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Metallography using Optical Microscopy

MICRO-SAMPLE PREPARATION AND GRAIN SIZE

DETERMINATION

I. PURPOSE AND REQUIREMENTS

Practice the steps of sample preparation to study the
microstructure of metals according to ASTM E3-01
standard.
Observe the microstructure of the prepared steel sample.
Determination of grain size of metal

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The method of metallographic analysis is to use an optical microscope with a

magnification of about 50-1000 times to observe, evaluate and analyze the
microscopic structure of metals and alloys (metals). The information of the
microstructure under the microscope that we can observe, store and analyze
includes phases in the microstructure, coating thickness, sphericity in cast iron,
defects of castings, of welds... in materials:

Evaluate the mechanical properties of the structure, technological parameters,

review the production process and develop new technology.

II. Sample preparation steps

1. Select and cut the sample
 The sample for microscopic study must be characteristic of the detail and
type of detail.
 Sample shape: cylindrical or rectangular with dimensions ranging from 12 to
25mm (0.5-inch to 1 inch).
 Use a hand saw (sample hardness less than 350HV) or a specialized cutting
machine, with lubricating oil and coolant. Ceramic and porcelain materials
are cut with a diamond blade.
 Note: cutting speed for each type of material; cutting too fast will generate
heat that will change the metal structure of the cut surface (the cut surface is
where the microstructure is observed). In some special cases, wire cutting
can be used to cut the sample.

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sample cutting
equipment

1. Select and cut the specimen

- In some cases: small samples, with special shapes, it is necessary to observe the
surface layer microstructure (observe the C, N, C+N, plating layers...)
Mounting sample

+ Hot mounting: standard sample diameter: 25, 32, 38mm

Plastic Phenolic ACRYLIC EPOXY

Status grainy flour grainy

Temperature 150-1650C 143-1770C 160-1770C
pressure(MPa) 21-28 17-28 24-41

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II. Sample preparation steps

2. Grinding
Grind on a grinder if the sample surface is rough after cutting.
 Grind on abrasive paper from coarse to fine :

European (P-grade) Standard grit Diameter (µm)

100 100 150
120 120 106
P240 240 58.5
P600 400 40.5
P1200 600 15.3
P2400 800 6.5
P4000 1200 2.5

Table 1. Types of abrasive paper for grinding samples

II. Sample preparation steps

2. Grinding
- Abrasive paper is placed on a flat and smooth table. When grinding, pay attention
to apply moderate pressure evenly, until the scratches are parallel to each other in
one direction. Then rotate the sample 90o, continue grinding until the scratches of
the first time are gone, on the surface of the sample there are new parallel
scratches, then switch to the next sandpaper (picture...)

Scratches form during the grinding process from rough to smooth.

Unsatisfactory grinding sample

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II. Sample preparation steps

3. Polishing: 2 polishing methods.
Electrolytic polishing: commonly used for stainless steel, Al, Cu, Mg alloy …

Hình 1. Nguyên lý của quá trình đánh bóng đ

Principle of electropolishing process

II. Sample preparation steps

3. Polishing
Mechanical polishing: polishing machine usually has one or more rotating discs. The
grinding disc is covered with a layer of soft felt or cotton cloth. During polishing, the
felt is always soaked with a grinding solution containing Cr2O3 oxide, diamond
powder with sizes from 6, 1, 0.25µm. Al2O3 powder (0.3-15µm).
- The sample is polished until the sample surface is scratch-free, flat and smooth

Sample surface after polishing

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II. Sample preparation steps

3. Etching
Etching method: After polishing, the sample is washed with water or alcohol, soaked
and dried. Use cotton to apply the etching solution to the surface of the sample so that
the solution corrodes the surface. When the surface of the sample has just changed
color, wash the sample with water, soaked and dried. Then observe under a
microscope.

The sample surface turns gray after etching

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Notes for sample preparation process :

 Deformations arising during cutting, grinding and polishing of the specimen shall be
removed to a size sufficient to be etched away.
 Coarse grinding marks must be removed, fine polishing scratches may be allowed
in production work.
 The sample must be absolutely flat, clean the sample carefully to avoid
contamination.
 Burling (large differences in height between structural members of different
stiffness) must be minimized; for best image clarity.
 Plated, coated, or impregnated surfaces must be kept flat if they are to be
analyzed, measured, or photographed.
 The sample washing, blotting and drying operations must be carried out quickly to
prevent the sample from being oxidized.
 The etching agent must be selected comprehensively or selectively depending on
the purpose (only clarifying the phase or component components, or at least
creating contrast and different colors between two or more phases), depending on
the purpose of the investigation, and must produce clear and high-contrast phase
boundaries, grain boundaries and phase images.

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III. Observation of metal structure on optical microscope

Optical microscope: consists of a system of optical lenses with

magnifications from 50 to 1000 times.

Metallurgical microscope (Model Axiovert 25CA)

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IV. Determine the grain size

3 methods to determine grain size
 Determined by average grain area

Z: the total number of grains

Z1 the number of whole grains
Z2 the number of cutted grains

N= Z x (0.064mm2/True Area)

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IV. Determine the grain size

 Determine the average diameter of the grain :

intersection of line
and grain boundary

Note: The more lines drawn on the image, the more accurate the
result.
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IV. Determine the grain size

Determine the grain size according to the standard table with the same
magnification of 100 times. In the experiment we use this method.

Figure 3: ASTM Grain Size Atlas,

with 100x Magnification

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V. Experimental report
1. Summarize the steps of microscopic sample preparation and state the objective of
each step.
2. Use the atlas to determine the grain size (image magnification x100).

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