only heat treated for a
short amount of time all of the atoms may not have
enough time to diffuse to equilibrium. The specific
properties of an alloy that arise from heat treatment can
be dependent on how much diffusion occurs. This is the
case with age hardening in certain alloys such as beryllium
copper alloys which has a peak strength that is reached at
a specific time. After that time the strength starts to go
down as shown in figure 1.
Figure 1. A graph of tensile strength vs time illustrating
3
the rise and drop of strength with age treatment times.
Lastly the cooling rate controls whether diffusion can
occur to obtain other structures or phases. The fastest
method of cooling is a quench which is performed by
submersing the alloy into a liquid (generally water or oil).
When an alloy cools this rapidly the microstructure and
phases that are present at the time of quench are locked
into place. Alternately, slower cooling methods include
air cooling or furnace cooling. These two cooling rates
can allow for other desired phases and structures. The
effects of cooling rate can be seen in figure 2 which
Figure 2. A graph temperature vs time with cooling rates
shows the structures arising in steel from cooling rate. 4
in red illustrating their effect on microstructure.
The different types of heat treatment cycles are classified into different categories and given letter
abbreviations. Anneal (O), solution heat treat (W), as fabricated (F), strain hardened (H), and the
broadest is tempers (T). Tempers can include a combination of solution treatment, artificial aging, cold
working, natural aging, stabilization, shaping processes, etc. To specify what type, the letter “T” is
accompanied by a numeral. Tables have been compiled that show optimal soak temperatures, times,
and cooling rates corresponding to the material and type of heat treatment.

Experimental Procedures

The specific type of aluminum studied in these experiments was a 356 series (A356). This means it had
an approximate composition of 7 wt% silicon and a small amount of magnesium (< 0.3 wt%). In a
previous lab two different samples were cast. The first had the normal composition of A356 and the
second had grain refiners added to it resulting in a composition with 0.05 wt% Ti and 0.01 wt% B. Both
of these samples were used in this heat treatment laboratory.

Heat treatment conditions for our samples of A356 were determined by consulting table 1. The samples
were to be solution heat treated and artificially aged which corresponds to a type 6 temper (T6). Due to
the fact that these tables are set for large amounts of material, the times were shortened to
accommodate the size of the samples. The temperature does not change because of size. For A356 and
a T6 heat treat the temperature of 540°C was used for the solution heat treatment and 155°C for the
age treatment. Soak times were shortened from 12 hours to 1.5 for the solution treatment and the
minimum of 3 hours was selected for the age treatment. A foot note at the bottom of the full table 1
states that unless specifically noted solution treatments are completed with a quench in room
temperature water.

Two samples of both the refined and unrefined grained aluminum alloys were solution treated in the
same furnace at 540°C for 1.5 hours. When the samples were removed from the furnace they were
immediately submerged in a bucket of water until cool. Next, one of each of the different sample was
aged in a furnace at 155°C for 3 hours. Aged samples were also cooled in water for convenience.

All four samples’ hardness was analyzed using a Rockwell hardness tester using the “H” scale (1/8”
diameter steel ball with 60kgf force). This scale was chosen because it could record an accurate
measure for both the solution and age treated samples making them easier to compare.

Once hardness measurements were taken the four samples were mounted and polished using SiC paper
in the following order: 240, 320, 400, and 600 grit paper. Next 1, 0.3, and .05 micron alumina slurry on
polishing wheels were used in that order. The samples were then observed under an optical microscope
and images were taken for comparison at 100X, 200X, and 500X.

Results & Discussion

The hardness results from the four samples are displayed in table 2 and show that after solution
Table 2

Solution Treated S.T. & Aged Percent Theoretical T6

Hardness Hardness Change Hardness
(HRH) (HRH) (*HRH)

Refined 98 115 16.95%

Unrefined 71 113 60.14% 90-105

treatment the grain refined sample was harder. Grain refined A356 is harder than unrefined A356
because it has smaller grains. This follows the Hall-Petch relation:5

This equation states that yield strength (σy) is inversely proportional to grain size (D). Figure 3 and figure
4 picture the unrefined and refined samples respectively, and it is discernable that the grain refined
sample has smaller grains. These smaller grains account for the higher hardness.
 Figure 3. A 100X micrograph of unrefined A356 Figure 4. A 100X micrograph of refined A356 in
in the S.T. condition showing large grains. the S.T. condition showing small grains.
In both the unrefined and refined samples the
hardness value rises after the aging process. This
increase is due equilibrium phases that arise from
the solution treatment and the age treatment. The
solution treatment at 550°C is at a temperature
just below the α-aluminum and liquid two-phase
region as seen as a red line in figure 5. This means
that material is still solid during solution treatment
and still in the Al + Si region, but when we look at
the same temperature on the Al-Mg2Si pseudo-
binary phase diagram (figure 6) it becomes
apparent that dissolution occurs. The Mg2Si Figure 5. An equilibrium phase diagram of aluminum
particles present dissolve into the α-aluminum matrix. and silicon with the solution treat temperature in red .
1

It was found that the maximum dissolution of Mg2Si particles was 1.4
wt%.1 With less than 0.3 wt % magnesium in A356, all of the Mg2Si
will dissolve. When the alloy is water quenched, after solution
treatment, the magnesium stays dissolved inside the matrix because
it does not have time to diffuse, thus supersaturating the aluminum.
The age cycle is at a much lower temperature, pictured in blue in
figure 6, well below the dissolution temperature for Mg2Si. This
means that the magnesium will diffuse back out and form Mg2Si
particles again. This is what is known as precipitation strengthening.
The particles impede dislocation movement and harden/strengthen
the material which explains why both samples were harder after age
treatment.

When observing the differences in microstructure from solution

Figure 6. A pseudo-binary phase treated sample to aged sample there is clearly more gray flakes in
diagram of aluminum vs Mg2Si with the aged samples. This can be seen when comparing unrefined and
the S.T. temperature in red and the solution treated to the unrefined and aged (figure 7). The refined
1
age temperature in blue. solution treated sample and its aged counterpart (figure 8) show the
same phenomena. An increase in gray flakes is not due to the presence of Mg2Si in the aged samples.
Figure 7. 500X micrographs of unrefined A356 and Figure 8. 500X micrographs of refined A356 and S.T.
S.T. on the left and S.T. and aged on the right. on the left and S.T. and aged on the right.

The amount of magnesium is so low that these particles are not discernable at these magnifications. In
addition to Mg2Si dissolving during solution treatment it has been shown that up to 1.5 wt% silicon will
also dissolve into the matrix.1 The increase in gray flakes, which are silicon clumps, is due to the
increase in silicon that comes out of supersaturation during aging.

The reason that the unrefined and refined A356 converge after age treatment is because there is a
switch in the mechanism dictating hardness/strength. Grain size dictated the hardness in the solution
treated samples, but after precipitation hardening occurs during the age treatment that overrides the
effects of grain size.

Theoretical T6 hardness for an A356 alloy was projected to be in the range of 90-105 HRH after
converting from Brinell scale. The values that obtained in this laboratory were higher than the
maximum. This could be explained by the fact that we were solution treating and ageing small samples
relative to the samples that the approximations were probably set from. Our small samples may have
reacted different to the heat treatment or high readings due to the close proximity of the edge of the
sample could have resulted.

Conclusion

The investigation into the hardness and microstructures of A356 under different heat treatments
answered many questions. Refined grain samples are harder than unrefined grain samples because of
the Hall-Petch relation relating strength to grain size. Age treatments raised the hardness for both
samples due to Mg2Si particles causing precipitation hardening. A more dense silicon flaked
microstructure arose in aged samples due to supersaturated silicon diffusing out. The converging
hardness values for the unrefined and refined samples after aging arose from the change in mechanism
that affects hardness. It switched from grain size dependant to precipitate dependent. Lastly, the error
from theoretical hardness values was due to our sample sizes.
References
1
Hernandez Paz, Juan F. “Heat Treatment and Precipitation in A356 Aluminum Alloy.” Montreal: McGill
University, Sept. 2003. Web. <http://digitool.library.mcgill.ca/R/BIGMRDGQ8MAVJ1P9S5VV8IR
A1RV1KHVTD8VJITQNSUAPUYL26T-01968?func=search>.
2
"Heat Treating Terms and Definitions - Engineers Edge." Engineers Edge - Design, Engineering &
Manufacturing Solutions. Web. 03 Nov. 2010.
<http://www.engineersedge.com/heat_treat.htm>.

3
"Age Hardening." Berylliumcopper-china|Strip、Rod、Plate / Bar、Wire. Web. 03 Nov. 2010.
<http://www.berylliumcopper-china.com/technical/indexx.htm>.
4
"CCT Curve Steel" Wikipedia, the Free Encyclopedia. Updated: 07 Jan. 2010. Web. 04 Nov. 2010.
<http://en.wikipedia.org/wiki/File:CCT_curve_steel.svg#filehistory>.
5
Murty, Dr. K. L. “The Hall-Petch Relation.” Raleigh: North Carolina State University, Feb. 2004. Web.
< http://www4.ncsu.edu/~murty/NE509/NOTES/Ch5d-Strengthening.pdf >.