International
Tables for
Crystallography
Volume C
Mathematical, physical and chemical tables
Edited by E. Prince

International Tables for Crystallography (2006). Vol. C, ch. 3.5, pp. 171-172

Section 3.5.1.2. Thin-section preparation

N. J. Tighe,a J. R. Fryerb and H. M. Flowerc

a42 Lema Lane, Palm Coast, FL 32137-2417, USA,bDepartment of Chemistry, University of Glasgow, Glasgow G12 8QQ, Scotland, and cDepartment of Metallurgy, Imperial College, London SW7, England

3.5.1.2. Thin-section preparation

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Bulk samples are reduced in size by cutting slices with a slow-speed diamond-bladed saw or by grinding the sample flat with a diamond-impregnated grinding wheel. The surfaces are fine ground, polished or left in the as-received condition as required for the analysis. Typical petrographic sections are 100 to 200 µm thick. Disc-shaped specimens are cut from the petrographic thin sections with an ultrasonic drill or a diamond-core drill (Tighe, 1964[link]).

Although discs and petrographic sections can be ground and polished as thin as 30 µm before ion thinning, experience has shown that such thin discs are extremely fragile and may not survive long enough for the complete analysis, which may require examination over long periods of time in different instruments. Extremely fragile materials and porous materials can be pressure impregnated with epoxy or bakelite before slicing and grinding. Cross-section specimens (Bach, 1970[link]) can be stacked together and pressure mounted in epoxy or plastic before carrying out the slicing and cutting operations.

Before the element-analysis techniques were available, thin fragile specimens were cemented to copper single-hole grids. However, in X-ray microanalysis, spurious copper signals are obtained from the mounting grid and this practice is no longer recommended unless absolutely necessary. Beryllium grids are available and should be used when extra support is required.

The mechanical profiling of a disc specimen is carried out using a diamond-impregnated metal tool, a small wood dowel with diamond paste, a small metal disc or ball tool with diamond or alumina paste that is held in a variable-speed hand drill or in a semi-automated profiling machine. The specimen is cemented to a metal disc or glass slide and the processes are monitored carefully with a light microscope. When an ultrasonic tool is used it must be slightly rounded because a flat tool will produce a profile with a hump at the centre.

The mechanical profiling technique must be used with some care in order to minimize surface strain from grinding. The damage consists of cracks, embedded grinding debris, and pull-outs. It is possible for cracks to be introduced by grinding and then propagated by both the continuing contact pressure and the presence of the liquid abrasive carrier. In some cases, it may be necessary to maintain inert grinding conditions by selecting special lubricants or by chilling the sample. These mechanical profiling techniques require some practice to obtain reproducible sample conditions.

Profiling in the ion-beam thinner occurs when a well aligned beam that is smaller than the specimen diameter or less than 2 mm in diameter is used or when the specimen edges are masked with the holder. The disc specimens can be profiled on both surfaces or one surface can be left flat. A flat surface is preferable for electron-diffraction analysis as well as for secondary electron imaging.

The mechanical preparation of specimens has been greatly simplified by the development of two instruments by Gatan Inc. (6678 Owens Drive, Pleasanton, CA 94566, USA) (Alani & Swann, 1990[link]). The first is a holder for disc samples that is used on a polishing wheel to grind and polish discs to a specific thickness. This holder has a height adjustment for the specimen, which can be ground and polished to a thickness of 50 µm by the use of various grades of abrasive. With the second instrument, called a `dimpler™', the polished disc is profiled or dimpled on one side. This dimple is ground and polished with a sensitivity of 1 µm. The dimpled disc is then ready to be thinned in an ion-bombardment instrument.

References

Alani, R. & Swann, P. R. (1990). Workshop on specimen preparation for transmission electron microscopy of materials. Materials Research Society, Vol. 199, p. 85.
Bach, H. (1970). Application of ion sputtering in preparing glasses and their surface layers for electron microscope investigations. J. Non-Cryst. Solids, 3, 1–32.
Tighe, N. J. (1964). Jet thinning device for preparation of Al2O3 electron microscopy specimens. Rev. Sci. Instrum. 35, 520–521.








































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