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, p. 174

Section 3.5.2.1. Thin sections

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

3.5.2.1. Thin sections

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Samples are taken from the bulk material either by a mechanical cutting operation or by spark erosion. The former is the most common technique, but it necessarily produces a region of plastic deformation, and hence microstructural modification, in the material adjacent to the cut faces. The severity of the damage is greatest with cutting by a hacksaw or bandsaw and least with machine cutting using an oil- or water-cooled and lubricated abrasive wheel. The lubricant prevents heating of the sample, which can also lead to microstructural modification. Whatever method of mechanical cutting is adopted, it is necessary to remove a section of sufficient thickness that the slice will contain a central core of unmodified microstructure. The minimum thickness required is not only a function of the cutting method but also of the material cut since softer materials will be damaged to greater depths than hard ones. Typically, a hacksawn slice thickness will lie in the range 2–5 mm, whereas with abrasive cut-off the minimum useable slice thickness is reduced by an order of magnitude.

Subsequent thinning can be carried out by grinding using water-lubricated and -cooled silicon carbide abrasive discs to grind down from both faces of the sample to remove the regions of surface damage. As the section is reduced, successively finer grades of abrasive are required to reduce the depth of damage that they themselves introduce into the material. The depth of damage may be between 10 and 50× the depth of penetration of the abrasive particles depending on the hardness of the metal (Metals Handbook, 1985[link]). Typically, grit sizes of 240 to 600 are employed to reduce the section thickness to 0.1 to 0.4 mm.

A spark-erosion method, which employs a high-voltage spark discharge between a tool and the work piece (immersed in paraffin or other insulating liquid with a high dielectric constant), can be used to perform the cutting. The metal is melted locally and eroded at the point of discharge. Both work piece and tool suffer erosion; for cutting slices, a continuously fed wire is used as the tool. With this method, cuts of the order of millimetres in depth may be made while retaining a constant tool profile. Damage at the sample surface is severe involving local melting and large thermally induced stresses. The depth of damage is typically less than 100 µm (Jansen & Zeedijk, 1972[link]) and is readily removed from slices during subsequent thinning procedures.

From the slice, the thin foil may be prepared by either the disc or the window method. For the window technique, samples approximately 10 mm square are employed and electron-transparent sections are cut from them after the sample has been thinned chemically or electrochemically.

For the disc technique, samples of diameter to fit in the electron-microscope specimen holder (typically 3 mm) are cut from the thin sections. The discs may be cut from many materials mechanically using a suitable sample stamping machine. However, in cases where the material is either too hard to stamp successfully (e.g. tool steels) or so soft that unacceptable mechanical damage would result, the discs are cut out by spark machining. A tubular tool is employed and it is moved towards the sample in order to keep a constant spark gap. The edges of discs cut in this way, or by punching, require no treatment as only the central portion of the disc is subsequently thinned to electron transparency.

References

Jansen, J. & Zeedijk, H. B. (1972). Deformation layers in spark-machined and mechanically sectioned specimens of 0.2% mild steel. J. Phys. E, 5, 973–975.
Metals Handbook (1985). Metals Park, Ohio. American Society for Metals.








































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