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Laboratory 7

Cold Work and Annealing Engineering Alloys


Goal
To investigate the change in mechanical properties produced by cold working and
annealing processes and to relate the properties to the microstructure.

Background
Why Study Deformation And Annealing In Metals?
It is no surprise to you that in order to get metals into the form of useful products,
be they crankshafts for bicycles or stents for angioplasty, they must be deformed (or
mechanically worked) in some way. This deformation is often done at temperatures
less than 40% of the metal’s melting temperature and thus categorized as cold work.
Most cold work is done at room temperature. Cold work can dramatically change the
properties of a metal or alloy. This change can be to our advantage: increasing the
alloy’s strength. It can be to our disadvantage: losing the alloy’s inherent ability to
withstand further deformation. For example, did you ever notice that when you bend
a metal paper clip back and forth, it gets harder and harder to bend before it
eventually breaks? This is an example of cold work and it actually summarizes some
important aspects of this laboratory.

The Effects of Cold Work on the Microstructure – Dislocations


When you permanently bend an alloy – such as bending a steel coat hanger 90° –
you have disturbed the arrangement of the atoms in the alloy’s crystal lattice. In
fact, you have dislocated the atoms from their original position. You have created
and caused the motion of dislocations. Dislocations represent a linear region of the
crystal where the arrangement of atoms departs from the regular crystalline
arrangement. This departure occurs only locally right at the dislocation. As you can
imagine, the distortion in the crystal causes strain all along the length of the
dislocation. You can think of a dislocation as a “tube” of strain, about 50 atoms in
diameter and running from one edge of a grain to the other. A single grain is the
same thing as a single crystal of atoms. Metals and alloys consist of countless grains
that fit together in three dimensions like soap bubbles in foam. Dislocations are
much too small to be seen by eye or even by a light microscope; we can use an
electron microscope to image them. But we can see evidence of their motion under
a light microscope by the preferred planes they move along. Ask your instructor to
set up some samples under the microscope if you are curious.

Dislocations are so important because they allow permanent deformation, also


known as plastic deformation, to occur. As shown in Figure 1, the passage of a
dislocation through a crystal can produce a net shift in atoms. Now, if you send lots
of dislocations through the metal, you can add up all those shifts to produce large
shape changes, like the 90° bend in our coat hanger. However, the overall crystal
structure or atomic spacings do not change. A common misconception is that atoms
get squished or compressed together during plastic deformation. In actuality, the
atoms are just getting shifted around by the dislocations. Any squishing of the
atomic bonds happens on a local scale right at the dislocation.

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Figure 1. A dislocation that passes through a crystal creates permanent or plastic deformation in the
material. The dislocation moves through a crystal much like a bump in a caterpillar.

Plastically deforming your coat hanger by putting one big bend in it has the effect of
not only moving dislocations (Figure 1), but creating them as well. This is the grain’s
way of accommodating the changes in shape that you are forcing on them.
Additional bends create more and more dislocations. And as the dislocations
intersect one another, it becomes more difficult to move them through the structure.
Since dislocation motion is necessary for plastic deformation, it gets harder and
harder to continue to cold work the material with more cold work. The process of
plastic deformation (moving and creating dislocations) has made continued plastic
deformation more difficult. This particular method of strengthening a metal is called
strain, or work, hardening. The mechanism of intersecting dislocations is why the
stress required for the next bend in your coat hanger (or paper clip) is more than the
stress needed for the previous one.

It’s a lot like traffic. Let’s say a dislocation is like a car. Driving in your car is like
the motion of a dislocation. Of course, there are other cars (dislocations) out there.
It’s easy to get where you want to go if the traffic is light. So, plastic deformation is
easy when there are not so many cars on the road. It is much more difficult to reach
your destination during rush hour. All those cars get in your way, and the flow of
traffic becomes slow. The same thing happens with dislocations: once there are lots
of dislocations in the structure, after a good amount of cold work, it is more difficult
to move any dislocation through, so the material is more resistant to plastic
deformation – the material is harder and stronger. It is like a “dislocation traffic
jam.”

Annealing: Three Steps to Reversing Cold Work


Now we are getting to the exciting part of our story. Imagine an engineering alloy
with lots and lots of dislocations in its structure. All those dislocations are jammed
together. The alloy is as hard (strong) as it can get. Another way of looking at this
is that you cannot move or introduce any more dislocations (i.e., plastically deform
the material) because it has reached its dislocation limit. If we wanted to continue
plastically deforming the alloy, to make some complex component shape, it would
not be possible because the alloy would fracture. We need a way to get rid of all
those dislocations; we need to anneal the cold worked metal.

Annealing is a heat treatment done to an engineering alloy. A heat treatment is the


process of controlled heating and cooling of a material. Annealing involves heating
the alloy to an elevated temperature and then slow cooling it or quickly water

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quenching it back to room temperature. Interesting effects happen to the structure
of the metal during the annealing process.

The initial change that occurs during annealing is that the thermal energy that the
atoms get through the elevated temperature allows them to rearrange themselves
into a slightly less-strained configuration. This is the first stage of annealing:
Recovery. Recovery is not too important because the mechanical properties of the
alloy do not change much from the cold-worked state. If the atoms get enough
thermal energy, they may continue their rearrangement into a nearly dislocation-free
structure. This is the second stage in the annealing treatment: Recrystallization.
Here is where the major mechanical property changes happen. This stage will be our
focus in the laboratory. With continued heating, or extended time at the heat
treatment temperature, the recrystallized grains might grow to become larger. This
is the third stage in annealing: Grain Growth. Grain growth, much like Recovery, is
not too important for changes in mechanical properties.

Recrystallization – The Most Important Stage in Annealing


Most of the “action” during the annealing heat treatment occurs during
Recrystallization. In this stage, the microstructure will change drastically, and this
means the mechanical properties are going to change also. The properties we are
interested in are strength and ductility. Recall that strength is resistance to
permanent deformation; ductility is the ability to permanently deform without
fracture.

We can track the microstructural changes occurring during Recrystallization. Figure


2 shows this in detail for α-brass, the alloy you will be working with in the laboratory.
α-brass is an alloy composed of copper (70%) and zinc (30%). Figure 2A shows
what the microstructure looks like after cold working. The brass grains have been
deformed, and this is evidenced by the many straight lines seen within each grain.
These lines, known as slip lines, are evidence of the motion of many dislocations.
The start of the Recrystallization process is shown in Figure 2B. Tiny new grains are
nucleated from of the cold-worked grains (red arrows). Notice how small these new
grains are relative to the cold-worked grains. The grains are so small at this point
that it is difficult to see them in the image. The process continues (Figure 2C) with
about half of the structure recrystallized. Now, you can clearly see which parts of
the structure have recrystallized and which are still cold-worked. Finally, Figure 2D
shows a completely recrystallized structure. These recrystallized grains are nearly
dislocation-free, although you cannot immediately determine this from the structure
shown in Figure 2D.

These microstructural changes occur because the alloy wants to attain a state of
lower energy. All the dislocations in the cold-worked alloy represent a lot of internal
strain in the structure. This is referred to as strain energy. It is just like the energy
you store when you stretch or compress a spring. A lower strain energy state would
be one that had many fewer dislocations in the structure. This is what happens
during Recrystallization where the atoms can rearrange themselves to remove the
dislocations. For Recrystallization to occur two conditions must be met; there must
be (i) enough dislocations in the structure, and (ii) a sufficiently high temperature.

The temperature for Recrystallization to occur (called the Recrystallization


Temperature or TRex) is usually about one third to one-half the melting temperature

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of the alloy. However, this temperature is also a function of the amount of cold work
done to the alloy – as you will discover in this laboratory.

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A B

C D

Figure 2. The microstructural changes that occur during the process of Recrystallization for α-brass.
Original magnification: 75x.

Mechanical Property Changes During Annealing


The overall reason for annealing is to reverse the effects of cold work on the
mechanical properties of the alloy. Recall that following cold work the alloy is rather
strong but not ductile. As the alloy is annealed, the yield strength and ductility
change drastically (Figure 3). Once again, the major activity occurs during the
Recrystallization stage. It is important to connect the behavior shown in Figure 3
with the microstructural changes depicted in Figure 2.

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Yield Strength

Figure 3. Mechanical properties as a function of the microstructure during the three stages of the
annealing process.

Processing & Properties


We can look at the bigger picture here, and this is important in materials
engineering. The cold work–annealing cycle is an example of how processing can
profoundly change a material’s properties. This is a constant theme in materials
engineering. We can use this information to design materials (engineering alloys in
this case) with a suitable microstructure to achieve the desired properties for a given
engineering application.

Safety First
1. Take care and follow instructions when using the rolling mill and the annealing
furnace.
2. Your instructor will explain and demonstrate the proper operation of the rolling
mill. Make sure your hair is tied back and you have no loose clothing.
3. The brass samples are hot when they come out of the furnace, take care.

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Lab Snapshot
You will explore the effects of cold work and annealing on the hardness (strength) of
α-brass. You will cold roll three brass samples to specified amounts of cold work and
measure the resulting hardness. Then you will anneal the samples at a range of
temperatures for 12 minutes each and measure the resulting hardness after each
annealing treatment.

Directions
Initial Specimen Conditions, Furnace Set-Up
1. Three α-Brass Samples. Locate the three α-brass specimens at your lab station.
These are in the annealed condition. Label the samples 1 to 3.
2. Furnace at 350°C. Make sure the tube furnace is set at 350°C and is up to
temperature. The needle on the small scale near the POWER switch should be in
the middle. Be careful, the furnace tube is hot.
3. Thickness Measurement. Using the micrometer attached to the rolling mill,
measure the initial thickness (t0) of each specimen to within 0.001" (it should be
close to 0.125"). When using the micrometer, use the small knurled knob to
tighten it. This knob has a clutch in it and will not allow you to overtighten the
micrometer. Do not overtighten the micrometer. Take multiple thickness
readings and determine the mean thickness value for each sample. Record the
values in your lab notebook.
4. Initial Hardness Measurement. Ask your instructor to demonstrate the use of the
hardness testing machine. Measure the initial hardness of the α-brass samples
using the Rockwell E scale (HRE = hardness Rockwell E). Take three
measurements of each sample (all on the same side of the sample, make sure
the impressions do not overlap). Use the “Statistics” program on the hardness
tester to determine the mean hardness value for each sample. Record all the
hardness values in your lab notebook.

Cold Rolling
1. Cold Working Ranges. Your goal is to cold work your samples to three specific
ranges (approximately) of percent cold work as shown in the table below.

Specimen Cold Work


1 2.5% ±0.5%
2 15% ± 1.0%
3 35% ± 1.0%

2. Determining Target Thicknesses for %CW. Using the formula below, calculate
the final thickness (tf) for each level of cold work. These final thickness values
will be your targets for cold rolling the samples.

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3. Cold Rolling Overview. Cold rolling works best when done in small increments.
Each pass through the rolling mill will reduce the thickness a small amount. So,
you will be incrementally rolling your samples, reducing the thickness by small
amounts with each pass through the rolling mill, until you reach each target
thicknesses. You must work carefully, though – the first level of cold work,
2.5%, represents only a slight amount of thickness reduction.

You will be rolling a sample, making a thickness measurement, comparing that


with your target value, adjusting the rolling mill, and continuing this progression.

Take Note!
A. Do not take too large of a reduction (10 thousandths of an inch, max.) on a single pass
through the rolling mill. It will damage the mill and alter the lab results.
B. Do not cold roll beyond 35% cold work.
C. Do not put anything other than brass samples through the rolling mill.

4. Rolling Mill Operation. Ask your instructor for rolling mill instructions.
5. Cold Rolling & %CW Calculation. Carefully cold roll your samples to your target
thickness values. Once you reach your final thickness values, use each specific
value of thickness to determine the precise amounts of cold work for your
samples.
6. Cold-Rolled Hardness Measurement. Measure the Rockwell E scale hardness for
your cold rolled samples. Take three measurements and calculate the mean for
each sample.

Annealing Cold Worked Samples


1. Sample Tray in the Furnace. On the left-hand side of the tube furnace is a
wooden handle. Attached to this wooden handle is a tray that slides inside the
tube of the furnace (Figure below). All three of your samples will go on this tray
for each annealing heat treatment.

Wooden handle Sample tray

2. Annealing Time & Temperature. Each annealing heat treatment will be done for
12 minutes. The annealing temperatures will be: 350ºC, 425ºC, 475ºC, and
525ºC.
3. Placing Samples in the Furnace. Pull out the sample tray from the furnace and
place all three samples in it. Separate the samples a bit so they can heat evenly.
It is fine if the samples touch each other. Slide the sample tray back into the
furnace.

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4. Water Quenching Samples. After 12 minutes has elapsed, slide the tray out of
the furnace and tip it down to let the samples fall into the water bath. Retrieve
the samples with tongs and dry them with a paper towel.
5. Set Furnace to Next Annealing Temperature. Increase the furnace temperature
to the next annealing temperature. It takes about 10 minutes for the furnace to
reach this next higher temperature.
6. Hardness Measurement After Anneal. Measure the hardness values of all three
samples after annealing at a given temperature. Take three measurements,
calculate the average, and record these in your notebook.
7. Repeat Steps 3-6 for Remaining Annealing Temperatures. Repeat the annealing
heat treatment & hardness measurement for the remaining three temperatures.
8. Furnace Reset. After you have completed annealing, reset the temperature to
350°C. You can turn the furnace OFF.

Plots & Questions


Plot 1. This plot deals with your cold worked samples before annealing. Make a plot
of the HRE readings (y-axis) vs. %CW (x-axis). It is best to use nearly a whole page
in your notebook for the plot. Be sure to include your as-received (0% cold work)
sample hardness. Draw a smooth curve through your data points.

Question 1. Explain the trend shown by the data in Plot 1. Your explanation should
be based on the microstructure of the material. Do not simply say that the hardness
increases or decreases with %CW, your task is to explain why this occurs.

Plot 2. This plot deals with your annealed samples. Make a plot of the HRE readings
(y-axis) vs. Annealing Temperature (x-axis) for each of your brass specimens. It is
best if this plot takes about 2/3rds of a page in your lab notebook. Include the
average hardness value obtained after cold working (HCW’d) for each sample as the
room temperature data point for each sample. Show the results of all three
specimens on the same plot. It is OK to connect-the-dots (data points) with a
straight line for each sample instead of drawing a smooth curve through your data.
Use different data markers or symbols for each sample, and include a legend that
includes the % cold work on each sample.

Indicate on your plot the Recrystallization Temperature for each sample. This is
going to be associated with a drastic decrease in hardness value.

On a separate page of your notebook, address the following questions about Plot 2.
Note: your explanations should be based on the microstructure of the material. Be
sure you explain the reasons behind the trends in the data instead of simply stating
the trend.
Question 2. Consider your 15% cold worked sample. Explain why the hardness
varies with annealing temperature.
Question 3. You have marked the Recrystallization Temperature for each of your
samples on your plot. Explain the reasons why the value of TRex changes with the
amount of cold work.
Question 4. Nitinol is a nickel-titanium alloy famous for its “shape memory” and
“superelastic” properties. It is common for Nitinol wire to undergo a lot of plastic

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deformation during processing to a small-diameter wire (called wire drawing) for
medical applications. Here’s a problem based on that.

A Nitinol wire sample originally 2 mm in diameter is drawn through a series of dies at


room temperature to a diameter of 0.75 mm. Calculate the percentage of cold work
put into the Nitinol. Note: Simply using thickness = diameter will not produce the correct
answer. Brainstorm with your team members about how to solve this problem (rather than
just asking your instructor). Think of what is physically happening to the wire during wire
drawing… a sketch or two may help.

Question 5. Let’s use the results from Question 4. Your goal is to produce fine
diameter wire (0.10 mm dia) from 2-mm diameter stock for a stent delivery wire.
You know from experience that if you tried to draw the 0.75-mm dia. wire (from
Question 4) any smaller at room temperature it would fracture. So, based on your
experiment, briefly list the processing steps you would use to make your 0.1-mm
diameter Nitinol wire from the 2-mm diameter stock. The final 0.10-mm diameter
wire needs to be relatively strong for the application. You may use calculations to
quantify the specifics.

Notebook Check
• Data: thickness & hardness values
• Plot of hardness vs. % cold work (Plot 1) with an explanation of reasons behind
the trend based on the microstructure (Question 1)
• Plot of hardness vs. annealing temperature for each specimen with the
recrystallization temperatures shown (Plot 2)
• Structure-based explanation of the reasons that the hardness changes with
annealing temperature and why the recrystallization temperature changes with
the amount of cold work (Questions 2, 3)
• Answers to Questions 4, 5 (Q5 has a good amount of detail including
calculations)

Clean Up
• Reset the furnace to 350°C and turn it off.
• Recycle the rolled brass samples (container may be near the sinks in the lab).
• Generally look around your lab area to make sure it is clean and well organized
for the next lab team’s use.
• Push the stools underneath the lab table.

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