Introduction to Optical Microscope

Sample Preparation Techniques Technique

Introduction to Optical Microscope

-Sample Preparation Techniques
Metallography: A systematic method to examine microstructure of materials (mainly metallic materials). 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.

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)

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.

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.

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.

Introduction to Optical Microscope

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

Introduction to Optical Microscope

-Sample Preparation Techniques

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.

Introduction to Optical Microscope

-Sample Preparation Techniques
(3) Grinding 1. 2. 3. 4. Grinding removes the damages on the surface produced by sectioning. Grinding also produced damages which must be minimized so that subsequent grinding with finer abrasives. At the end of grinding phase, the only grinding damages present must be from the last grinding step. 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

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.

Introduction to Optical Microscope

-Sample Preparation Techniques
Samples of grinding and polishing

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 m using diamond grits of several micrometers. Fine polishing: abrasives in the range of 1 m using diamond grits of 1 m, followed by 0.3 ~ 0.05 m alumina slurries.

Introduction to Optical Microscope

-Sample Preparation Techniques

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.

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

Introduction to Optical Microscope

-Sample Preparation Techniques
Ultrasonic wash
di re ct io n

Ultrasonic wash

Ultrasonic wash

Po l is hi ng

Polishing 240 Grit 600 Grit

Ch eck un de r OM

400 Grit

6 m

3 m

Ch eck un de r OM

1 m Polishing

0.25 m

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

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

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+)

Introduction to Optical Microscope

-Sample Preparation Techniques
Common etchants for metals (for example) Kellers reagent 2.5 ml HNO3/1.5 ml HCl 1.0 ml HF, 95 ml water Nital 1-10 ml HNO3 in 90-99 ml methanol Picral 4 -10 g picric acid, 100 ml ethanol 10 ml HF/5 ml HNO3 85 ml water NH4OH/3% H2O2

for Al and alloys for Fe and steel

for Fe and steel for Ti and alloys for Cu and alloys

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

Introduction to Optical Microscope

-Sample Preparation Techniques
Etchant effects on microstructure images