Course Code: MSE 359/METE 357

Materials/Metallurgical Processing
Laboratory

Dr. Emmanuel Kwesi Arthur

Department of Materials Engineering,

Kwame Nkrumah University of Science and Technology,
Kumasi, Ghana

Email: [email protected]
Phone #: +233541710532
©2023
Experiment 6: Metallography Specimen Preparation, Examination
And Hardness Testing

•Objectives:

1. To familiarize with the procedure for preparation of material specimen for

microscopic examination.

2. To familiarize with the optical microscopy and metallography.

3. To determine grain size of metals.

4. To learn and measure the hardness of the metallographic specimens

Materials and apparatus:
1. Metallic specimen
2. Grinding/Polishing wheel
3. Metallurgical microscope
4. Hardness tester
5. Alumina suspension
6. Emery cloth
7. Etchant (98% ethanol + 2% nitric acid)
8. SiC grinding/polishing papers
9. Ethanol
 Introduction and Theory
• Metallography consists of the study of the composition and structure of metals
and alloys

• Optical microscopy is sufficient for general-purpose examination

• Electron microscopes (SEM and TEM), X-ray and electron diffractometers and
other scanning devices are used for advanced examination and research
laboratories

• Incorrect technique used in metallographic sample preparations may result in

altering the true microstructure and most likely lead to erroneous conclusions
 Steps for Specimen Preparation:
1.Sectioning
• Abrasive cutting (sectioning) offers the best solution to eliminate severe cold
work which can alter the microstructure of the sample giving smooth resultant
surface.

• Low-speed cut-off wheels are utilized in cases where the heat created by
standard abrasive cutters must be avoided.

• Rubber bonded abrasive cut-off wheels are most extensively used for wet
operation and resin bonds for dry cutting.
 2. Mounting
• Small samples are generally mounted in plastic for convenience in handling and
to protect the prepared specimen’s edges.

• Compression-type moulding is commonly applied to encase specimens in 1 to

1.5 inch diameter plugs of a hard polymer.

• Some compression moulding materials are;

1. Bakelite
2. Transoptic Thermoplastics
3. Coarse Grinding
• Course grinding can be accomplished either wet or dry using 80 to 180 grit.

• The final objective is to obtain a flat surface free from all previous tool
marks and cold working due to specimen cutting.

• Proper grinding involves rotation of the sample by 90o between stages while
the grinding angle must be held constant during the grinding at any stage.

• The sample MUST be washed thoroughly before proceeding from one grinding
stage to the next
4. Medium and Fine Grinding

• Medium and Fine Grinding must be carefully performed to produce a

scratch free surface by employing a series of successively finer abrasives .

• Wet grinding is generally applied in medium and fine grinding

• This prevents tempering, transformation, aging or incipient melting that can

occur due to the heat effect.

• Wet grinding also provides a flushing action for loose particles and keeps
sharp edges of the grinding medium exposed at all times.
5. Mechanical Polishing
• Polishing involves the use of abrasives and a polishing cloth that covers an
electrically powered wheel

• We have diamond abrasives and aluminium oxide abrasives

• During polishing, the specimen is initially held at one position on the wheel,
without rotation, until most of the previous grinding marks are removed

• After polishing, a properly polished specimen should have a mirror-like

surface free of scratches
 6. Etching
• Etching is used to highlight microstructural features or phases present

• Etchants are usually dilute acid or dilute alkalis in water, alcohol or some other
solvent

• Etching is merely immersing a polished surface in the appropriate etchant for

several seconds to minutes depending on the type of metal

• Etching can also be done by swabbing the etchant on the polished surface.
7. Microscopic Examination

• 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.

• Scanning Electron Microscopes (SEMs) and Transmission Electron

Microscopes (TEMs) are used for highly detailed microstructural study.
 Grain size calculation
• The ASTM grain size number, n, can be calculated using the following
relationship:

• N = number of grains per square inch at 100X

• n = ASTM grain size number
• M = Magnification

• If there are N grains per square inch at a magnification M then there are (N)1/2
grains along a 1-inch length.

•The size of each grain at magnification M is then 1/(N)1/2 inches.

•The actual size of the grain is given by Actual Grain Size =

Hardness Testing
Background
• Hardness is a measure of a material’s resistance to indentation or localized
plastic deformation (e.g., a small dent or scratch).

• Hardness testing involves a small indenter being forced into the surface of
the material under controlled conditions of load and rate of application.

• The depth or size of the resulting indentation is measured, which in turn is

related to a hardness number

• The softer the material, the larger and deeper the indentation, and the
lower the hardness index number

• The two most common methods applied to measure material hardness

macroscopically are Rockwell and Brinell methods
The Rockwell hardness test
• The Rockwell Hardness Test consists of measuring the additional depth to which
an indenter is forced by a heavy (major) load beyond the depth of a previously
applied light (minor) load.

• The minor load is applied first, and a "set" position is established

• Then the major load is applied at a prescribed, controlled rate without movement
of the workpiece.

• The major load is removed and the Rockwell hardness number is indicated on the
dial gage.

• Hardness value is based on the difference in depths of indentation produced by

minor and major load.
Figure 1 – Diamond-Cone Brale Indenter used in Rockwell
Hardness Testing

Figure 2 – Indentation in a work piece made by application of (a) the

minor load, and (b) the major load,

Figure 3: Rockwell hardness testing machine

Vickers Hardness Test
• Very Hard materials (e.g. Mild steel, case hardened steel, etc,) can be tested by the Vickers’
method
• It can also be used for a sub-group of hardness testing of welds.

Figure 4: Vickers Hardness Testing Machine.

 Brinell Hardness Test
•The Brinell Hardness Test consists of applying a constant load, usually 500 to 3000kg, on a
hardened steel ball-type indenter to the flat surface of a work piece.

•Tungsten carbide balls are recommended for Brinell testing materials of hardness from 444 HB up
to 627 HB

• The Brinell hardness test is performed on metals such as copper and aluminum alloys, steels and
cast irons.

•Calculating the Brinell hardness number (HB) by dividing the applied load by the surface area of
the indentation according to the expression:

•where:
• P = applied forced (kgf)
• D = diameter of indenter (mm)
• d = diameter of indentation (mm
Correlation between Hardness and Tensile Strength

•Both tensile strength and hardness are indicators of a metal’s

resistance to plastic deformation

•Consequently, they are roughly proportional. As a rule of thumb for

steels (steels only), the HB and tensile strength are related according
to;

TS (MPa) = 3.45 X HB or
TS (psi) = 500 HB
 POST LAB QUESTIONS
1. Briefly (not more than two sentences each) describe the steps involved in the
preparation of a metallographic sample:
• Sectioning
• Mounting
• Course Grinding
• Fine Grinding
• Polishing
• Etching

2. Why must metallographic samples be washed and carefully dried before

proceeding from one grinding or polishing operation to the next?

3. What is the purpose of etching metallographic samples?

4. Explain why metallographic samples are sometimes mounted in plastic?

5. Briefly explain the effect of grain size on the strength of a metal.

6. How should a Rockwell hardness reading of 63 be expressed if tested
with the C scale?

7. Would you expect a deep hardness indentation to result in a high

hardness number? Explain. Why isn't the diamond Brale indenter used on
copper alloys?

8. If 10 hardness tests were to be conducted on the same specimen, why

would large errors result if the measurements were all made at the same
point?

9. What is "Superficial Rockwell Hardness Testing" and when should it be

used?

10. Determine the Tensile Strength of a steel sample with a Rockwell C

reading of 63.