Sample Preparation.pdf
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1. Specimen preparation involves sectioning, mounting, grinding, polishing, and etching. Sectioning reduces the specimen size, and mounting embeds specimens in resin for shaping. 2. Grinding and polishing flatten the surface using abrasives in sequence from coarse to fine grit. Etching enhances contrast by chemically dissolving areas of different composition. 3. Mounting techniques include hot mounting using heat and pressure to embed in powder, and cold mounting casting resin around specimens at room temperature.
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The document provides guidelines for preparing metal specimens for microscopic examination. Key steps include carefully selecting and cutting a representative sample, mounting it, grinding it with successively finer grit paper to create a flat surface, polishing it to remove scratches, and sometimes etching it to reveal microstructural features. Proper preparation helps facilitate clear examination and accurate interpretation of grain structure, phases, inclusions and other microscopic characteristics of the material.
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This document describes the procedure for preparing a metal specimen for microscopic observation. Key steps include:
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- 2. 1. Sectioning 2. Mounting 3. Grinding 4. Polishing 5. Etching PREPARATIONOF SPECIMEN
- 3. Sectioning • Sectioning serves two purposes: – generating a cross-section of the specimen to be examined; – reducing the size of a specimen to be placed on a stage of light embedded in mounting microscope, or reducing size of specimen to be media for further preparation processes. • Cutting
- 4. Microtomy • Microtomy refers to sectioning materials with a knife. It is a common technique in biological specimen preparation. • It is also used to prepare soft materials such as metals. • Tool steel, tungsten carbide, glass and diamond materials. polymers and soft are used as knife • A similar technique, ultramicrotomy, preparation of biological and polymer electron microscopy. is widely used for the specimens in transmission 52
- 5. Mounting • Mounting refers to embedding specimens in mounting materials (commonly thermosetting polymers) to give them a regular shape for further processing. • Mounting is not necessary for bulky specimens, but it is required for specimens that are too small or oddly shaped to be handled or when the edge of a specimen needs to be examined in transverse section. • Mounting is popular now because most automatic grinding and polishing machines require specimens to have a cylindrical shape. • There are two main types of mounting techniques: 1. hot mounting 2. cold mounting. 53
- 6. Hot Mounting equipment • Hot mounting uses hot-press as shown in Figure. • A specimen is placed in the cylinder of a press and embedded in polymeric powder. • The surface to be examined faces the bottom of the cylinder. Then, the specimen and powder are heated at about 150 ◦C under constant pressure for tens of minutes. • Heat and pressure enable the powder to bond with the specimen to form a cylinder.
- 7. ColdMounting • In cold mounting, a polymer resin, commonly epoxy, is used to cast a mold with the specimen at ambient temperature. • A cold mounting medium has two constituents: a fluid resin and a powder hardener. • The resin and hardener should be carefully mixed in correct proportion. • Curing times for mounting materials vary from tens of minutes to several hours, depending on the resin type.
- 8. • Cold mounting of specimens: • (a) place specimens on the bottom of molds supported by clamps • (b) cast resin into the mold.
- 9. • Cold mounted specimens: • (a) mounted with polyester • (b) mounted with acrylic • (c) mounted with acrylic and mineral fillers.
- 10. Grinding • Grinding refers to flattening the surface to be examined damage caused by sectioning. • The specimen surface to be examined is abraded using a graded sequence of abrasives, starting with a coarse grit. and removing any • Abrasive paper is graded according to particle size of abrasives such as 120-, 240-, 320-, 400- and 600-grit paper. •Running water is supplied to cool specimen surfaces during hand grinding.
- 11. Polishing • Polishing is the last step in producing a flat, scratch-free surface. • After being ground to a 600-grit finish, the specimen should be remove all visible scratches from grinding. • Polishing generates a mirror-like finish on the specimen surface further polished to to be examined. • Polishing is commonly conducted by placing the specimen surface against a rotating wheel either by hand or by a motor- driven specimen holder. • Coarse polishing uses abrasives with a grit size in the range from 3 to 30μm.
- 12. Etching • Chemical etching is a method to generate contrast between microstructural features in specimen surfaces. • Etching is a controlled corrosion process by electrolytic action between surface areas with differences in electrochemical potential. • During etching, chemicals (etchants) selectively dissolve areas of the specimen surface because of the differences in the electrochemical potential by electrolytic action between surface areas that exhibit differences.