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In-Situ Transmission Electron Microscopy of the Solid-Phase Epitaxial Growth of GaAs: Sample Preparation and Artifact Characterization

Published online by Cambridge University Press:  10 February 2011

K. B. Belay
Affiliation:
Department of Electronic Materials Engineering, Research School of Physical Sciences and Engineering, The Australian National University, Canberra, Australia.
M. C. Ridgway
Affiliation:
Department of Electronic Materials Engineering, Research School of Physical Sciences and Engineering, The Australian National University, Canberra, Australia.
D. J. Llewellyn
Affiliation:
Electron Microscopic Unit, Research School of Biological Sciences, The Australian National University, Canberra, Australia.
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Abstract

In-situ transmission electron microscopy (TEM) has been used to characterize the solidphase epitaxial growth of amorphized GaAs at a temperature of 260°C. To maximize heat transfer from the heated holder to the sample and minimize electron-irradiation induced artifacts, non-conventional methodologies were utilized for the preparation of cross-sectional samples. GaAs (3xI) mm rectangular slabs were cut then glued face-to-face to a size of (6x3) mm stack by maintaining the TEM region at the center. This stack was subsequently polished to a thickness of ~ 200 ýtm. A 3 mm disc was then cut from it using a Gatan ultrasonic cutter. The disc was polished and dimpled on both sides to a thickness of ~15 mimT.h is was ion-beam milled at liquid nitrogen temperature to an electron-transparent layer. From a comparison of in-situ and ex-situ measurements of the recrystallization rate, the actual sample temperature during in-situ characterization was estimated to deviate by ≤ 20°C from that of the heated holder. The influence of electron-irradiated was found to be negligible by comparing the recrystallization rate and microstructure of irradiated and unirradiated regions of comparable thickness. Similarly, the influence of “thin-foil effect” was found to be negligible by comparing the recrystallization rate and microstructure of thick and thin regions, the former determined after the removal of the sample from the microscope and further ion-beam milling of tens of microns of material. In conclusion, the potential influence of artifacts during in-situ TEM can be eliminated by the appropriate choice of sample preparation procedures.

Type
Research Article
Copyright
Copyright © Materials Research Society 1997

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