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Sample preparation vs quality of X-ray phase analysis results

Chylińska R.

Archives of Foundry Engineering

2007

Vol. 7, iss. 4

21-24

In this study, taking as an example the creep-resistant austenitic cast steel, the results of the investigations were presented whose aim was to show what effect the specimen surface condition, discussed in terms of its roughness obtained by grinding, polishing with diamond paste, electrolytic polishing and etching, may have on the quality of results obtained by X-ray phase analysis. The preset goal has been achieved comparing the quantity and intensity of reflections on X-ray diffraction patterns obtained from the prepared specimens. The test material was cast steel containing (in wt.%): 0.29%C, 1.02%Mn, 4.36%Si, 0.007%S, 0.015%P, 17.8%Cr, 29.3%Ni, 1.59%Nb and 1.19%Ti, subjected to the process of annealing at a temperature of 850°C for 100 hours. For identification of structural constituents by the technique of X-ray phase analysis, four solid specimens were prepared. Their surfaces were successively ground, polished, and subjected to electrolytic etching. The reference sample (isolate) was obtained by the method of electrolytic extraction. In solid material the following phases were identified: Fe[gamma], NbC and G; in the isolate additionally the presence of TiC, M23C6 and [sigma] was reported. It has been proved that in the case of solid specimens partial identification of phase constituents may be carried out on surfaces subjected only to grinding with 600 grit abrasive paper without the need of any further preparation.