MET 264 Lab 6 – Heat Treatment and Metallurgy

Objective
1. Increase understanding of heat treatment
2. Learn metallurgical sample preparation
3. Study the importance of each step within this process
4. Understand why it is necessary to use the mounting, polishing, and etching
processes
5. Evaluate the different grain structures

Introduction
Metallography is the study of microstructure of metals and alloys using a microscope.
Preparing, interpreting, and analyzing microstructures in materials allows us to better
understand their behavior and performance. In order to evaluate different material structures,
we will subject one type of steel to five different heat treatment techniques. We will also
evaluate how those techniques change the hardness of the material.

Figure 1: TTT Diagram for steel

Heat Treatment (Steel)
Heat treatment of the five samples your group has been given.
Table 1: Heat treatment steps for steel samples
Sample Number Initial Action Secondary Heat Treatment
1 CONTROL (NO HEAT TREATMENT) Control – No heat treatment
2 Harden samples 2, 3, 4,5 as follows: HARDENED Sample 2 – has
 Coat the four samples in anti- already been hardened to the
scaling compound to reduce martensitic structure.
oxidation and decarburization Requires no further heat
during treatment.
3 the heating process. TEMPERED Sample 3 –
 Heat the four samples to 1550 - Place the hardened sample 3
1600 °F for 30 minutes in a in a furnace treated to 700°F
preheated furnace. Heat sample for 30 minutes at
 Quench the samples in 700°F
Air cool sample
4 a water bath NORMALIZED Sample 4 –
 Upon cooling, treat sample: Place the hardened sample 4
in a furnace treated to 1600°F
Heat sample for 30 minutes at
2 as HARDENED 1600°F
Air cool sample
5 3 as TEMPERED ANNEALED Sample 5 –
Place sample 5 in a furnace
4 as NORMALIZED treated to 1600°F
Heat sample for 30 minutes at
5 as ANNEALED
1600°F
Shut down furnace and leave
sample to cool inside furnace
*Notice the similarities between the Normalized and Annealed procedures
Hardness Testing
Material Testing Steps
1. Make sure the material, indenter, and platen are clean
2. Pick the spot for your first test
a. Make sure that all test locations are at least 3 mm from the edge of the
specimen and not too close to each other
3. Install the appropriate indenter tip into the tester
4. Make sure you know the appropriate major and minor loads for your scale
5. Measure the hardness of each of the heat treated specimens using Rockwell C.
a. Each sample should have the hardness measured at least three times on this
scale and averaged.
Standard Procedures for Metallography
Compression Mounting:
Key Safety Points:

Compression molding is typically performed at 300°F. Proper gloves must be worn when
the potential of hot surfaces exist.

Should the ram become stuck during the removal step, the pressure built up until the
mold releases is considerable and can cause injury. To minimize the risk, use a mold release on
the ram sides and top surface, as well as the ram cap. DO NOT put hands and face near or over
the ram during the ejection step.
Mounting Steps:
1. Turn the oven switch to ON, then push the line button to pre-heat the machine. Watch
for the pilot light to go off. This will indicate that the correct temperature has been
reached.
2. Push the ram button to expose the ram.
3. Set system pressure to 4200 PSI (should be done prior to placing specimens in).
4. Place the selected heat treated specimen as close to the center of the ream as possible.
5. Place the 1.25” diameter phenolic pre-mold directly on top of the specimen. Try to place
the pre-mold to maintain the specimen as close to the center of the ram as possible.
6. Place the screw guide on top of the pre-mold, making certain not to shift the assembly.
7. Push the ram button to retract the ram into the cylinder. When fully retracted, screw
the top all the way down then back off a half turn.
8. Push the ram button once more to activate compression within the chamber.
9. Set the timer for 5-6 minutes.
10. When time goes off, turn off and remove the heater. Replace with cooling sleeve.
11. After 2 minutes, remove the cooling sleeve and cool under cold water. Put sleeve back
in place for 2 minutes.
12. Push ram button to remove the pressure.
13. Using gloves, unscrew the guide (if it does not move, use a mallet and bar to back the
ram off the guide due to the applied pressure).
14. After the guide is unscrewed, push the ram button to extend the ram.
15. Remove the mounted specimen. Scribe an identification mark on the side opposite the
specimen.
Preparation for Polishing:
Materials:
The following materials are need to perform the grinding, polishing, and etching steps:

 Allen driver or screw driver to fit the chuck of the polisher sample fixture
 Polishing platens (aluminum and/or magnetic base).
 3 sheets of 120 grit grinding paper.
 2 sheets of 240 grit grinding paper.
 2 sheets of 400 grit grinding paper.
 2 sheets of 600 grit grinding paper.
 Texmet and Trident polishing cloths (1 each).
 1 final polishing cloth (choice of Microcloth, FinalPol, Red Final C, DP Nap)
 15 micron diamond paste and suspension.
 3 micron diamond polishing paste and suspension.
 Diamond extender (Metadi Fluid or Green Lube)
 Methanol or ethyl alcohol for cleaning samples.
 Distilled water in bottle.
 Bottle of 0.05 micro alumina (if mixing from powder, clean use DI water)
 Solution of 3% nitric acid in methanol (Nital) for etching
 Soap and water source
 Clean air source for drying samples or hot air dryer.
Assembly:

 Assemble the mounted samples into the polishing fixture. They must be evenly
distributed by hardness and sample size.
 Tighten the samples into the clamp using heavy hand pressure (20 pounds max).
 Set the automatic polisher to 150-200 RPM (platen speed).
 Set the polisher head to 18-20 PSI and “Contra” direction (switch on rear)
Operation:
Rough Grinding:
1. Place a 120 grit grinding paper on the polisher platen, minimizing the presence of air
pockets.
2. Using the above initialized settings, run the specimens for 1 minute, with water as a
lubricant.
3. Remove fixture and inspect samples for complete sanding across all samples.
4. Repeat this 120 grit grinding step until all samples are sanded across their entirety,
changing the 120 grit paper every other grinding cycle.
5. Remove the fixture from the polisher and clean them with running water. Dry
immediately to prevent corrosion.
6. Place a 240 grit grinding paper on the polisher platen, minimizing the presence of air
pockets.
7. Using the above initialized settings, run the specimens for 1 minute, with water as a
lubricant.
8. Repeat the 240 grit for a total of 2 cycles, using a new paper each time.
9. Remove the fixture from the polisher and clean them with running water. Dry
immediately to prevent corrosion.
Fine Grinding:
1. Place a 400 grit grinding paper on the polisher platen, minimizing the presence of air
pockets.
2. Using the above initialized settings, run the specimens for 40 seconds, with water as a
lubricant.
3. Repeat the 400 grit for a total of 2 cycles, using a new paper each time.
4. Remove the fixture from the polisher and clean them with running water. Dry
immediately to prevent corrosion.
5. Place a 600 grit grinding paper on the polisher platen, minimizing the presence of air
pockets.
6. Using the above initialized settings, run the specimens for 40 seconds, with water as a
lubricant.
7. Repeat the 600 grit for a total of 2 cycles, using a new paper each time.
8. Remove the fixture from the polisher and clean them with running water. Dry
immediately to prevent corrosion.
Rough Polishing:
1. Clean a polishing platen and place a sheet of Texmet cloth on it, making sure not to
create air pockets.
2. Place the platen on the polisher without touching the polishing surface. Contamination
must be avoided.
 3. Direct the water hose away from the platen.
4. Set polisher speed (platen) to ~100 rpm.
5. Wash Hands and keep clean.
6. Spread some 15 micron diamond paste (roughly 7-8 inches from tube) onto the
polishing cloth.
7. Add some diamond extender and spread again.
8. Set polisher to concurrent head direction, and timer to 2 minutes.
9. Polish specimens for 2 minutes, adding alternating applications of diamond extender
and diamond suspension (15µ).
10. Remove the fixture from the polisher and clean them with soap and running water. Add
methanol or ethyl alcohol to displace the water. Dry immediately to prevent corrosion.
11. Clean a polishing platen and place a sheet of Trident cloth on it, making sure not to
create air pockets.
12. Place the platen on the polisher without touching the polishing surface. Contamination
must be avoided.
13. Direct the water hose away from the platen.
14. Set polisher speed (platen) to ~100 rpm.
15. Wash Hands and keep clean.
16. Spread some 3 micron diamond paste (roughly 7-8 inches from tube) onto the polishing
cloth.
17. Add some diamond extender and spread again.
18. Set polisher to concurrent head direction, and timer to 2 minutes.
19. Polish specimens for 2 minutes, adding alternating applications of diamond extender
and diamond suspension (3µ).
20. Remove the fixture from the polisher and clean with soap and running water. Add
methanol or ethyl alcohol to displace the water. Dry immediately to prevent corrosion.
Final Polishing:
1. Clean a polishing platen and place a sheet of final polishing cloth on it, making sure not
to create air pockets (see choices in materials list).
2. Manually start the polisher and fully wet the wheel with distilled water.
3. Apply 0.05µ alumina suspension to cloth.
4. Set polisher to concurrent head direction, and timer to 40 seconds.
5. Polish specimens for 40 seconds, adding polishing suspension as needs to keep
lubricated.
6. Remove the fixture from the polisher and clean with soap and running water. Add
methanol or ethyl alcohol to displace the water. Dry immediately to prevent corrosion,
preferably with a duster can or an air dryer (oil residue and water may be present in
compressed air).
Etching:
1. With the samples still in the sample holder, apply a small amount of the Nital solution to
each specimen, until the specimen begins to cloud or frost over.
2. Clean immediately with soap and running water. Add methanol or ethyl alcohol to
displace the water. Dry immediately to prevent corrosion, preferably with a duster can
or an air dryer (oil residue and water may be present in compressed air).
3. Polish specimens for 10 seconds, adding polishing suspension as needs to keep
lubricated.
4. Remove the fixture from the polisher and clean with soap and running water. Add
methanol or ethyl alcohol to displace the water. Dry immediately to prevent corrosion,
preferably with a duster can or an air dryer (oil residue and water may be present in
compressed air).
5. Remove the samples from the sample holder and re-clean them per previous step.
6. Apply a small amount of the Nital solution to each specimen, until the specimen begins
to cloud or frost over.
7. Clean with soap and running water. Add methanol or ethyl alcohol to displace the
water. Dry immediately to prevent corrosion, preferably with a duster can or an air
dryer (oil residue and water may be present in compressed air).
8. Check etch quality on microscope. Re-polish and re-etch if needed.

Analysis
What is the grain structure of each specimen?
What is the hardness?
Why are the hardness measurements different?
How did the heat treatment affect the grain structure?
Compare the different types of heat treatment.