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Nanoengineered Glancing Angle Deposition Thin Films for Ultrathin-Layer Chromatography Open Access


Other title
concentration zone
time-resolved ultrathin-layer chromatography
atomic layer deposition
stationary phase
macroporous thin film
planar chromatography
glancing angle deposition
reactive ion etch
thin-layer chromatography
ultrathin-layer chromatography
nanostructured thin film
columnar thin film
Type of item
Degree grantor
University of Alberta
Author or creator
Jim, Steven R.
Supervisor and department
Brett, Michael (Electrical and Computer Engineering)
Examining committee member and department
Poole, Colin (Chemistry, Wayne State University, Detroit, MI, USA)
Thundat, Thomas (Chemical and Materials Engineering)
Cadien, Kenneth (Chemical and Materials Engineering)
Zemp, Roger (Electrical and Computer Engineering)
Brett, Michael (Electrical and Computer Engineering)
Department of Electrical and Computer Engineering
Microsystems and Nanodevices
Date accepted
Graduation date
Doctor of Philosophy
Degree level
Analytical separations are important methods of identifying and quantifying molecular compounds present in complex sample mixtures. These approaches are popular in biochemistry, medical diagnostics, quality control, and numerous other applications. In these techniques, constituent analytes are separated according to their characteristic physical and chemical properties. Planar chromatography analytical separations leverage the effects of these properties on competing interactions between the compounds, moving liquids, and stationary flat porous solids. Engineered solid-liquid interfaces can improve performance since these interactions occur at the nanoscale. Ultrathin-layer chromatography (UTLC) is a miniature form of planar chromatography in which sample analytes are carried by solvents that wick through < 10 um thick solids with extraordinarily fine pores. The technique achieves fast separations (minutes) over short distances (millimetres to centimetres) with high sensitivity. The strong dependence of UTLC performance on layer microstructure motivates pursuit of new chromatographic media. This dissertation studies UTLC layers produced using glancing angle deposition (GLAD). GLAD is an excellent platform for engineering nanostructured thin films of varied material, porosity, and architecture. It can achieve ~ 5 um thick columnar morphologies well-suited for UTLC that are unattainable or impractical using other techniques. Unique anisotropic media exhibited channel features that strongly influenced analyte migration direction and velocity. Further control of chromatographic behaviours was achieved using post-deposition enhancements. Fluorocarbon reactive ion etching (RIE) selectively modifies film microstructure, increases porosity, and decreases the surface area over which analytes may interact. Atomic layer deposition (ALD) applies extremely thin < 10 nm conformal coatings that produce alternative chromatographic surface chemistries over GLAD UTLC film scaffolds. These investigations required invention of new instrumentation and analysis techniques since conventional planar chromatography equipment is unoptimized for miniaturized GLAD UTLC plates. Approaches to fabricating, utilizing, characterizing, and enhancing nanoengineered GLAD UTLC media are considered in this thesis. The intriguing behaviours described within provide insight into the manner in which the microscopic features of GLAD films impact macroscopic development phenomena. These investigations simultaneously advanced both the capabilities of the UTLC planar chromatography technique and the understanding of GLAD nanostructured thin film materials.
Permission is hereby granted to the University of Alberta Libraries to reproduce single copies of this thesis and to lend or sell such copies for private, scholarly or scientific research purposes only. Where the thesis is converted to, or otherwise made available in digital form, the University of Alberta will advise potential users of the thesis of these terms. The author reserves all other publication and other rights in association with the copyright in the thesis and, except as herein before provided, neither the thesis nor any substantial portion thereof may be printed or otherwise reproduced in any material form whatsoever without the author's prior written permission.
Citation for previous publication
S.R. Jim, M.T. Taschuk, G.E. Morlock, L.W. Bezuidenhout, W. Schwack, M.J. Brett, Engineered anisotropic microstructures for ultrathin-layer chromatography, Analytical Chemistry. 82 (2010) 5349–5356.
. Oko, S.R. Jim, M.T. Taschuk, M.J. Brett, Analyte migration in anisotropic nanostructured ultrathin-layer chromatography media, Journal of Chromatography A. 1218 (2011) 2661–2667.
. Jim, A.J. Oko, M.T. Taschuk, M.J. Brett, Morphological modification of nanostructured ultrathin-layer chromatography stationary phases, Journal of Chromatography A. 1218 (2011) 7203–7210.
. Oko, S.R. Jim, M.T. Taschuk, M.J. Brett, Time resolved chromatograms in ultra-thin layer chromatography, Journal of Chromatography A. 1249 (2012) 226–232.
. Jim, A. Foroughi-Abari, K.M. Krause, P. Li, M.R. Kupsta, M.T. Taschuk, K.C. Cadien, M.J. Brett, Ultrathin-layer chromatography nanostructures modified by atomic layer deposition, Journal of Chromatography A. 1299 (2013) 118–125.
. Wannenmacher, S.R. Jim, M.T. Taschuk, M.J. Brett, G.E. Morlock, Ultrathin-layer chromatography on SiO2, Al2O3, TiO2, and ZrO2 nanostructured thin films, Journal of Chromatography A. 1318 (2013) 234–243.

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