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Methods for Performing Atomic Force Microscopy Imaging of Clay Minerals in Aqueous Solutions

Published online by Cambridge University Press:  28 February 2024

Barry R. Bickmore ,
Michael F. Hochella Jr. ,
Dirk Bosbach  and
Laurent Charlet
Barry R. Bickmore
Affiliation:
Department of Geological Sciences, 4044 Derring Hall, Virginia Polytechnic Institute and State University, Blacksburg, Virginia 24061 USA
Michael F. Hochella Jr.
Affiliation:
Department of Geological Sciences, 4044 Derring Hall, Virginia Polytechnic Institute and State University, Blacksburg, Virginia 24061 USA
Dirk Bosbach
Affiliation:
Institut für Mineralogie, Universität Münster, Corrensstr. 24, 48149 Münster, Germany
Laurent Charlet
Affiliation:
Environmental Geochemistry Group, L.G.I.T., B.P. 53, F-38041 Grenoble Cedex 9, France
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Abstract

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Three methods were developed that allow for the imaging of any clay mineral in aqueous solutions with atomic force microscopy (AFM). The methods involve fixing the particles onto special substrates that do not complicate the imaging process, but hold the particles sufficiently so that they do not move laterally or float away during imaging. Two techniques depend on electrostatic attraction under circumneutral pH conditions, between the negatively charged clay particles and the high point of zero charge substrate (either aluminum oxide or polyethyleneimine-coated mica) whereas the third technique depends on adhesion to a thermoplastic film. The first electrostatic technique involves a polished single crystal α-Al2O3 (sapphire) substrate. This was used successfully as a substrate for clay-sized minerals with high permanent layer charge localized on the basal planes (phlogopite and vermiculite) and when the AFM was operated in TappingMode to limit the lateral forces between the probe tip and the particles. However, electrostatic attraction between the sapphire surface and clay minerals such as smectite and kaolinite (low or no permanent layer charge) is not sufficiently strong to adequately fix the particles for imaging. The second electrostatic technique involves a polyethyleneimine-coated mica surface designed to immobilize a larger variety of clay minerals (phlogopite, vermiculite, montmorillonite, and kaolinite), and in this technique weak bonding between the clay and the organic film is also a factor. The third technique, which does not depend on electrostatic attraction, fixes clay particles into the surface of a thermoplastic adhesive called Tempfix. This has proven useful for fixing and imaging relatively large clay particles with well-defined morphology. The Tempfix mount also requires imaging in TappingMode because the Tempfix is relatively soft.

Keywords

Atomic Force MicroscopyCMS Source Clay KGa-1CMS Source Clay SWy-1Fluid CellParticlesPolyethyleneimineSapphireTappingModeTempfix
Type
Research Article
Information
Clays and Clay Minerals , Volume 47 , Issue 5 , October 1999 , pp. 573 - 581
Copyright
Copyright © 1999, The Clay Minerals Society

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