Hostname: page-component-78c5997874-m6dg7 Total loading time: 0 Render date: 2024-11-04T21:21:54.314Z Has data issue: false hasContentIssue false

In Situ Recrystallization Imaging of Polycrystalline Ni-S Alloy by SEM

Published online by Cambridge University Press:  26 February 2011

Marilyne Cornen
Affiliation:
[email protected], Polytech'Nantes, LGMPA, rue Christian Pauc, Nantes Cedex03, N/A, 44306, France, +33 2 40 68 31 61, +33 2 40 68 31 99
René Le Gall
Affiliation:
Get access

Abstract

Impurity segregation at alloy grain boundaries (GB) depends on many parameters such as GB character and prior thermomechanical history. In this paper we describe an experimental set-up designed to record the individual behaviour of GB during recrystallization of a Nickel-Sulphur alloy. The aim is to correlate segregation level with mobility and disorientation of GB. Therefore a method allowing direct observation of the GB motion as well as disorientation mapping is needed.

Studying grain growth and recrystallization of this particular alloy by Scanning Electron Microscopy is possible thanks to real time in-situ imaging. This requires a sensitive crystal orientation contrast and the ability to image hot evolving samples. To heat the samples, a special device designed for the SEM analysis chamber is used. This device is used at 455°C but is able to reach higher temperatures. In order to get the orientation contrast images, as well as to protect the Secondary Electron (SE) detector from heat and light, a channel plate converter has been designed. This experimental set-up, combined with the heating system, allow the observation of the sample during recrystallization and recording small videos providing information such as grain boundary displacement rate. Then, associated with an EBSD analysis we can get the disorientation map of the area of interest and eventually an electrochemical technique is performed to create preferential dissolution at GB. Geometry of the grooves resulting from an electrochemical etching gives an evaluation of the segregation level in GB.

Type
Research Article
Copyright
Copyright © Materials Research Society 2006

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

[1] Lejček, P., Hofmann, S. and Paidar, V., Acta Mat. Vol. 51 (2003), p. 3951.Google Scholar
[2] Le Gall, R., Liao, G. and Saindrenan, G., Scripta Mater. Vol. 41 (1999) p. 427.Google Scholar
[3] Reimer, L., Volbert, B., Electron Microscopy and Analysis, 1979, 1980, p 8992.Google Scholar
[4] Kim, W.S. and authors, co, Applied Physics Letters -Vol. 81 (2002), Issue 6, pp. 10981100.Google Scholar
[5] Cahn, J.W., Acta Metall. Vol. 10 (1962) p. 789 Google Scholar
[6] Beaunier, L., Froment, M. and Vignaud, C., Electrochem. Acta Vol 25 (1980), p. 123 Google Scholar
[7] Quérard, E., Saindrenan, G., Mourton, H. and Roptin, D. Scripta Mat. Vol. 35 (1996) p. 1175.Google Scholar