Introduction to Optical Microscope

-Sample Preparation Techniques

Metallography:
ƒ A systematic method to examine microstructure of materials (mainly
metallic materials).
ƒ Metallography does not only apply to metallic materials, such
technology
can also be used to examine ceramics, polymers and semiconductors.

Sample preparation for optical microscopy

(1) Sectioning
Why sectioning?
1. Size limitation of specimen to be examined under optical microscope.
2. Locate area needs to be selected from a large sample.

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Introduction to Optical Microscope
-Sample Preparation Techniques
Abrasive Cutting is the most common sectioning method.

The abrasive cutoff disc is usually made by silicon carbide particles, or

diamond particles (called Diamond saws)
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 Introduction to Optical Microscope
-Sample Preparation Techniques

Electric Discharge Machining

(EDM)
Electrically conductive materials can be
sectioned by EDM.
Cutting is accomplished by an electric
discharge between an electrode and the
sample submerged in a dielectric fluid.

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 Introduction to Optical Microscope
-Sample Preparation Techniques
Microtomy is useful to
prepare soft materials such as
polymer samples.

Steel, glass or diamond knife in

a microtome can cut sample to
a very thin section.

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 Introduction to Optical Microscope
-Sample Preparation Techniques
(2) Mounting is required when (1) sample is small or oddly shaped to be
handled.(2) The sample edge area needs to be examined.

Thermal mounting:
The sample is embedded in
thermosetting plastics at
elevated temperatures and pressure.

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 Introduction to Optical Microscope
-Sample Preparation Techniques
Cold mounting:
The sample is embedded in epoxy type of materials.

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Introduction to Optical Microscope
-Sample Preparation Techniques

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Introduction to Optical Microscope
-Sample Preparation Techniques
Adhesive mounting: The sample is glue to a piece of large holder.
Clamps: The sample is fixed in mechanical clamping devices.

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Introduction to Optical Microscope
-Sample Preparation Techniques
(3) Grinding

1. Grinding removes the damages on the surface produced by sectioning.

2. Grinding also produced damages which must be minimized so that subsequent
grinding with finer abrasives.
3. At the end of grinding phase, the only grinding damages present must be from
the last grinding step.
4. Such damages will be removed by polishing.

Grinding materials: Abrasive paper (covered with silicon carbide grits). Commonly, a
series of abrasive paper is used, from coarse to fine one.

Grit sequence: 120-, 240-, 320-, 400-, and 600-mesh

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 Introduction to Optical Microscope
-Sample Preparation Techniques
The initial grit size depends on the
surface roughness and depth of
damage from sectioning.

• Surfaces cut by abrasive cutoff

saw start with 120 to 240 grits.
• Surfaces cut by EMD or diamond
saw start with 320 to 400 grits.

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 Introduction to Optical Microscope
-Sample Preparation Techniques
Samples of grinding and polishing

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Introduction to Optical Microscope
-Sample Preparation Techniques
(4) Polishing

After being ground to a 600-grit finish, the sample is polished to produce a flat and
scratch-free surface with high reflectivity.

Coarse polishing: abrasives in the range of 30 ~ 3 µm using diamond grits of

several micrometers.

Fine polishing: abrasives in the range of ≤ 1 µm using diamond grits of 1 µm,

followed by 0.3 ~ 0.05 µm alumina slurries.

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Introduction to Optical Microscope
-Sample Preparation Techniques

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 Introduction to Optical Microscope
-Sample Preparation Techniques
Artifact structure from improper grinding
Surface deformation from improper grinding should be avoid, otherwise the
microstructure may be obscured as shown below.

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Introduction to Optical Microscope
-Sample Preparation Techniques
Artifact from improper polishing
Polishing should produce a scratch-free surface. Excessive pressure may cause
artifact of second phase particles as shown below.

20 x 200 x

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 Introduction to Optical Microscope
-Sample Preparation Techniques
n Ultrasonic wash Ultrasonic wash Ultrasonic wash
io
ct
re
di
ng
hi

Polishing
l is
Po

OM
400 Grit

OM
240 Grit 600 Grit

de r

de r
un

un
eck

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Ch

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6 µm 3 µm 1 µm 0.25 µm
Polishing HKUST
Introduction to Optical Microscope
-Sample Preparation Techniques

Glass Fiber Composite

A thin section after

grinding on the machine

Microstructure of wood cell

Patro-thin sectioning machine

PP crystal structure
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 Introduction to Optical Microscope
-Sample Preparation Techniques

(5) Etching
Using chemical to dissolve selectively
the surface of materials in order to
reveal the inhomogeneous nature in
microscopic scale.

For example the grain boundaries of

polycrystalline metal

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 Introduction to Optical Microscope
-Sample Preparation Techniques
Etching is basically a controlled corrosion process resulting from electrolytic action
between surface area of different potential.

Electrolytic activity results from local physical or chemical heterogeneities which

render some features anodic and others cathodic under the specific etching
conditions.

Chemical Etchants produce contrast by

• Crystal faceting
• Selective phase dissolution.

Common chemical etchants have three components:

• A corrosive agent (acids)
• A modifier (alcohol, glycerin…)
• An oxidizer (hydrogen peroxide, Fe3+, Cu2+…)

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Introduction to Optical Microscope
-Sample Preparation Techniques
Common etchants for metals (for example)

Keller’s reagent
2.5 ml HNO3/1.5 ml HCl
1.0 ml HF, 95 ml water for Al and alloys

Nital
1-10 ml HNO3 in 90-99 ml methanol for Fe and steel

Picral
4 -10 g picric acid, 100 ml ethanol for Fe and steel

10 ml HF/5 ml HNO3 85 ml water for Ti and alloys

NH4OH/3% H2O2 for Cu and alloys

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Introduction to Optical Microscope
-Sample Preparation Techniques
Etchants for polymers (for example)

Aqueous solution of CrO3 for bulk polypropylene (PP)

Aqueous solution of H2SO4/H3PO4/CrO3 for ABS, HIPS and PPO

Etchants for minerals (for example)

Concentrated HCl for CaO, or MgO.

Aqueous solution of H3PO4 for Al2O3
Aqueous solution of HNO3/HF for CeO2, SrTiO3, Al2O3, and ZrO-ZrC.

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Introduction to Optical Microscope
-Sample Preparation Techniques
Etchant effects on microstructure images

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