EYPME1A

METALLOGRAPHY, PRINCIPLES AND PRACTICE

Chemical & Metallurgical Engineering

DI0850/DE0850 – POS C
(Diploma Metallurgy)

www.vut.ac.za
Lecturer: Ms. Baloyi N
2024: January Semester 1
 www.vut.ac.za

INDEX
• Introduction
• Tools of a metallurgist
• Metallographic steps
• Microscopes
• Material testing 2

The contents of this presentation is confidential. ©VUT

Microscopy
 EYPME1A: Learning Unit 1

Microstructure
• Good metallographic preparation
• Light microscopy imaging techniques, such as brightfield, darkfield,
are used to examine metal surfaces and polished/etched
metallographic cross sections.
• Grain size and shape, inclusions, and internal stress patterns are
some of the common items of interest for light microscopy imaging
of metals.

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 Light Microscopy EYPME1A: Learning Unit 1

• The light microscope is the most important device in metallography. Currently more
detailed type of microscopy such as the transmission electron microscope (TEM) and
the scanning electron microscope (SEM) are overcoming limitations of the light
microscope on the bases of resolution and depth of field. Still, they have not reduced
the importance of the light microscope.
• In any study of materials, the wisest procedure is to start on the macroscopic level
before proceeding to microscopic and submicroscopic detail.
• For this level of study we discuss the application of light microscopy, typically at
magnifications between about 50 and 2000X, to the study of materials.
• Although a thorough understanding of optics is not usually necessary for the bulk of
metallographic observations, a basic knowledge is required in more fundamental
studies or in working with unusual or difficult materials.
• Although the bulk of metallographic observation is conducted using incident bright-
field illumination, application of other illumination techniques is imperative with
materials exhibiting low contrast or with optically anisotropic materials, especially
those that are difficult to etch.

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 EYPME1A: Learning Unit 1

cont….
In order to obtain optimum resolution of detail, the sample surface
being examined must have adequate contrast. The types of
surfaces examined by these techniques include the following:

• As-polished surfaces (inclusions and precipitates)

• As-polished surfaces of optically anisotropic metals
• Relief-polished, unetched surfaces
• Etched surfaces

The technique used depends on the nature of the problem, the

expertise of the investigator, and the available equipment.
Microscopy methods for enhancing contrast include the following:

• Dark-field illumination
• Polarized light
• Phase contrast
• Interference methods
• Filters
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Examination modes in light microscopy EYPME1A: Learning Unit 1

• High resolution can be achieved only if there is adequate contrast between details so
that varying amounts of light reach the observer's eye.
• There are two types of features that can be discerned on metal surfaces—amplitude
features and optical phase features. Amplitude features occur as a result of reflectivity
differences.
• Samples with the same reflectivity but with differences in surface height can be
detected by the differences in optical phase, since there is a phase-path reflectivity
difference.
Methods of Examination
Bright-field illumination The predominant method of examination of metallurgical
specimens is by incident bright-field illumination.
Oblique illumination Oblique illumination is obtained by decentering the condenser
assembly or the mirror.
Dark-field illumination Dark-field illumination produces an intensity contrast image
from effects which do not usually contribute significant intensity contrast to the image in
bright-field illumination.
Polarized light While the use of polarized light in the identification of minerals is a long-
established important practice, its use in metallography has, in general, been limited to
the study of only certain metals
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Photo-micrographs
EYPME1A: Learning Unit 1

Characteristics of a photo-micrograph
• Clear
• Flat without blurriness
• Should show features of the
material
• Should have a scale bar
• Use corresponding magnification
to view details.
c d

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Steps to a good photomicrograph

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 Specimens are embedded in resin to facilitate their
EYPME1A: Learning Unit 1
handling and to improve the preparation result. For the Cutting Machine can be used to cut various
best possible result, specimens should be cleaned prior metal or non-metal specimens so as to observe
to mounting. The best possible adhesion of resin to the the Metallographic structure.
specimen requires the surface to be free from grease
and other contaminants.

Proper grinding removes damaged

or deformed surface material.
Grinding removes material using
fixed abrasive particles that
produce chips of the specimen
material. The process of making
chips with a sharp abrasive grain
Polishing is the final stage in producing a produces the lowest amount of
surface that is flat, smooth, scratch-free and deformation in the specimen,
mirror like in appearance. Such a surface is while providing the highest
necessary for subsequent accurate removal rate.
metallographic interpretation, both qualitative
& quantitative. Etching: the purpose of etching is
to make visible the many
structural characteristics of the
metal or alloy. The purpose must
be such that the various parts of
the microstructure may be clearly
differentiated.

Microscopy: Used for investigating

microscopically the structure of
metals. The metal under examination
is polished and then etched, this
process disclosing its crystalline
structure.

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Obtaining Good Photomicrographs EYPME1A: Learning Unit 1

In the observation of details through the microscope, three

separate effects are used to create the visual impression of good
focus over the field of view:
1. The depth of field of the objective (depends on magnification, NA,
light wavelength, etc.)
2. The adjustment of the fine-focus control while viewing
3. The slight change in focus due to eye accommodation
In the photographic process, only the first effect can be used. In
obtaining sharp photomicrographs, the microscopist must control
the following variables:
• Eliminate vibrations
• Align illumination
• Match illumination color to objective corrections
• Maintain cleanliness of optics
• Correct adjustment of field and aperture diaphragms
• Focus precisely, generally with the aid of a focusing

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 Camera attachment, consisting of a
film casing, shutter and photo tube
EYPME1A: Learning Unit 1

Eyepiece micrometer with a

measuring drum and zeroing device

Knurled screw for focusing the light

on the test-piece surface, and knob
for centering the light band on the
reticle

Combined coarse and fine focusing adjustment

Switch for
ocular viewing
photographing

Revolving nosepiece for pairs of objectives

of 200 X and 400 X magnification

Mechanical stage 2,5X25 mm (1 x 1 in.)

On — off switch
with brightness adjuster

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Hardness
 Microhardness EYPME1A: Learning Unit 1

• Microhardness testing, or the technique of making hardness measurements

of phases observable only with the aid of the light microscope, is a very
useful tool.
• Most microscope manufacturers supply accessory equipment for
microhardness determinations with bench microscopes or metallographs.
• Single-purpose units are also available which cover a variety of loads from
as low as 1 to 1000 g and, thus, can be used for measuring the hardness
of a wide range of materials (soft to hard) or sizes.
• Microhardness testing is useful for determining the depth of
decarburization, carburization, nitriding, etc. Microhardness testing is also
useful in phase identification and is ideal for evaluating weldments.
• This method accurately reflects the fundamental intuitively simple concept
widely used in the metals industry. It is a low costly and straightforward
manner of implementation, it cannot be defined rigorously nor be
measured absolutely, it is an estimate of the mechanical properties of
metals.
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 cont…. EYPME1A: Learning Unit 1

• However, hardness data do provide important information about material quality that is of
indispensable value in quality control, design, alloy development, and materials selection.
The science of physical metallurgy has relied heavily on hardness tests.
• In its most general sense, hardness implies resistance to deformation. As applied to metals,
hardness is a measure of resistance to plastic, i.e., permanent, deformation as would be
determined in a uniaxial tensile test.
• It is not surprising, therefore, that hardness can be correlated with both yield strength and
tensile strength. Hard materials exhibit high strengths, while soft materials have low
strengths.
• Hardness also has other connotations—resistance to scratching, resistance to cutting,
ability to cut softer materials, brittleness, lack of elastic damping, wear resistance, lack of
malleability, magnetic retention, and so forth.
• Because of these different attributes, the myriad of materials tested, and the multitude of
tests available, hardness has not been defined in the neat, concise, universal manner
normally desired in science.
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Indentation hardness EYPME1A: Learning Unit 1

• Hardness testing using indentations can be accomplished in several ways. If a hard

object is pressed into the surface of a softer material with enough force to produce an
indentation, the indentation size will depend on the magnitude of the applied force and
the hardness of the indented material.
• For a fixed set of test conditions, if two different materials are indented, the one with
the smaller indentation is harder. If these test conditions can be accurately controlled
and reproduced, a hardness number can easily be calculated from the applied load and
the projected area of the impression in terms of a pressure in units such as kilograms
per square millimeter.
Indentation Size and Shape Changes
• It is well recognized that on removal of the indenter, size and shape changes of the
impression can occur in varying amounts as a result of elastic recovery.
• Recovered cone impressions exhibit larger included angles than the unloaded
impression, while recovered ball impressions exhibit an increased radius of curvature.
• With microindentation hardness testing, because of the small size of the impression is a
finely polished surface required. In this instance, the quality of the polished surface
affects the microhardness values substantially as the test load decreases.

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 Methods of hardness test EYPME1A: Learning Unit 1

a. Brinell Hardness
• Brinell uses a 10-mm diameter ball pressed into
the flat, smooth specimen surface for 30 s.
After the load is removed, the impression
diameter is then measured. To calculate the
hardness value, the Brinell indentation is used
to calculate the pierced surface; therefore
divide the load by the surface area of the
impression.
• Brinell decided to adopt standard loads L of 500
kgf (kilograms-force) for soft metals and 3000
kgf for harder metals such as steel. The Brinell
hardness number (HB) is calculated on the
basis of the average of two measurements of
the impression diameter d made at right angles
to each other using the following formula in
which D is the ball diameter:

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b. Vickers Hardness EYPME1A: Learning Unit 1

• A pyramidal-shaped indenter made from diamond in order to test

metals too hard. • A square-based pyramid was chosen
with an angle of 136° between
opposite faces in order to obtain
hardness numbers similar in
magnitude to Brinell numbers.
• The ideal dID ratio for a spherical
indenter is 0.375. Tangents drawn to
the ball at the impression edges meet
below the center of the impression at
an angle of 136°.
• Thus, a square-based pyramidal
indenter with a 136° angle between
opposite faces will produce Vickers
hardness (HV) values approximately
equal to HB values over the range of
the Brinell test.
• This seemed to be the better
hardness method.
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c. Knoop Hardness
EYPME1A: Learning Unit 1

• The Knoop hardness test method, also referred to as a microhardness

test method, is mostly used for small parts, thin sections, or case
depth work.
• A pyramid shaped diamond is used for testing
in the Knoop scale. This indenter differs from
the pyramid indenter used on a Vickers test.
The Knoop indenter is more elongated or
rectangular in shape.
• Since the test indentation is very small in a
Knoop test, it is useful for a variety of
applications: testing very thin materials like
foils
• Sectioning is usually necessary; test in order
to provide a small enough specimen that can
fit into the tester.
HK = 14.229L/d2 • Additionally, the sample preparation will need
to make the specimen’s surface smooth to
permit a regular indentation shape and good
measurement, and to ensure the sample can
be held perpendicular to the indenter.

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d. Rockwell Hardness EYPME1A: Learning Unit 1

• As the development of high strength metals progressed they required to

tests with the large impression size. The fact that high-hardness steels
could not be tested, prompted development of other tests such as the
Vickers test just described and the Rockwell test. Rockwell was a
metallurgist in a ball-bearing factory, invented the tester known today by
his name. In the original tester, the hardness scale was 0 to 100, with low
hardness numbers for hard materials and high numbers for soft materials.

• In the Rockwell test, a 10-kgf

minor load is used to press the
indenter into the sample and
establish a zero point for the
test. Then the major load,
60,100, or 150 kgf, is applied
and removed.
• The hardness is indicated on
the dial gauge with the minor
load still applied. The hardness
is an inverse function of the
penetration depth due to the
major load
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 EYPME1A: Learning Unit 1

Exercise 1/Quiz 1
Submission TBA

Hardness conversions
1. Consult the tables in ASTM E140 to convert hardness values
from one method to the other using these references:
• Brinell
• Vickers
• Rockwell
• Knoop

Describe your observation with the hardness values.

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Summary
• Metallurgist are the quality control specialist in
components manufacturing. One should have skills to
investigate poor and properly produced parts in a plant by
learning microstructural investigation.
• As much as you could understand the macrostructure, the
microstructure is the most important part of the properties
of metals, be able to learn their effect thereof.
• Microscopy dwell deeper into the vision of human eye to
view micro arrangement of structures in metals, though not
deeper to the atomic scale.
• The microhardness and metallography are basically
laboratory minimum practice to understand the type and
composition of metal.
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Typical Questions

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3
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Microstructures

1. Objectives

Magnification

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 EYPME1A: Learning Unit 1

2. Magnification

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3. Scale bar

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4. Illumination

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Hardness EYPME1A: Learning Unit 1

1. Impressions

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Optical Microscope
• Flat surface
Measuring for Vickers,
the measured diagonals
should not deviate more
than 5% from each
other. Also the indenter
should be perpendicular
to the test surface and
not deviate from this
with more than 2° in
order to give a reliable
result.

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Optical Microscope: EYPME1A: Learning Unit 1

poor preparation • Incorrect load

• Flat surface 2. Poor preparation
Measuring for Vickers,
the measured diagonals After impression, the
should not deviate more surface should not
than 5% from each show excessive load
other. Also the indenter ridges, this could
should be perpendicular result to incorrect
to the test surface and reading. Confirm
Cnfirm the
not deviate from this amount of load prior
with more than 2° in to testing.
order to give a reliable
result.

• Polishing
If the surface finish of a
specimen is too rough, it
might be problematic to
evaluate the corners of an
2. Poor preparation indent, especially if
automatic equipment is
used. A clean reflective
surface is needed. Also the
surface preparation should
have a minimum influence
on the properties of the 30
material to be tested.
 • Incorrect load
Optical Microscope: poor preparation EYPME1A: Learning Unit 1
• Flat surface
Measuring for Vickers,
the measured diagonals After impression, the
should not deviate more surface should not
than 5% from each show excessive load
other. Also the indenter ridges, this could
should be perpendicular result to incorrect
to the test surface and reading. Confirm the
not deviate from this amount of load prior
with more than 2° in to testing.
order to give a reliable
result. 2. Poor preparation
• Etching & cleaning
• Polishing
If the surface finish of a
specimen is too rough, it
might be problematic to
evaluate the corners of an
indent, especially if
automatic equipment is
used. A clean reflective
Etching should, as far as possible, be avoided since it
surface is needed. Also the
results in a less reflective surface. If etching is
surface preparation should
necessary, a light etch is preferable so that it will be
have a minimum influence
possible to discriminate the corners of the indent.
on the properties of the
material to be tested.
Always ensure that the specimens are cleaned
properly, otherwise e.g. dirt or fibres from the
polishing cloth might complicate the reading. 31
Optical Microscope: poor preparation EYPME1A: Learning Unit 1

Example 1: 3. Calculation
A 10mm diameter Brinell hardness (HB)
indenter produced an indentation of 2.50mm
diameter on a steel alloy when a load of
1000kg was used. Calculate the HB of this
material.

Solution 1: work it out for Friday

class

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