Tafila Technical University

Faculty of Engineering
Department of Mechanical Engineering

Metallurgical Processes LAB

“Exp.3: Specimen Preparation ”

Student Name: Ahmad Nader Ibrahim Ghawanmeh.

Student ID: 320180101053.

Instructor name: Dr. Rashid Abdul Latif Lotfi Abdullah.

1. Introduction
Sample Cutting and Sectioning

a- Sectioning

Sectioning means removal of convenient size specimen from large sample with minimal damage to
microstructure with the help of abrasive cut off machine. Abrasive cutting wheel/saw is attached to
cutting machine and for work piece holding proper vice is provided on machine. The primary concern in
this process is to minimize the heating of the sample due to the cutting. For this reason, the cut-off saws
that is equipped with either water-cooling systems.

b- Mounting

If sample is large enough (about 25 mm square or larger) than do not need to mount it, as it will be able
to control the sample during polishing without a mount. For smaller samples there are two basic
mounting techniques used in this laboratory. Mounting facilitates handling during preparation and
handling. It also avoids damage to polishing wheels during polishing. The most common uses a
thermosetting plastic compound (Bakelite) to encapsulate the specimen known as hot-mounting
process, and the second uses a room temperature curing epoxy known as cold mounting process. The
Bakelite mounting is by far the most common and easiest. The room temperature curing epoxy mount
should only be used for samples that are extremely sensitive to heat.

c- Sample Surface Polishing

The goal of the surface polishing is to end up with a planar cross section of sample free from scratches
or disturbed metal introduced by the cutting and sectioning. This process is a step-wise process that can
be broken into three loosely separate parts: grinding, coarse polishing, and final polishing.

d- Grinding

The first step in preparing your sample is to ensure that you have a flat surface to begin with. A water-
cooled abrasive grinder is available to form a flat initial surface from which to begin. After getting a flat
sample on the belt grinder, WASH sample thoroughly. The hand lapping station has four graded abrasive
papers to produce a sequentially finer surface finish. Be sure the water is turned on and flowing
uniformly over the abrasives. Start with the coarsest grit (240) and, using a firm and uniform pressure,
slowly move the specimen forward and back across the abrasive. This will produce parallel scratches of
uniform size. Continue this step until the entire surface of your sample is flat and contains only scratches
of the size of 240 grit abrasive. When the sample is flat and the only scratches remaining are those due
to the 240-grit abrasive, WASH your sample and your hands thoroughly, and move to the 320-grit
abrasive. Repeat this procedure for the 400 grit and the 600-grit abrasive, checking after each step to be
sure that only those scratches remain that are due to the smallest grit.
 e- Etching

Grains cannot be seen without etching. Cracks, pores and defects are observed without etching.
Etchant reacts with atoms and dissolves them. Atoms at grain boundaries dissolve quickly. Dissolved
grain boundaries appear dark.

2. Objectives
1. To learn and to gain experience in the preparation of metallographic specimens.

2. To examine and analyze the microstructures of metals and metallic alloys.

3. Abstract
Proper preparation of metallographic specimens to determine microstructure and content requires that
a rigid step-by-step process be followed. In sequence, the steps include sectioning, mounting, course
grinding, fine grinding, polishing, etching and microscopic examination. Specimens must be kept clean
and preparation procedure carefully followed in order to reveal accurate microstructures. Each student
will prepare and examine a brass, steel or aluminum sample for metallographic examination.
Additionally, a brass, steel or aluminum sample with different composition, a eutectoid steel sample and
a eutectoid Pb-Sn sample will be examined under the metallographic microscope. Photographs will be
taken of the samples and the ASTM grain size number determined for each of the specimens if
applicable.

4. Background
Metallography consists of the study of the constitution and structure of metals and alloys. Much can be
learned through specimen examination with the naked eye, but more refined techniques require
magnification and preparation of the material's surface. Optical microscopy is sufficient for general
purpose examination; advanced examination and research laboratories often contain electron
microscopes (SEM and TEM), x-ray and electron diffractometers and possibly other scanning devices.

Incorrect techniques in preparing a sample may result in altering the true microstructure and will most
likely lead to erroneous conclusions. It necessarily follows that the microstructure should not be altered.
Hot or cold working can occur during the specimen preparation process if the metallurgist is not careful.
Expertise at the methods employed to produce high-quality metallographic samples requires training
and practice.

The basic techniques can be learned through patient persistence in a matter of hours. This module takes
the student through the metallographic sample preparation process step-by-step with demonstrations
and explanations of sectioning, mounting, course & fine grinding, polishing, etching and microscopic
examination.
5. Sectioning
Operations such as shearing produce severe cold work, which can alter the microstructure of a sample.
Abrasive cutting (sectioning) offers the best solution to eliminate these undesirable features; the
resultant surface is smooth, and the sectioning task is quickly accomplished. Low-speed cut-off wheels
are utilized in cases where the heat created by standard abrasive cutters must be avoided. Ample
coolant and proper speed control is essential in all sectioning operations.

Abrasive Cut-Off Wheels consist of abrasive grains (such as Aluminum Oxide or Silicon Carbide), bonded
together with rubber or other materials in the form of a thin wheel. Rubber bonded wheels are most
extensively used for wet operation and resin bonds for dry cutting. When sectioning a piece of metal,
the abrasive grains on the cutoff wheel become dull, therefore, the bond must be destroyed at the
correct rate so that new grains are always at the edge and are still held firmly by the bonding material.
The rate at which the bond breaks down is affected by several different factors, including:

1) The hardness of the bond.

2) The hardness and workability of the metal sample.

3) The size and speed of the wheel.

4) The power of the driving motor.

5) The type and amount of coolant and its method of application.

6) The amount of pressure by which the wheel is applied to the sample.

7) The amount of vibration in the machine.

Cutoff wheels are indexed from hard to soft and are referred to by "grade". As a rule of thumb, a hard
bonded wheel should be selected when sectioning soft stock, and a soft wheel for sectioning harder
material.

A reasonable amount of wheel pressure must be applied so the abrasive grains will "bite" and remove
the metal in fine chips. An experienced operator can tell whether the wheel is cutting or merely "dragging"
by the feel of the control arm and monitoring of the power consumption of the cutting equipment.

Lab Procedure - Sectioning

1. Place the sample on the slotted Table so that it is at the centre of the swing of the head.

2. Place the Locking Lever in the forward position to allow the Control Rod to be moved to the furthest
position. Move the Rear Vise section to contact the rear face of the sample. Move the Front Section to a
position near the front face of the sample.

3. Tighten the Nuts that secure the Vise sections to the Table.
4. Push the Control Rod in to make firm contact with the sample and pull back the Locking Level to
secure the sample.

5. Turn on the coolant; it should flow readily to both cool and clean the cutting area.

6. Apply steady moderate pressure until the specimen is sectioned; avoid jerking motions that may
cause the blade to splinter.

6. Mounting
Small samples are generally mounted in plastic for convenience in handling and to protect the edges of
the specimen being prepared. Compression-type molding is commonly applied to encase specimens in
1-to-1.5-inch diameter plugs of a hard polymer. Compression molding materials are classified as either
thermosetting or thermoplastic:

1) Bakelite is a low cost, relatively hard thermosetting polymer that is commonly utilized.

2) Expensive Trans optic Thermoplastics are utilized when transparency is required.

Trans optic materials remain molten at maximum temperature and become transparent with an
increase in pressure and a decrease in temperature. By definition, thermosetting materials require heat
and pressure during the molding cycle. During mounting, the pressure and molding temperature are
generally held constant thus, time is the only variable. The metal sample is placed in the mounting
cylinder which is then encased in a pre-measured number of powdered polymers. The mounting
cylinder is then sealed, pressurized and heated to complete the polymerization process necessary to
solidly encase the metal sample. Although inferior in quality to compression-type molding, cold molding
(room temperature) is often used with epoxy to mount samples by simply mixing the epoxy and pouring
it over a sample that is positioned face down in a cold-mounting ring. When the epoxy cures the
specimen can be prepared. Caution must be exercised when cold mounting due to relatively poor
adhesion between the specimen edges and the epoxy plug; gaps often form which can degrade the
quality of the specimen.

Lab Procedure Mounting Procedure

Supplies for Cold-Mounting:

- KoldMound Kit (Vernon-Benshoff Co.): Mix 2 parts powder with 1 part liquid

- Plastic Mounting Ring with Removable Bottom

- 8 Ounce Paper Cup with Stirrer

- Weight Scale

- Liquid Soap

1. Apply liquid soap to the inner walls and base of the mounting ring.
2. Place the specimen in the center/bottom of the plastic mounting ring base with the examination
surface facedown.

3. Attach the mounting ring cylinder to the base by simple pressing firmly in place.

4. Mix the appropriate amount of KoldMount (2/1 Powder/Liquid - 15 grams of Powder/7.5 grams of
Liquid per Sample) in a paper cup.

5. Simply pour the epoxy mixture into the mounting ring; sample should be approximately 0.75" thick.

6. After one hour, remove the sample from the mounting ring and proceed with course grinding.

7. Coarse Grinding
In view of the perfection required in an ideally prepared metallographic sample, it is essential that each

preparation stage be carefully performed. The specimen must:

1. Be free from scratches, stains and others imperfections which tend to mark the surface.

2. Retain non-metallic inclusions.

3. Reveal no evidence of chipping due to brittle intermetallic compounds and phases.

4. Be free from all traces of disturbed metal.

The purpose of the coarse grinding stage is to generate the initial flat surface necessary for the
subsequent grinding and polishing steps. As a result of sectioning and grinding, the material may get
cold worked to a considerable depth with a resultant transition zone of deformed material between the
surface and the undistorted metal. Course grinding can be accomplished either wet or dry using 80 to
180 grit electrically powered disks or belts, but care must be taken to avoid significant heating of the
sample. The final objective is to obtain a flat surface free from all previous tool marks and cold working
due to specimen cutting.

An important factor throughout the Coarse Grinding and Fine Grinding Stages is that the scratches be
uniform in size and parallel to each other in any one grinding stage. Proper grinding involves rotation of
the sample by 90o between stages while the grinding angle must be held constant during the grinding at
any one stage.

The sample MUST be washed thoroughly before proceeding from one grinding stage to the next

Failure to follow this basic rule will result in transferring abrasive particles between stages and will cause
time-consuming, frustrating problems in removing unwanted scratches.

Lab Procedure-Coarse Grinding:

*Note: Safety Glasses must be worn when operating the Course Grinding Equipment
1. Label the specimen with your name so that it can be easily identified.

2. Turn the Motor On, then the water, adjust the flow to obtain a good film of water. Too much water
will cause a spray when it contacts the sample.

3. Beginning with the 120-grit belt and using both hands to hold the specimen, carefully place the
sample face onto the exposed area of the belt being careful not to contact the rotating surface with a
sharp edge of the specimen or your hand.

4. Applying moderate pressure evenly, move the sample left-and-right across the belt surface to obtain
uniform grinding. Use both hands to hold the specimen; unsecured specimens can "Catch an Edge and
FLY"!

5. Lift the sample from the wheel periodically to determine the progress of grinding but do not rotate
the sample. The 120-grit stage is complete when all the lines scratched in by the grinder are parallel on
the specimen surfaces. If any line or scratch is not in the same direction as the other lines, continue
grinding until all of the lines are parallel.

6. When all of the sample's scratches are parallel, carefully wash all of the debris from sample using tap
water and dry the specimen immediately using a paper towel or pressurized air to avoid corrosion.

7. Proceed to the 180-grit stage with the scratches oriented approximately perpendicular to the
intended grinding direction and repeat steps 3 through 6.

8. When the 180-grit stage is complete, you're ready to move on to the medium/fine grinding station.

8. Polishing
Polishing involves the use of abrasives, suspended in a water solution, on a cloth-covered electrically
powered wheel. Diamond abrasives provide the best, and most expensive, compounds utilized in
polishing; standard sized aluminum oxide powders are applied for general use purposes. Following the
final 600 grit fine-grinding stage, the sample MUST be washed and carefully dried before proceeding to
the first polishing stage! At the polishing stages, even hard dust particles in the air which settles on the
polishing cloth can cause unwanted scratching of the specimen! Careful washing of the specimen and
the operator's hands must be carried out prior to each stage of polishing! Beginning with 25-micron
suspended aluminum oxide particles (suspended in water) on a Nylon-cloth, the final fine-grinding
surface layer resulting from the previous grinding procedure should be completely removed with a
rotation rate of 150-200 rpm.
Lab Procedure - Mechanical Polishing

1. Safety goggles must be worn when using the Polishers!

2. Make sure your specimen and hands have been thoroughly cleaned before Polishing!

3. Begin with the 25-micron, nylon cloth polishing station!

4. Turn the water on adjusting to less than one drop per second!

5. Apply a small amount of the aluminum oxide abrasive solution to the polishing cloth.

6. When polishing the specimen, hold it with both hands, apply a moderate amount of pressure, and
don't let it go. The Rough Polishing Stages (5-25 microns) should take between 1 and 2 minutes each! If
you let go of the specimen it may fly, harm you or others in the laboratory and become damaged forcing
you to start over again with coarse grinding - hold it tight and be careful!

7. Do not contaminate the polishing wheel; cover the wheel when it's not in use!

8. Before proceeding to the next polishing stage, wash and dry both the specimen and your hands
thoroughly then rinse the specimen.

9. Repeat steps 4 through 8 for the 5-micron stage.

10. Proceed to the Final Polishing Station (1 micron) when all of the 25-micron marks are removed at the
5-micron stage.

9. Etching
Microscopic examination of a properly polished, unetched specimen will reveal only a few structural
features such as inclusions and cracks or other physical imperfections. Etching is used to highlight, and
sometimes identify, microstructural features or phases present. Even in a carefully prepared sample, a
surface layer of disturbed metal, resulting from the final polishing stage, is always present and must be
removed. Etchants are usually dilute acid or dilute alkalis in a water, alcohol or some other solvent.
Etching occurs when the acid or base is placed on the specimen surface because of the difference in rate
of attack of the various phases present and their orientation. The etching process is usually
accomplished by merely applying the appropriate solution to the specimen surface for several seconds
to several minutes.
Lab Procedure- Etching Steel Specimens

1. Place the specimen on the table under the Fume Hood with the polished surface up.

2. Turn on the Fume Hood.

3. Without touching the specimen surface, clean the surface with alcohol and let it dry using the hot air
gun. Do not let anything but the alcohol touch the specimen surface!

4. Using the Eye-Dropper, apply a few drops of Etchant to the specimen surface covering the entire
metallic surface of the specimen.

5. After about 20 to 30 seconds, rinse the Etchant into the sink with water and quickly rinse the
specimen with alcohol, but do not touch the surface!

6. Use the Hot Air Gun to dry the sample.

7. Proceed to Microscopic Examination; if further etching is required you may return and proceed
through steps 1 through 6 varying the time in step 5 depending on the results.

8. If the specimen has many scratches and marks or the microstructure cannot be seen after several
etches, return to fine grinding and go back through the necessary steps.

10. Microscopic Examination

Initial microscopic viewing should be done utilizing a stereomicroscope, which reveals a three-
dimensional scanning of the specimen surface. The specimen is placed on the stage of the microscope so
that its surface is perpendicular to the optical axis. Detailed viewing is done with a Metallurgical
Microscope. A metallurgical microscope has a system of lenses (objectives and eyepiece) so that
different magnifications (25X to 1000X) can be achieved. The important characteristics of the
microscope are: (1) magnification, (2) resolution and (3) flatness of field. The resultant magnification is
the product of the magnifying power of the objective and that of the ocular.

Scanning Electron Microscopes (SEMs) are capable of magnifications up to 20,000X and Transmission
Electron Microscopes (TEMs) are utilized to view at magnifications up to 100,000X for highly detailed
microstructural study.