ME83L – Structure/Properties of Solids

Fall 2004

Lab #5 - Metallography Lab

Introduction

In this lab, we will investigate the relationship between material composition, processing,
structure, and properties in practice, and evaluate how this ultimately relates to the
performance of a material for a particular application. This lab will focus on the most
widely used engineering material in our society, steel. Of all metallic materials, ferrous
alloys (steels) are used more than 90% by weight than any other. Ferrous alloys represent
an immense family of engineering materials with a wide range of microstructures and
related properties. The majority of engineering designs that require structural load
support or power transmission involve ferrous alloys.

General types of ferrous alloys are:

 Carbon steels
 Alloy steels
 Tool steels
 Stainless steels
 Cast iron

Metallography is the study of metallic microstructures and has been developed to be an

indispensable technique over the past three centuries. For example, metallography is
used for:

 Quality control in metal processing

 Failure analysis
 Alloy compositional analysis
 Alloy development.

The key to obtaining an accurate interpretation of a microstructure is a properly prepared

specimen that is truly representative of the material being examined. A properly prepared
metallographic surface must:

 Be flat, free from scratches, stains, and other imperfections that tend to mar the
surface,
 Contain all non-metallic inclusions intact,
 Show no chipping or galling of hard and brittle intermetallic compounds,

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  Be free from all traces of disturbed metal.
To achieve metallographically useful surfaces, sample preparation must be carried out,
accurately and with a clear understanding of what must be accomplished during each
specific stage. The most straight-forward approach is to divide the entire process into a
logical series of stages involved and deduce the purpose of each. The stages of
preparation are as follows:

1. Sectioning. Sectioning is the removal of a representative area from the parent

piece. The microstructure must not be altered in the process. Heat or cold
working are the two most likely conditions which would quickly bring about
structure changes. This step has already been done for you (about ½ inch
diameter rods were sectioned into roughly 3/8 inch lengths).
2. Coarse grinding. The purpose of coarse grinding is to remove deformation
produced during sectioning and to provide the initial flat surface. A secondary
purpose may often be to remove gross amounts of surface material for
microsample preparation or macroetching.
3. Mounting. Metallographic samples are mounted primarily for ease of
manipulation and for edge protection during preparation.
4. Fine grinding. The abrasives used for fine grinding are Silicon Carbide, Emery
and Aluminum Oxide. Generally, fixed type abrasives are used, i.e., the abrasive
grain is bonded to the paper or cloth backing. In this lab we will be using Silicon
Carbide paper. (Note: This is not sand paper). Wet grinding is preferred as it
offers a flushing action to prevent the surface from becoming clogged with
removal products. Flushing will also keep the cutting edges of the abrasive
grains exposed.
5. Polishing. This stage is considered the most important in the entire preparation
sequence. Polishing serves to remove any deformation resulting from grinding.
Here, a uniformly polished and scratch-free surface must be produced. Care
must be taken to insure removal of any and all surface deformation introduced by
grinding. If this is not accomplished, scratches may still be apparent in the
unetched state. The same artifacts will appear to an even greater extent if any
proceeding steps or stages have not been properly accomplished.

The previously listed stages are detailed with step-by-step procedures in the following
sections. After performing the sample preparation stages, the sample will be etched.
Etching is a procedure that reveals structural details through differential removal of
various surface compounds of a metal surface by preferential attack with an acid or basic
chemical solution. A micrograph of the etched sample surface will often be obtained, for
example by capturing a digital image of the etched sample surface in a light microscope,
and the sample’s microstructure can then be analyzed to gather information such as grain
size, carbon content, and phases present. Mechanical tests, such as hardness testing yield
information by which mechanical properties can be correlated with a sample’s
microstructure.

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Laboratory Logistics

Students will work in teams of three (or two if an odd number). Each team will receive
three samples of a particular steel type. They will be labeled with a number and letter.
The number represents the type of steel (see list below) and the letter is the unknown type
of thermal processing condition. The following is a list of common ferrous alloys and
note that the * denotes the ones chosen for this lab. All of these ferrous alloy samples
were originally obtained from 6 ft long ½ in diameter rods, sectioned to 3/8 inch lengths.

List of commonly used ferrous alloys

 1010 carbon steel  8620 alloy steel
 1018 carbon steel*  W1 tool steel
 1045 carbon steel*  P20 tool steel
 1144 carbon steel*  304 stainless steel
 A36 carbon steel  410 stainless steel
 4140 alloy steel*  Grey cast iron ASTM A48
 4340 alloy steel

The three different types of processing conditions:

 As-received: It has not been processed after received from the manufacture.
 Annealed: Heat treated to 900oC, held about 15 minutes, then slowly cooled in the
powered off furnace (cooled over night).
 Quenched: Heat treated to 900oC, held about 15 minutes, then removed from
furnace and immediately placed in bucket of water to cool the sample in seconds.

Each team member should prepare and analyze one of the samples. Make sure you
remember which sample type you received and do NOT mix-up the specimens, as the
microstructures and hardness properties are different. It is the job of the team to work
together to discover what type of steel they have and how each sample was processed.
Your team will accomplish this from both experimental and library research. You must
justify your conclusions with micrographs and hardness values of the samples, along with
literature sources. Each team member will write up their own report, while each team
will give a 10 minute presentation in lab sections on November 17th or 19th (depending on
your section).

On the next page is a summary of what we will be doing in lab over the next few weeks.
This lab is a bit more involved than the previous ones. It is your responsibility to keep up
and finish the lab on time, since you are working as a team. Following the summary, all
lab procedures and report requirements you will need to know to complete this lab are
described below, including: sample mounting preparation, grinding, polishing, etching,
microscope observing, image capture, microstructure interpretation, hardness testing,
technical report expectations, and presentation expectations. Some of these procedures
are similar to ones previously handed out, but have been slightly modified for this
particular lab. Be sure to read them!

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Lab Summary

Here is a summary of what we will do over the next four weeks. Items in bold are items
that your team needs to accomplish before we meet the following week. Please
follow the suggested time frame and get the work you need done as we go along. You
cannot finish all of the lab work, report writing, and presentation in the last week. You
should start on the report before the final week, add introduction/background material
and results as you go along. You will be dependent on the rest of your team for getting
this done and you may want to meet outside of lab time and work together to make sure
everyone is doing their part. It is up to you as a team to finish this project. Part of your
grade depends on the rest of the team.

November 3/5, Metallography

In the first metallography lab session, you will learn how to polish and etch the sample in
order to observe its microstructure. First we will discuss overall goal of the laboratory,
then determine teams of three (come up with a team name), hand out samples to teams
and briefly review standard designations of steels and compositions. Then we will go to
the lab and while half of the lab learns to polish and etch their samples, the other half will
learn how to use a microscope and how to capture an image to the computer.
Mount sample in puck, grind (180, 240, 320, 800 grit), polish (1 m alumina),
observe on microscope, and capture image on computer. Lab 4 is due next week.

November 10/12, Optical Microscopy and Quantitative Metallography

In the second lab session, you will learn how to observe the microstructure with a light
microscope and perform qualitative metallography on an image (find grain size, % phases
present, etc). You will also learn the basics of the optical microscope. In addition, you
will have time to ask questions about your results, the report, and team presentation. This
is a good time for your team to discuss the oral presentation.
Polish/etch sample, acquire representative digital images of microstructure,
hardness test, and Lab 6. Oral presentations are next week.

November 17/19, Metallography Oral Presentations

Team presentations lasting 10 minutes: Be sure to submit your teams PowerPoint

presentation to your TA by noon the day of your presentation. ONLY FLOPPY DISKS
OR CDS WILL BE ACCEPTED. Lab 5 reports will be due on December 1/3.

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Sample Mounting Preparation

You will use a standard sample mounting technique that is often used for preparing metal
samples for metallographical evaluation. The steel samples you have received are
already pre-cut to match the size requirements for the “sample pucks” you will be
molding. For mounting you will be using a thermosetting mold material (Bakelite).
Bakelite is a thermosetting, crosslinked phenol-formaldehyde polymer that is thermally
stable, resistant to organic solvents, and hard which helps to preserve edge-definition of
the sample. Bakelite is a thermosetting plastic; therefore pressure must be maintained
while it is at the molding temperature. Be careful when handling the equipment and
mounted samples, initially they are quite hot. Before molding, if necessary, first level the
sample surface by a coarse grinding using the 120 or 180 grit SiC paper to get a relatively
flat surface.

Step-by-Step Procedure
1. Preheat the mold by placing the heater on mold with top in place for 15 minutes
(leave heater in place and ON until step 11.)
2. Remove top by unscrewing, making sure to wear gloves.
3. Close valve and pump up bottom piston until you can see the piston well enough (this
will take about 60 pumps).
4. Carefully clean off the top of the piston with a glove (there may be bakelite left from
the previous preparation.)
5. Position sample in the middle of the piston with the cross section you want to observe
facing down towards the piston.
6. Slowly open valve to retract piston all the way to the bottom.
7. Pour in approximately 35 mL of Bakelite powder. (Do not use too much).
8. Replace top (only snug tight, do not over tighten).
9. Close valve and pump to 4.2 kpsi (inner rod dot for the 1 ½ inch mold size).
10. Maintain pressure for approximately 15 minutes while still heating.
11. Turn off and remove the heating unit and then place on the holding rack.
12. Place cooling fin over mold for 5 minutes or until a noticeable drop in pressure
occurs.
13. Open valve and then remove top.
14. Close valve and pump up sample puck. (Use gloves to remove sample since it will be
hot!)
15. Replace top and clean up.
16. Allow the puck to cool down approximately 10-15 minutes before moving to next
step.
17. Use the electric scribe to label the back of the mount with important information (type
of steel, processing letter, and initials). If you prefer you can use a marker or white
out instead.

NOTE: After preparing the puck, it can be stored in the metal cabinet for further use at
a later time. Be sure to label it and place in drawer of your lab section so you
can identify it later.

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Grinding Procedure

The embedded specimen now needs to be prepared for hardness testing and/or
microscopy. This requires a grinding and polishing procedure that will yield a smooth
and flat surface. Also, with the microscope setup we have in the lab, the puck thickness
cannot be greater than 20mm. If your puck is greater than 20mm, you will not be able to
focus on the sample, and then you must grind down the backside of the puck (opposite
side of the sample) using the 120 or 180 grit paper. You should take care in grinding this
specimen, since you will be observing and taking an image of it. If there are scratches
remaining or it is not flat, it will be much harder to analyze the sample.

Grinding Step-by-Step Procedure

1. Turn on grinding wheel by the switch on the right front.
2. Position the water faucet over BOTH wheels and then turn the water on.
3. Start on grinder with the coarsest paper (180 grit).
4. Bevel sharp edges of the mount (on both the front and back).
5. Hold the mount flat against the grinding surface and grind without turning the
specimen until it is flat and the entire specimen is streaked in a single direction.
The purpose of this step is to remove the deformation produced during sectioning,
and to produce an initially flat surface. This is a very important step. If done
correctly, the remaining steps will be much faster and easier. Try to avoid lifting
the specimen from the wheel as much as possible, repositioning will frequently
lead to a faceted surface rather than a flat one!
6. Remove old abrasive by washing under running water (use liquid detergent if
available).
7. After the coarsest paper, proceed to the next less coarse paper. (Leftmost grinder
= 180 and 240 grit, rightmost = 320, 400 or 800 grit). Turn sample puck 90 and
grind top surface on next finer sand paper. This reduces the lines created by
grinding. Repeat the last two steps (grinding and washing) until you arrive at the
finest grit paper.
8. Turn off faucets and replace them in the center position. Allow for all water on
the wheels to dry off before turning them off.

NOTE: When grinding the mounted samples, be extremely careful not to grind your
fingertips. The cold water from the faucet “numbs” your fingers and you will
not feel it until it is too late!

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Polishing Procedure

Polishing is the next step after grinding, in preparing a sample for observing its structure
in the microscope. The object of polishing is to get a flat, mirror-like surface with no
trace of smearing. Polishing is a technical art, learned by experience, but the basic steps
of the process are quite simple.

Polishing Step-by-Step Procedure

1. Make certain that the sample has been ground through 600 or 800 grit SiC paper
and that the edges are beveled (to avoid tearing the cloth on the polishing laps).
Note: If hardness indentations are present, it is not necessary to remove them
completely; but the “lips” around the indentations should be ground down.
2. Wash the sample and your hands thoroughly (to avoid carrying dirt and SiC grit
onto the polishing laps).
3. Use rotating lap wheel labeled 1 m.
4. Turn wheel speed to 0, turn ON wheel by the switch on top, then turn up wheel
speed to 30.
5. Squeeze a suspension of one-micron alumina in distilled water onto the lap.
6. Polish puck surface by rotating your sample in a direction opposite to that in
which the lap rotates (this eliminates “directional polishing”). Concentrate on
keeping the sample level, and on applying uniform pressure. Polishing should
take 5-15 minutes, depending on the hardness of the metal.

Use enough pressure that you feel the resistance of the wheel but not so much that
the wheel starts to “drag” the sample or so much that the alumina suspension
splashes over the machine.

If the alumina - water suspension “froths” on the wheel, dilute it with distilled
water. If the wheel becomes dry and feels like it is “dragging” the sample, put
more water or alumina - water suspension on the polishing lap.

7. COVER THE ROTATING LAPS WHEN NOT IN USE. If they are not covered,
dirt particles fall on them and become embedded in the polishing cloth. (Even if
only walking away to observed on the microscope for a minute).
8. Observe with microscope (see next section).
9. Turn off and cover.

The wetness of the cloth with water has a great bearing on the end result. If the cloth is
too wet, the sample can show pits; if too dry, buffing and/or smearing can result. To
determine proper wetness, remove the sample from the wheel and check the time
necessary for the polishing film to dry. In general, this should take no longer than five to
eight seconds. To check for abrasive addition, note the color and consistency of the film.
The film should not be opaque, but rather sufficiently transparent to reveal the sample
shape and luster.

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After polishing observe with microscope

See “How to use a microscope” if you have never used this microscope before.

A sample always should be viewed before it is etched, both to determine the quality of
the polish and to look for any features which might be masked by etching.

See “How to Interpret Microstructure”- “on as polished surface” and make notes for your
report.

1. Wash the sample thoroughly. Spray the surface with some alcohol, and dry in a
warm air blast. (Use red “hair dryer”).

2. Look for traces of parallel, directional scratches from the grinding operation. Their
presence means the sample was not polished long enough.

3. If your sample was polished on a rotating lap, and exhibits a few criss-crossed, fine
scratches, they are from dirt particles which have become embedded in the polishing
cloth. Don't waste time trying to eliminate these scratches; just don't interpret them
later as something “significant”.

4. Put your sample on the microscope, and examine the surface at low power. Make a
sketch of a typical field of view, and make a record of any unusual markings (phase
distributions, plated surfaces, etc.) which appear. Many of these will show up better
on this polished surface than they will later, when the sample is etched.

A metallographic specimen in the “as polished and unetched” state will reveal inclusions,
porosity, cracks, intergranular corrosion, surface conditions, etc.

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Etching Procedure

Etching is a controlled chemical attack of the material's polished surface, designed

to delineate the details of the microstructure. The etching of a properly polished metallic
sample may show one or more (but not necessarily all) of the following:
a. grain size (average crystal size)
b. the effects of special heat treatment
c. the existence of surface hardening
d. the presence of plating on the surface
e. working direction of a cold-worked metal, provided the normal to the
polished surface is not parallel to the working direction
f. effects of localized heating, or overheating
g. presence of welds, brazed joints, etc.
h. the carbon content of a slowly cooled steel
i. phase distributions (carbides in a tool steel or graphite in gray cast iron).

There are many different etchants in the technical literature but for steel and cast iron the
general-purpose one is 1/2% - 4% HNO3 in alcohol (called “Nital”).
KEEP THE ETCH AWAY FROM EYES, FINGERS, CLOTHES, ETC.; it is not terribly
corrosive, but nitric acid does attack proteins.

Scratches may also be evident after etching. This signifies the deformed surface was not
completely removed. The etchant attack will be more severe and preferential along those
regions of localized deformation as they possess higher surface energy levels.

Etching step-by-step procedure

1. Put on gloves and safety glasses!
2. All etching should be done in a fume hood.
3. Turn on the water in the fume hood.
4. Hold the sample (in tongs) over the sink, and swab its surface with a cotton “Q-
tip” soaked in etch.
5. When the sample turns light gray and develops a matte appearance, put it under
running water to stop the etching attack.
6. Squirt the surface with alcohol or acetone, and dry it in a hot air blast. Do not use
paper towels as they may scratch the surface! DRY THE SAMPLE
THOROUGHLY BEFORE PUTTING IT ON THE MICROSCOPE STAGE. Look
at the structure in the microscope, and record your observations, and take a digital
image with the camera.
7. WHEN YOU HAVE FINISHED ETCHING, PLEASE CLEAN UP. Throw away
used pieces of cotton, (after cleaning the acid out with running water), paper
towels, etc. Wash beakers and put them on the drying rack in the hood.

In the past, the best results have been obtained by students who have repolished and re-
etched their samples one or two times. Apparently, this procedure removes more of the
“disturbed” metal produced by the grinding operation. For best results, etching should be
done to a freshly polished surface.

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How to Interpret Microstructure

On As-Polished Surface:

1. Look for signs of porosity, indicating shrinkage during casting or fabrication by

powder processes. Working may eliminate porosity by “healing” the pores, so in
general worked materials show no porosity.
2. Look for inclusions. Their shape, size and distribution may provide clues to the
processing history. Note, however, that you are looking at a two-dimensional
section; if it is transverse to the working direction, you will see no sign of the
working. Elongated inclusions suggest hot working. If inclusions have been
“pulled out” during polishing, the remaining pits will appear as black spots; they
are not carbon particles or porosity, just small holes which originally contained
inclusions.
3. Look at the cross-section near the surface for signs of plating, oxidation,
corrosion, cracking, etc.

On Etched Surface:

1. Estimate the average grain size, distance between phases and/or size of phases;
indicate the probable accuracy of your estimate.
2. Note whether most of the grains are elongated in the same direction. Such
elongation of the grains is a sign of cold-working; the amount of cold-work can be
estimated by assuming that the grain began as a sphere or cube or some other
“equiaxed” shape. Local distortion may be an indication of how the part was
fabricated
3. Look for signs of special heat treatment. In steels, a needle-like structure
indicates that the alloy was quenched to form martensite or bainite. Lamellar
regions are probably pearlite, suggesting that the steel was cooled slowly. If the
part was surface hardened, martensite should be visible on the surface, but mixed
with pearlite farther below the surface. If the steel is a tool steel, many small
carbide particles should be visible on a background of martensite. If the steel has
been forged without further heat treatment, the pearlite will have broken up into
scattered carbide particles to a ferrite matrix. Cast iron often has a matrix similar
to steel, but it also will have graphite (gray cast iron) or massive cementite (white
cast iron) distributed through the matrix.
4. Twins (regions with a grain, separated from the rest of the grain by parallel
boundaries) in equiaxed grains of a steel alloy usually mean that the crystal
structure is face-centered cubic, not body-centered cubic; it is particularly
characteristic of austenitic stainless steels.
5. Look for any particular distributions of phases which did not appear on the as-
polished surface; this may indicate something of the processing history.
6. If the part is plated, estimate the plating thickness; note its uniformity and how
well it is bonded to the substrate material.
7. If cracks or pores are present, check their locations with respect to other structural
details and with respect to how the part was stressed in service.

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How to use the microscope
Please remember the following things at all times when you operate the microscope:
a. Do not ever touch the lenses or filters with your hands. Skin oils can permanently
damage them, and cleaning can scratch them.
b. When changing magnification, move the objective into place by turning the turret
on which the lenses are mounted. Do not grab the objective itself. These
objectives are pre-centered, but abrupt movements can jar the adjustments and
loosen them from the turret.
c. Start with a low magnification (5x), and proceed to higher magnifications. It is
easier to find the focus with a lower magnification and it is less likely you might
accidentally crash the objective into the specimen since a lower magnification
lens has a larger working distance. Once the specimen is in focus with the lower
magnification objective, the higher magnification objective can be moved into
place and will be approximately in focus. For the 5X objectives, the sample will
be in focus when the objective is about 3/8 in. from the surface.
d. Try to keep the illumination voltage at about 5. Operating at high brightness not
only fatigues the eye, but prematurely burns out the bulbs.
e. The total magnification with which you view the samples is the product of the
objective magnification and the eyepiece magnification.
f. Never ever run an objective into the sample surface while focusing, this can
damage and scratch the objective lens permanently.
Microscope Step-by-step procedure
1. Turn the lamp on by the green switch on the right side (near the back) of
the microscope.
2. Turn the illumination knob (knob next to the power switch) to a setting
between 4 and 7.
3. Select the objective with the smallest magnification (5x).
4. Lower the stage one inches below the end of the objective (about length of
5x objective).
5. Position the specimen on the stage and while looking through the eyepiece
bring into focus by turning the focusing knob so the specimen is moving
away from the objective. In this way, you are always putting distance
between the objective lens and the sample as you focus the eyepiece, so
you can focus without risking damage to the lenses.
6. Adjust the iris diaphragm of the illuminator so there is no glare, but note
that too small an opening will reduce the resolving power of the
microscope.
7. Adjust for the distance between your eyes by sliding the eyepieces
together or apart.
8. Adjust the field iris diaphragm. If you pull the slider all the way out, you
will see a 10 sided polygon of light. Slowly push the slider just until the
polygon is out of view and the light shows a circular pattern.
9. Move the specimen by rotating the stage control knobs.
10. When finished, always leave it with either no objective or the lowest
power objective in line with the microscope barrel, remove your specimen,
power off the illuminator, and cover the microscope with plastic cover.

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The microscope shown below is similar to the one in the materials lab. The major
components are labeled. Become familiar with each component and its purpose. The
aperture and field iris diaphragm have one slider knob and two that are used for centering
purposes.

Light port
Video camera
Lamp

Filters

Eyepiece Aperture Iris

diaphragm

Field iris diaphragm

Objectives
Illuminator knob
Stage
Power switch
Stage control
Focus knob

The figure below shows a schematic of the reflected light path internal to the microscope.

The resolution of a light microscope can be estimated by the following equation:

where  is the wavelength of light and NA is the numerical aperture of the objective. The
NA is printed on the objective itself. The terms resolution and numerical aperture will be
further defined in Lab 6 on the Light Microscope and Quantitative Metallography.

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Video viewing and capturing images on a computer

Viewing video from the microscope

1. Setup microscope for viewing (see previous section)
2. Start up computer (press cancel if asked for password)
3. Run the “ATI video player” program (should be an icon on the desktop)
4. Press OK initial info box that states “Your channel list is currently empty”.
5. Pull the video port knob all the way out (this switches the path of the light to the
video camera at the top of the microscope instead of the eyepiece).
6. Image should now be displayed on the computer monitor.

Capturing digital images

1. Setup microscope and computer as stated above.
2. Focus image as viewed on the computer monitor
3. Press the capture still button just below the image. It looks like a still camera, not
a video camera which will capture video, capturing video is not necessary for this
lab.
4. The still image will pop up. If you want to save the image, press the disk button.
5. Title the image with an appropriate name that will distinguish it from any others
you take with the sample name, objective used, location on the sample, whatever
is important.
6. Change the file type to a “Windows BMP 8” (this file type can be directly opened
with the image program later)
7. Save it to your ME83 sections folder on the desktop and in a folder for your team.
8. To transfer the image to your acpub account, see the next section. Alternatively,
you can email it to yourself or copy it to a floppy.

How to transfer file from lab computer to your account

1. Open SSH secure file transfer client (should be a shortcut on the desktop)
2. Press quick connect (press OK if an error type box pops up)
3. Type in host name: godzilla.acpub.duke.edu
4. Type in user name: (your duke user name)
5. Press enter
6. Enter password in pop up box.
7. Press enter
8. Drag files to transfer from the left local computer (the desktop) to the right remote
computer (your acpub account).
9. When finished, disconnect and close this window

Note: You can download the “SSH secure file transfer client” from OIT to your own
computer and transfer the files from your acpub account back to your computer.

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Quantitative Metallography
Quantitative microstructural analysis is important in materials characterization, but the
same principles are used commonly in many fields, including medicine, biology,
geology, mineralogy, etc. Advances in computers have had a major impact on the field
of quantitative metallography. Because microstructures are 3-D, the parameters used to
describe them should describe 3-D geometry. Quantitative metallography provides
methods of studying 3-D metal from 2-D sections taken through a solid body. Some
assumptions are usually necessary, although one can use serial sections to obtain 3-D
information at a greatly increased effort. Experimentally, three general methods are used
to get information from a 2-D section like a polished surface or micrograph. These
methods help the researcher find grain size, percent carbon content and percent phases
present. They are:
a. Point counting: Overlay a grid on top of the micrograph and record the number of
grid nodes (points) lying in the object of interest.
b. Linear analysis: Use either a line or circle of a known length or circumference
and overlay it on the micrograph. Record the number of times the line or circle
intersects with phase boundaries or grain boundaries. In general, the circle
method is more accurate than the line method due to “end effects” of the line.
c. Area analysis: Measure and count the areas of microstructural constituents. This
is usually impractical without the use of a computer. Before computers, the
researcher would actually cut out the phases from a micrograph and weigh them.
The weight fraction of a particular phase was then the used as the quantitative
area fraction.

Point counting and linear analysis are the preferred methods for manual microscopy
analysis and will be the ones used in this lab. Quantitative microscopy can either be
accomplished on a computer with an image program or by hand. Both will be explained
in the following sections. The focus of the lab is to learn quantitative microscopy by
hand. This handout integrates information about more sophisticated quantitative
metallography that the computer can do for those who later study metallography in more
depth.

Computer Image Analysis Program

NIH Image is a public domain image processing and analysis program for the Macintosh.
It was developed at the Research Services Branch (RSB) of the National Institute of
Mental Health (NIMH), part of the National Institutes of Health (NIH). It can be
downloaded for Apple computers at http://rsb.info.nih.gov/nih-image/. A free PC version
of NIH-Image, called Scion Image for Windows, is available from Scion Corporation
(www.scioncorp.com). There is also Image/J, a Java program inspired by Image that
"runs anywhere" (http://rsb.info.nih.gov/ij/). All of these are free and can be found on the
noted web pages. You can transfer the images to your computer and download one of
these programs so you can analyze the images from your own computer. The following
is an introduction from the NIH-Image website (about page) and manual:

NIH-Image can acquire, display, edit, enhance, analyze and animate images. It
reads and writes many different file types, providing compatibility with many

14
 other applications, including programs for scanning, processing, editing,
publishing and analyzing images. It supports many standard image processing
functions, including contrast enhancement, density profiling, smoothing,
sharpening, edge detection, median filtering, and spatial convolution with user
defined kernels. Image can be used to measure area, mean, centroid, perimeter,
etc. of user defined regions of interest. It also performs automated particle
analysis and provides tools for measuring path lengths and angles. Spatial
calibration is supported to provide real world area and length measurements.
Density calibration can be done against radiation or optical density standards
using user specified units. Results can be printed, exported to text files, or copied
to the Clipboard. A tool palette supports editing of color and gray scale images,
including the ability to draw lines, rectangles and text. It can flip, rotate, invert
and scale selections. It supports multiple windows and 8 levels of magnification.
All editing, filtering, and measurement functions operate at any level of
magnification and are undoable. Image directly supports Data Translation and
Scion frame grabber cards for capturing images or movie sequences using a TV
camera. Acquired images can be shading corrected and frame averaged. Other
frame grabbers are supported via plug-in modules. Image can be customized in
three ways: via a built-in Pascal-like macro language, via externally compiled
plug-in modules and on the Pascal source code level. Example macros, plug-ins
and complete source code can be downloaded from the Download page.

Calibration of Size Scale of Image

You must use a scale bar on any image you include in a paper. Only stating the objective
used or magnification is not enough. The size scale is altered if the size of the image is
changed. For example, when you print the image, its size may be slightly distorted. The
table below illustrates the actual size of the specimen in a captured image taken with one
of the four objectives in place. The calibration is the number of pixels per distance of the
image (actual size) and is used to calibrate a software program like Scion Image. The
native pixel resolution of the captured image is 320 x 240, so it is rectangular at a 4:3
ratio. The resolution can be changed, so double check the resolution of your image and
adjust the calibration accordingly. The pixel aspect ratio should be 1.0, since you are not
distorting the image.

Objective Image Size (width x height) Calibration

5x 960 µm x 720 µm 167 pixels = 500 µm
10x 480 µm x 360 µm 200 pixels = 100 µm
20x 240 µm x 180 µm 133 pixels = 100 µm
50x 96 µm x 72 µm 167 pixels = 50 µm

Image program calibration

1. Open saved micrograph of a steel sample. NOTE: All three programs should
have very similar pull-down menus.
2. Go to the analyze pull down menu and click on set scale. Set the values
according to the calibration table above.

15
Grain Size
Knowing the 3-dimensional grain microstructure is very important when determining
grain size. For example, the grains may be very long in a longitudinal section of a cold-
rolled steel; a cross-section, however, would show very small grains. The take-home
point is that a 2-D section cannot always describe a 3-D structure. A thorough analysis
would include multiple longitudinal as well as cross sectional micrographs. Any method
chosen should be repeated at least 5 times to generate an average and standard deviation.

Via Hand: Line and circle method

Grain size is best determined by linear analysis and defined as the number of grains
intersected by a traverse of a known length (be it a straight line or a circle). This can
easily be done by hand. Print the micrograph and overlay with a clear overhead projector
transparency. Draw a line or circle of known length or circumference. Randomly
overlay the line or circle on the micrograph and count the number of times the line or
circle intersects a grain boundary. Be sure to draw as thin of a line as possible in order to
more accurately distinguish intersections.

Via Computer: Line and circle method

This can also be done with image software program. Start the program and open the
micrograph (File-Open). Make sure to calibrate the image as above.
Line method: Use the line icon to draw a line randomly on your image, long enough to
cover many grains. Click analyze, then measure and the distance of the line will be
shown in the pop up results box. Count the number of grain boundary intersections (you
could have the program do this for you as well, but it involves more advanced knowledge
of the program and image processing).
Circle method: Use the circle icon to draw a circle randomly on your image much larger
than a grain. Click analyze, then measure and the area of the circle will be shown in the
pop up results box. From this area, calculate the circumference. Count the number of
grain boundary intersections and use the equation above to calculate grain size.

Area (Volume) Fraction

Volume fractions are best determined by point counting due to its higher precision. Of
course it is necessary that the specimen surface be representative of the sample and also
free of artifacts. Draw a regularly spaced grid to overlay the microstructure image.
Ideally, the spacing of the grid of points should be at least of the order of the diameter of
the largest area so that no more than one node falls on any given area. Count how many
nodes fall on dark (carbon rich pearlite) areas, and divide by the total number of nodes.
Use this fraction to calculate carbon content fraction (see equation below). Be careful not
to count grain boundaries as pearlite regions. The 0.77 factor in the equation is the
fraction of carbon in pearlite and the 0.02 factor is the carbon fraction in ferrite. Adjust
these two factors as it pertains to your particular sample. Move the grid at least 5 times
to generate an average and standard deviation.

16
Hardness Testing

Here you will be using the Rockwell hardness testing machine, fitted with an appropriate
indenter. The Rockwell hardness test measures the indentation depth of a standardized
indenter into the specimen under a predetermined load. To achieve some uniformity in
the measurement, the indenter is preloaded under a specified load after engaging on the
sample surface. This will establish a “datum” from which the indentation depth is
measured. Although you are measuring penetration depth, the results will be shown as
Rockwell Hardness values. Rockwell scale from hardest to softest: C>A>B>E>H.

The Rockwell hardness test method consists of indenting the test material with a diamond
cone or hardened steel ball indenter. The indenter is forced into the test material under a
preliminary minor load F0 (see Figure A below) usually 10 kgf. When equilibrium has
been reached, an indicating device that follows the movements of the indenter and so
responds to changes in depth of penetration of the indenter is set to a datum position.
While the preliminary minor load is still applied an additional major load is applied with
a resulting increase in penetration (Figure B). When equilibrium has again been reached,
the additional major load is removed but the preliminary minor load is still maintained.
Removal of the additional major load allows a partial recovery, thereby reducing the
depth of penetration (Figure C). The permanent increase in depth of penetration,
resulting from the application and removal of the additional major load is used to
calculate the Rockwell hardness number.

HR = E - e

F0 = preliminary minor load in kgf

F1 = additional major load in kgf
F = total load in kgf
e = permanent increase in depth of penetration due to major load F1 measured in units of
0.002 mm
E = a constant depending on form of indenter: 100 units for diamond indenter, 130 units
for steel ball indenter
HR = Rockwell hardness number
D = diameter of steel ball

Rockwell Principle

17
Rockwell Hardness Scales
Minor Load Major Load Total Load
Value of
Scale Indenter F0 F1 F
E
kgf kgf kgf
A Diamond cone 10 50 60 100
B 1/16" steel ball 10 90 100 130
C Diamond cone 10 140 150 100
D Diamond cone 10 90 100 100
E 1/8" steel ball 10 90 100 130
F 1/16" steel ball 10 50 60 130
G 1/16" steel ball 10 140 150 130
H 1/8" steel ball 10 50 60 130
K 1/8" steel ball 10 140 150 130
L 1/4" steel ball 10 50 60 130
M 1/4" steel ball 10 90 100 130
P 1/4" steel ball 10 140 150 130
R 1/2" steel ball 10 50 60 130
S 1/2" steel ball 10 90 100 130
V 1/2" steel ball 10 140 150 130

Typical Application of Rockwell Hardness Scales

HRA . . . . Cemented carbides, thin steel and shallow case hardened steel
HRB . . . . Copper alloys, soft steels, aluminium alloys, malleable irons, etc
HRC . . . . Steel, hard cast irons, case hardened steel, materials harder than 100 HRB
HRD . . . . Thin steel and medium case hardened steel and pearlitic malleable iron
HRE . . . . Cast iron, aluminium and magnesium alloys, bearing metals
HRF . . . . Annealed copper alloys, thin soft sheet metals
HRG . . . . Phosphor bronze, beryllium copper, malleable irons. Aluminium, zinc, lead
HRK, HRL, HRM, HRP, HRR, HRS, HRV
….Soft bearing metals, plastics and other very soft materials

Advantages of the Rockwell hardness method include the direct Rockwell hardness
number readout and rapid testing time. Disadvantages include many arbitrary non-related
scales and possible effects from the specimen support anvil (try putting paper under a test
block and take note of the effect on the hardness reading! Vickers and Brinell methods
don't suffer from this effect).

18
 Hardness Conversion Table
Approximate Hardness Equivalents Covering Range of Rockwell C and Rockwell B Scales
SCLERO-
VPN ROCKWELL SCALES BRINELL SCOPE U.T.S.
DPH BHN BHN
HV/10 A B C D E F G H K 15N 30N 45N 15T 30T 45T 500kg 3000kg Kpsi Mpa
1865 92 80 87 97 92 87
1787 92 79 86 96 92 87
1710 91 78 85 96 91 86
1633 91 77 84 96 91 85
1556 90 76 83 96 90 84
1478 90 75 83 95 89 83
1400 89 74 82 95 89 82
1323 89 73 81 95 88 81
1245 88 72 80 95 87 80
1160 87 71 80 94 87 79
1076 87 70 79 94 86 78 101
1004 86 69 78 94 85 77 99
940 86 68 77 93 84 75 97
900 85 67 76 93 84 74 95
865 85 66 75 93 83 73 92
832 84 65 75 92 82 72 739 91
800 84 64 74 92 81 71 722 88
772 83 63 73 91 80 70 705 87
746 83 62 72 91 79 69 688 85
720 82 61 72 91 79 68 670 83
697 81 60 71 90 78 67 654 81 320 2206
674 81 59 70 90 77 66 634 80 310 2137
653 80 58 69 89 76 64 615 78 300 2069
633 80 57 69 89 75 63 595 76 290 2000
613 79 56 68 88 74 62 577 75 282 1944
595 79 120 55 67 88 73 61 560 74 274 1889
577 78 120 54 66 87 72 60 543 72 266 1834
560 78 119 53 65 87 71 59 523 71 257 1772
544 77 119 52 65 86 70 57 512 69 245 1689
528 77 118 51 64 86 69 56 496 68 239 1648
513 76 117 50 63 86 69 55 481 67 233 1607
498 75 117 49 62 85 68 54 469 66 227 1565
484 75 116 48 61 85 67 53 455 64 221 1524
471 74 116 47 61 84 66 51 443 63 217 1496
458 74 115 46 60 84 65 50 432 62 212 1462
446 73 115 45 59 83 64 49 421 60 206 1420
434 73 114 44 59 83 63 48 409 58 200 1379
423 72 113 43 58 82 62 47 400 57 196 1351
412 72 113 42 57 82 61 46 390 56 191 1317
402 71 112 41 56 81 60 44 381 55 187 1289
392 71 112 40 55 80 60 43 371 54 182 1255
382 70 111 39 55 80 59 42 362 52 177 1220
372 70 110 38 54 79 58 41 353 51 173 1193
363 69 110 37 53 79 57 40 344 50 169 1165
354 69 109 36 52 78 56 38 336 49 165 1138
345 68 109 35 52 78 55 37 327 48 160 1103
336 68 108 34 51 77 54 36 319 47 156 1076
327 67 108 33 50 77 53 35 311 46 152 1048
318 67 107 32 49 76 52 34 301 44 147 1014
310 66 106 31 48 91 76 51 33 294 43 144 993
302 66 105 30 48 91 75 50 31 286 42 140 965
294 65 104 29 47 89 75 50 30 279 41 137 945
286 65 104 28 46 88 74 49 29 271 41 133 917
279 64 103 27 45 87 73 48 28 264 40 129 889
272 64 103 26 45 86 73 47 27 258 39 126 869
266 63 102 25 44 85 72 46 26 253 38 124 855
260 63 101 24 43 84 72 45 24 247 37 121 834
254 62 100 23 42 83 71 44 23 93 82 72 201 240 36 118 814
248 62 99 22 42 81 71 43 22 93 82 71 195 234 35 115 793
243 61 98 21 41 79 70 42 21 93 81 70 189 228 35 112 772
238 61 97 20 40 78 69 42 20 92 81 69 184 222 34 109 752
234 60 97 19 77 92 80 69 181 218 34 107 738
230 59 96 18 76 92 80 68 179 214 33 106 731
226 59 96 17 75 92 80 68 177 210 33 104 717
222 58 95 16 74 92 79 67 175 208 32 102 703
DPH BHN BHN
HV/10 A B C D E F G H K 15N 30N 45N 15T 30T 45T 500kg 3000kg Kpsi Mpa
SCLERO-
VPN ROCKWELL SCALES BRINELL SCOPE U.T.S.

19
 Hardness Conversion Table
Approximate Hardness Equivalents Covering Range of Rockwell C and Rockwell B Scales (Cont.)
SCLERO-
VPN ROCKWELL SCALES BRINELL SCOPE U.T.S.
DPH BHN BHN
HV/10 A B C D E F G H K 15N 30N 45N 15T 30T 45T 500kg 3000kg Kpsi Mpa
217 58 95 15 73 92 79 67 171 205 31 100 690
213 58 94 14 73 91 79 66 169 203 31 99 683
208 57 93 13 71 91 78 66 167 200 30 98 676
204 57 92 12 70 100 91 78 65 163 195 30 96 662
200 56 92 11 69 100 91 77 64 162 193 29 95 655
196 56 91 10 68 100 90 77 64 160 190 28 93 641
192 56 90 9 66 99 90 76 63 157 185 27 91 627
188 55 89 8 64 98 90 76 62 154 180 26 88 607
184 54 88 7 63 97 90 75 61 151 176 26 86 593
180 54 87 6 61 97 89 75 60 148 172 26 84 579
176 53 86 5 59 96 89 74 59 145 169 25 83 572
172 53 85 4 58 95 89 74 58 142 165 25 81 558
168 52 84 3 56 94 88 73 57 140 162 25 79 545
164 51 83 2 54 93 88 72 56 137 159 24 78 538
160 51 82 1 53 92 88 72 55 135 156 24 76 524
156 50 81 0 51 91 87 71 54 133 153 24 75 517
152 50 80 49 91 87 70 53 130 150 73 503
148 49 79 48 90 87 70 52 128 147
144 49 78 46 89 86 69 51 126 144
141 48 77 44 88 86 68 50 124 141
139 47 76 43 87 86 68 49 122 139
137 47 75 100 41 86 85 67 49 120 137
135 46 74 99 39 85 85 66 48 118 135
132 46 73 99 38 85 85 66 47 116 132
130 45 72 98 36 84 84 65 46 114 130
127 45 71 100 98 35 83 84 64 45 112 127
125 44 70 100 97 33 82 84 64 44 110 125
123 44 69 99 96 31 81 83 63 43 109 123
120 43 68 98 96 30 80 83 62 42 107 121
118 43 67 98 95 28 79 83 62 41 106 119
116 42 66 97 95 27 78 82 61 40 104 117
115 42 65 96 94 25 78 82 60 39 102 116
114 42 64 96 94 24 77 82 60 38 101 114
113 41 63 95 93 22 76 81 59 37 99 112
112 41 62 95 92 21 75 81 58 36 98 110
111 40 61 94 92 19 74 81 57 35 96 108
110 40 60 93 91 18 73 81 57 34 95 107
108 39 59 93 91 16 72 80 56 32 94 106
107 39 58 92 90 15 71 80 55 31 92 104
106 38 57 91 90 13 71 80 55 30 91 102
105 38 56 91 89 12 70 79 54 29 90 101
104 38 55 90 88 10 69 79 53 28 89 99
103 37 54 90 88 9 68 79 53 27 87
102 37 53 89 87 7 67 78 52 26 86
101 36 52 88 87 6 66 78 51 25 85
100 36 51 88 86 4 65 78 51 24 84
100 35 50 87 86 3 65 77 50 23 83
99 35 49 87 85 64 77 49 22 82
98 35 48 86 85 63 77 49 21 81
97 34 47 85 84 62 76 48 20 80
96 34 46 85 83 61 76 47 19 79
95 33 45 84 83 60 76 46 18 79
95 33 44 84 82 59 75 46 17 78
94 32 43 83 82 58 75 45 16 77
93 32 42 82 81 58 75 44 15 76
92 31 41 82 81 57 74 44 14 75
91 31 40 81 80 56 74 43 13 74
90 31 39 80 79 55 74 42 11 74
90 30 38 80 79 54 73 42 10 73
89 30 37 79 78 53 73 41 9 72
88 29 36 79 78 100 52 73 40 8 71
88 29 35 78 77 100 52 72 40 7 71
87 28 34 77 77 99 51 72 39 6 70
87 28 33 77 76 99 50 72 38 5 69
86 28 32 76 75 99 49 71 38 4 68
86 27 31 76 75 98 48 71 37 3 68
85 27 30 75 74 98 47 71 36 2 67
85 26 29 74 74 98 46 70 36 1 66
84 26 28 74 73 97 45 70 35 66 BHN
DPH BHN
HV/10 A B C D E F G H K 15N 30N 45N 15T 30T 45T 500kg 3000kg Kpsi Mpa
SCLERO-
VPN ROCKWELL SCALES BRINELL SCOPE U.T.S.

20
 Hardness Conversion Table
Approximate Hardness Equivalents Covering Range of Rockwell C and Rockwell B Scales (Cont.)
SCLERO-
VPN ROCKWELL SCALES BRINELL SCOPE U.T.S.
DPH BHN BHN
HV/10 A B C D E F G H K 15N 30N 45N 15T 30T 45T 500kg 3000kg Kpsi Mpa
85 27 30 75 74 98 47 71 36 2 67
85 26 29 74 74 98 46 70 36 1 66
84 26 28 74 73 97 45 70 35 66
84 25 27 73 73 97 45 70 34 65
83 25 26 73 72 97 44 69 33 65
83 24 25 72 71 96 42 69 33 64
82 24 24 71 71 96 42 69 32 64
82 24 23 71 70 96 41 68 31 63
81 23 22 70 70 95 40 68 31 63
81 23 21 70 69 95 39 68 30 62
80 22 20 69 69 95 38 68 29 62
80 22 19 68 68 94 38 67 29 61
79 21 18 68 67 94 37 67 28 61
79 21 17 67 67 93 36 67 27 60
78 21 16 67 66 93 35 66 26 60
78 20 15 66 66 93 34 66 26 59
77 14 65 65 92 33 66 25 59
77 13 65 65 92 32 65 24 58
76 12 64 64 92 32 65 24 58
76 11 64 64 91 31 65 23 57
75 10 63 63 91 30 64 22 57
75 9 62 62 91 29 64 22 56
74 8 62 62 90 28 64 21 56
74 7 61 61 90 27 63 20 56
73 6 61 61 90 26 63 20 55
73 5 60 60 89 26 63 19 55
72 4 59 60 89 25 62 18 55
72 3 59 59 88 24 62 17 54
71 2 58 58 88 23 62 17 54
71 1 58 58 88 22 61 16 53
70 0 57 57 87 21 61 15 53
DPH BHN BHN
HV/10 A B C D E F G H K 15N 30N 45N 15T 30T 45T 500kg 3000kg Kpsi Mpa
SCLERO-
VPN ROCKWELL SCALES BRINELL SCOPE U.T.S.

Hardness References

1. Small, L., Hardness, theory and practice. 1960, Ferndale, Mich.,: Service
Diamond Tool Co. v.
2. Tabor, D., The hardness of metals. Monographs on the physics and chemistry of
materials. 1951, Oxford,: Clarendon Press. ix, 175.
3. Boyer, H.E. and American Society for Metals., Hardness testing. 1987, Metals
Park, Ohio: ASM International. 188.
4. Chandler, H. and ASM International., Hardness testing. 2nd ed. 1999, Materials
Park, OH: ASM International. vii, 192.
5. Lysaght, V.E. and A. De Bellis, Hardness testing handbook. 1969, [Wilkes Barre?
Pa.,: American Chain and Cable Co. 141.
6. O'Neill, H., Hardness measurement of metals and alloys. 2nd ed. 1967, London,:
Chapman & Hall. iii-xvi, 238.
7. Westbrook, J.H., H. Conrad, and American Society for Metals., The Science of
hardness testing and its research applications. 1973, Metals Park, Ohio,:
American Society for Metals. xiv, 520.

21
Hardness Testing Step-by-Step Procedure
Note that the larger of the two Rockwell Hardness Testers (Model 4 TT BB) has a
variable minor load weight on the top of the loading arm. WHEN USING THIS
MACHINE AS A NORMAL ROCKWELL HARDNESS TESTER, THIS MINOR
LOAD WEIGHT MUST BE DOWN, RESTING ON THE LOADING ARM!

1. Read the scale on front of the machine. For this lab experiment, take the reading
from the C scale.
2. Make sure the load lever (located directly on the right-hand side of the scale) is
oriented in a forward direction.
3. Place puck on stage and rotate stage upward using the spindle located at the bottom
of the tester.
4. Once contact is made, continue rotating upward until the small needle points to the
black dot on the scale and the large needle points upward. NEVER retract the stage
to compensate an overshoot. Be careful when moving the stage up.
5. Turn the dial to the set position; i.e., to match the large needle.
6. Push trip lever slightly to release.
7. When the lever stops moving, return it to the forward position.
8. Read hardness on the dial of the tester and record it in your lab notebook. Be certain
to also record the location of this hardness on a sketch of the specimen in your
notebook!
9. In this lab, it is up to you to decide how many measurements to take. Use the
knowledge you gained from the statistical lab. You must choose the appropriate
number and location of hardness tests to perform. State the location and number in
your report.
10. Take an image of the hardness indentation for use in your report. Make sure to
include length scale.

Notes: Indentations should be sufficiently spaced apart to obtain independent hardness

values. A rule of thumb is to choose at least 3 (better 5) indentation diameters between
locations and from any edge.

If the object of measuring hardness is to correlate it with tensile strength, make certain
that the hardness scale chosen is one for which such a correlation exists. If your hardness
reading is too low or too high for an exact correlation with tensile strength, make a plot of
T. S. vs. hardness from the chart, and extrapolate.

Calibration blocks are available to check machine accuracy. If you use one, make
certain that the surface resting on the platen contains no indentations and is flat and
smooth.

22
References:

Most of these references are on the reference/ reserve shelf.

1. L. Van Vlack, Elements of Materials Science. Chapter 9-11.

2. W. Moffatt, G. Pearsall and J. Wulff, The Structure and Properties of Materials

Vol. I.

3. H. Hayden, W. Moffatt and J. Wulff, The Structure and Properties of Materials,

Vol. III.

4. C. Parker, The Metallurgy of Quality Steels.

5. C. Samans, Engineering Metals and Their Alloys.

6. E. Reed, Photomicrographs of Iron and Steel.

7. W. Rostoker and J. Dvorak, Interpretation of Metallographic Structures.

8. R. Brick, R. Gordon and A. Phillips, Structure and Properties of Alloys.

9. N. Woldman, Engineering Alloys.

10. U. S. Steel, The Making, Shaping and Testing of Steel.

11. DeFerri Metallographia.

12. ASM Metals Handbook. (Several Volumes).

13. Modern Steels and Their Properties, 6th ed. Bethlehem Steel Corp., Bethlehem,
PA (1967).

14. There are a number of materials handbooks on the reference shelf.

In addition, there are many books on steels, other alloys and on design in the
Engineering Library. For articles in periodicals, check Engineering Index, Applied
Science and Technology Index, and Metals Abstracts.

23
Technical Report

Please follow the general suggestions in the “Writing Technical Reports” outline given to
you earlier in this semester when preparing your report. The following is a brief outline
of what is expected in each section of the report. Even if you are unable to determine the
processing condition of each sample, show some logical reasoning behind some choice.
The report should include statistical evaluation as introduced previously.

Important:
 Although you are working in teams, it is expected that every student will turn in
his/her own lab report. You may consult each other on technical issues, but the
writing is to be that of each student.
 Do not just answer the questions in the order they are presented here, write a
continuous and coherent report while making sure you address all of the questions
and comments below.

1. Title Page
 A title for the lab report, the class for which the report was prepared, a date, your
team name and your name.

2. Introduction
 Explain the objective of the lab as well as a brief outline of the remainder of the
report.

3. Background
 Find and state the chemical composition of the sample in the literature. What is
the basic purpose of each component? Explain the designation number.
 What are the general characteristics typical of this type of material (good or bad)?
For example does it have relatively good or bad: yield strength, tensile strength,
compressive strength, impact strength, fatigue strength, shear strength, elastic
modulus, corrosion resistance, wear resistance, machinability, formability,
electrical conductivity, thermal conductivity, etc?
 Find an example of an engineering application of your sample and explain why
one would select this type of material for this particular design application.

4. Experimental Procedure (Materials and Methods)

 This section is straightforward. Describe the steps required to prepare the sample
specimens, image the microstructure and perform the hardness test. You also may
want to include safety concerns.
 DO NOT copy the laboratory procedure verbatim. Describe in your own words
how the specimens were prepared and tested. Also, include any problems you
may have run into while preparing or testing the specimens.
 This section should be written in such a way that a student with some background
knowledge could walk into the lab and follow your instructions.

24
  You do not have to explain every step as described in the procedures. Decide
what is important to be in a report. It is not important, for example, to go through
all of the steps about using a microscope.

5. Results
 Present all data obtained in the form of a figure or table. Ensure that everything is
properly labeled with units and scale bars. Briefly, state the results in the text as
well.
 State the name of person corresponding with the sample they prepared (a use of a
table with person, sample number given, processing type and hardness would be
good).
 Determine average grain size with standard deviation and explain how you
calculated it.
 Determine carbon content of your team’s steel (average and standard deviation)
and explain how you calculated it.
 Images (of all three if necessary) before etching.
 Images of all three samples after etching, showing representative phases and
explain what phases are present in each micrograph.
 Hardness: indicate location and number of measurements on the sample, state
average and standard deviation of all three, and corresponding tensile strength.
Include an image of the hardness indentation.

6. Discussion
 Through the data your team obtained, determine what conditions each of your
three samples has been subjected to, (as-received, annealed or quenched).
Thoroughly explain your reasoning.
 Present a hypothetical TTT Diagram, indicate the cooling rate of all 3 samples.
 Explain how you expect the microstructure of the as-received, annealed and
quenched samples to be different from each other.
 Describe and compare microstructure of all three samples from your team
(phases, grain size, etc), explain why (or why not) they are different. Compare to
what you expected.
 Hardness: compare and explain why (or why not) they are different from each
other and if the result is what you expected. Does the relative order of hardness
make sense (ie from hardest to softest)?
 Compare mechanical properties (hardness and UTS) you experimentally found to
literature values, are they equal? Why or why not?
 Explain the mechanical properties (hardness and tensile tests) from the observed
microstructure. Would you consider each one ductile, brittle, and/or tough?

7. Conclusions
 Summarize the report and give the conclusions you drew from the lab. When
writing this section, keep in mind that this is the likely section that your boss or
colleague will read first; thus it needs to concisely convey the scope of the

25
 experiments and a clear summary of the results, and your conclusions. You can
think of the conclusion section as sort of an extended abstract of the report.

8. References
 Please reference all sources used for preparing the report. The references should be
labeled (e.g., [2]) in the text and should appear in chronological order at the end
of the report in the reference section in a complete and consistent way. See
“Writing technical reports” for examples. Internet sources need to be cited as
well, together with the URL and the date of access.

ME83L – Structure/Properties of Solids

Fall 2004

Lab #5 - Metallography Lab Report Grading Sheet

Overall structure 10
Overall grammar 5
Overall figures and tables 5
Intro 5
Methods 5
Results 10
Discussion 50
Conclusion 5
References 5
Total 100

26
Team Oral Technical Report

The primary purpose of an oral technical report is to communicate technical information

quickly and concisely and to leave a lasting impression of the most important points.
Pretend like you are a team of engineers and this is the presentation you have to describe
what your results were. The presentation time should last no longer than 10 minutes with
a couple of minutes after for questions and discussion. You cannot explain everything
you did, but you must decide what is important for someone that doesn’t know what you
did and explain it to them. You are also encouraged to be creative with the presentation.
You must meet as a team and prepare one presentation. Make sure to be concise, clear,
and do not go over on time.

a. Rehearse the report to gain familiarity with its organization and details, and to
check on the time it will take. Consider this situation: you were asked by your
boss to perform an experiment whose outcome is important to make a business
decision. You have done the tests and were now called to the board room to
present your results and conclusions in front of the board of directors (some of
which are not engineers). You were given 4 minutes to present your results and
conclusions.
b. You can use overheads or computer projection. Good rule of thumb for the
number of slides or transparencies you use is: 1 slide per minute. This means you
need to convey all your information in about 10 slides. Keep in mind that you
likely want to convey graphical information; do not expect someone to read a lot
of print. Use color and graphics to convey your message.
c. Use each oral report as an opportunity to experiment with the ways in which you
can use voice inflections and other techniques to emphasize the key points in the
oral presentation.

The following is a suggestion on what to include in the presentation. The number of

slides is just a suggestion for this lab. Feel free to be creative and present your teams
work in the most clear and understandable way for the audience.

a. Title slide (1 slide)

b. A brief introduction (1-2 slides)
c. Background of your steel. (1-2 slides)
d. Materials and Methods (1-2 slides)
e. Present results obtained (each member must present what they did).
 Show microstructure images and corresponding hardness values and
processing conditions. Compare them. (3-5 slides)
f. Discuss conclusions. (1 slide)

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 ME83L – Structure/Properties of Solids

Fall 2004

Lab #5 - Metallography Lab Team Presentation Grading Sheet

You will be evaluated by the following:

Content
Title slide 1
Intro/Background 2
Materials and methods 1
Results 2
Discussion 3
Conclusion 1
Overall Presentation
Visual 3
Communication 7
Total 20

Comments:

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