Hostname: page-component-745bb68f8f-b95js Total loading time: 0 Render date: 2025-01-27T16:19:41.974Z Has data issue: false hasContentIssue false
  • English
  • Français

An In situ Time-Resolved XRD-PSD Investigation into Na-Montmorillonite Interlayer and Particle Rearrangement during Dehydration

Published online by Cambridge University Press:  01 January 2024

James Wilson ,
Javier Cuadros  and
Gordon Cressey
James Wilson
Affiliation:
Department of Earth Sciences, University of Bristol, Wills Memorial Building, Queen’s Road, Bristol BS8 1RJ, UK
Javier Cuadros*
Affiliation:
Department of Mineralogy, The Natural History Museum, Cromwell Road, London SW7 5BD, UK
Gordon Cressey
Affiliation:
Department of Mineralogy, The Natural History Museum, Cromwell Road, London SW7 5BD, UK
*
*E-mail address of corresponding author: j.cuadros@nhm.ac.uk
Rights & Permissions [Opens in a new window]

Abstract

Core share and HTML view are not available for this content. However, as you have access to this content, a full PDF is available via the ‘Save PDF’ action button.

X-ray diffraction with a position-sensitive detector (XRD-PSD) was used to make a time-resolved study of the dynamics of deposition and dehydration of Na-montmorillonite crystallites on flat substrates from deionized water suspensions. The static PSD geometry and simultaneous counting procedure allowed the acquisition of high-resolution data on the dynamics of interlayer and interparticle arrangements during dehydration. Three experimental datasets of Na-smectite dehydration are presented, each one representing different initial sample states (suspension, slurry and re-wetted thin film). The computer program NEWMOD was used to simulate one of the three datasets (dehydration of a smectite suspension) and thus obtain the apparent changes in relative proportions of different 00l values as smectite crystallites formed and dehydrated. Two types of diffracting domains formed: water-dispersed ‘packets’ of 1–2 smectite layers gaining long-range order in the c axis direction as water was lost to evaporation, and smectite layers deposited as hydrated crystallites with variable interlayer water contents. The experimental patterns show the rapid step-wise transition of Na-montmorillonite layers from d values of ∼55 to 18.5, 15.4 and 12.5 Å, with variations that depended upon how the hydrated smectite sample was prepared. The simulations show that there was a wide range of d values whose frequency distribution changed as dehydration proceeded and that transient d values occurred between the peaks observed experimentally. The data obtained in this study illustrate that XRD-PSD instruments have great potential in providing detailed data on the rapid kinetics of interlayer reorganization.

Keywords

DehydrationPosition-sensitive DetectorSmectiteX-ray Diffraction
Type
Research Article
Information
Clays and Clay Minerals , Volume 52 , Issue 2 , April 2004 , pp. 180 - 191
Copyright
Copyright © 2004, The Clay Minerals Society

References

Batchelder, M. and Cressey, G., (1998) Rapid, accurate phase quantification of clay-bearing samples using a position-sensitive X-ray detector Clays and Clay Minerals 46 183–194 10.1346/CCMN.1998.0460209.CrossRefGoogle Scholar
Bergaya, F. and Vayer, M., (1997) CEC of clays: measurement by adsorption of a copper ethylenediamine complex Applied Clay Science 12 275–280 10.1016/S0169-1317(97)00012-4.CrossRefGoogle Scholar
Blanton, T.N. Huang, T.C. Toraya, H. Hubbard, C.R. Robie, S.B. Louër, D. Göbel, H.E. Will, G. Gilles, R. and Raferty, T., (1995) JCPDS — International Centre for Diffraction Data round robin study of silver behenate. A possible low-angle X-ray diffraction calibration standard Powder Diffraction 10 91–95 10.1017/S0885715600014421.CrossRefGoogle Scholar
Boek, E.S. Coveney, P.V. and Skipper, N.T., (1995) Monte Carlo molecular modeling studies of hydrated Li-, Na-, and K-smectites: Understanding the role of potassium as a clay swelling inhibitor Journal of the American Chemical Society 117 12608–12617 10.1021/ja00155a025.CrossRefGoogle Scholar
Boek, E.S. Coveney, P.V. and Skipper, N.T., (1995) Molecular modeling of clay hydration: A study of hysteresis loops in the swelling curves of sodium montmorillonites Langmuir 11 4629–4631 10.1021/la00012a008.CrossRefGoogle Scholar
Bradley, W.F. Grim, R.E. and Clark, G.L., (1937) A study of the behaviour of montmorillonite upon wetting Zeitschrift Kristallographie A97 216–222.Google Scholar
Brindley, G.W., Brindley, G.W. and Brown, G., (1980) Quantitative X-ray mineral analysis of clays Crystal Structures of Clay Minerals and their X-ray Identification London Mineralogical Society 411–438.CrossRefGoogle Scholar
Cases, J. Bérend, I. Besson, G. François, M. Uriot, J.P. Thomas, F. and Poirier, J.E., (1992) Mechanism of adsorption and desorption of water vapor by homionic montmorillonite. 1. The sodium-exchanged form Langmuir 8 2730–2739 10.1021/la00047a025.CrossRefGoogle Scholar
Chang, F-RC Skipper, N.T. and Sposito, G., (1995) Computer simulation of interlayer molecular structure in sodium montmorillonite hydrates Langmuir 11 2734–2741 10.1021/la00007a064.CrossRefGoogle Scholar
Chatterjee, A. Iwasaki, T. Ebina, T. and Miyamoto, A., (1999) A DTF study on clay-cation-water interaction in montmorillonite and beidellite Computational Materials Science 14 119–124 10.1016/S0927-0256(98)00083-4.CrossRefGoogle Scholar
Collins, D.R. Fitch, A.N. and Catlow, R.A., (1992) Dehydration of vermiculites and montmorillonites: A time-resolved powder neutron diffraction study Journal of Materials Chemistry 2 865–873 10.1039/jm9920200865.CrossRefGoogle Scholar
da Silva, G., Fossum, J., DiMasi, E., Måløy, K. and Lutnæs, S. (2002) Synchrotron X-ray scattering studies of water intercalation in a layered synthetic silicate. Physical Review E, 66, 011303-1–011303-8.CrossRefGoogle Scholar
DiMasi, E., Fossum, J., Gog, T. and Venkataraman, C. (2001) Orientational order in gravity dispersed clay colloids: A synchrotron X-ray scattering study of Na fluorohectorite suspension. Physical Review E, 64, 061704-1–061704-7.CrossRefGoogle Scholar
Glaeser, R. and Méring, J., (1968) Homogeneous hydration domains of the smectites Comptes Rendus de Seances de l’academie des sciences, Paris 267 436–466.Google Scholar
Howard, S.A. Preston, K.D., Bish, D.L. and Post, J.E., (1989) Profile fitting of powder diffraction patterns Modern Powder Diffraction Washington, D.C Mineralogical Society of America 217–276 10.1515/9781501509018-011.CrossRefGoogle Scholar
Karaborni, S. Smit, B. Heidug, W. Urai, J. and van Oort, E., (1996) The swelling of clays: molecular simulations of the hydration of montmorillonite Science 271 1102–1104 10.1126/science.271.5252.1102.CrossRefGoogle Scholar
Kawamura, K. Ichikawa, Y. Nakano, M. Kitiyama, K. and Kawamura, H., (1999) Swelling properties of smectite up to 90°C. In-situ X-ray diffraction experiments and molecular dynamic simulations Engineering Geology 54 75–79 10.1016/S0013-7952(99)00063-0.CrossRefGoogle Scholar
Keren, R. and Shainberg, I., (1975) Water vapor isotherms and heat of immersion of Na/Ca montmorillonite systems — 1: homoionic clay Clays and Clay Minerals 23 193–200 10.1346/CCMN.1975.0230305.CrossRefGoogle Scholar
MacEwan, D.M.C. Wilson, M.J., Brindley, G.W. and Brown, G., (1980) Interlayer and intercalation complexes of clay minerals Crystal Structures of Clay Minerals and their X-ray Identification London Mineralogical Society 197–248.CrossRefGoogle Scholar
Moore, D.M. and Hower, J., (1986) Ordered interstratification of dehydrated and hydrated smectite Clays and Clay Minerals 34 379–384 10.1346/CCMN.1986.0340404.CrossRefGoogle Scholar
Moore, D.M. and Reynolds, R.C., (1997) X-ray Diffraction and the Identification and Analysis of Clay Minerals Oxford, UK Oxford University Press.Google Scholar
Reynolds, R.C. Jr. and Reynolds, R.C. III (1996) NEWMOD: The Calculation of One-Dimensional X-ray Diffraction Patterns of Mixed-Layered Clay Minerals. Computer Program. 8 Brook Road, Hanover, New Hampshire, USA.Google Scholar
Skipper, N.T. Refson, K. and McConnell, J.D.C., (1991) Computer simulation of interlayer water in 2: 1 clays Journal of Chemical Physics 94 7434–7445 10.1063/1.460175.CrossRefGoogle Scholar
Skipper, N. Chang, F.-R. and Sposito, G., (1995) Monte Carlo simulation of interlayer molecule structure in swelling clay minerals. 1. Methodology Clays and Clay Minerals 43 285–293 10.1346/CCMN.1995.0430303.CrossRefGoogle Scholar
Sposito, G. Park, S.-H. and Sutton, R., (1999) Monte Carlo simulation of the total radial distribution function for interlayer water in sodium and potassium montmorillonites Clays and Clay Minerals 47 192–200 10.1346/CCMN.1999.0470209.CrossRefGoogle Scholar
Yamada, H. Nakazawa, H. Hashizume, H. Shimomura, S. and Watanabe, T., (1994) Hydration behavior of Na-smectite crystals synthesized at high-pressure and high-temperature Clays and Clay Minerals 42 77–80 10.1346/CCMN.1994.0420110.CrossRefGoogle Scholar