Hostname: page-component-cd9895bd7-dk4vv Total loading time: 0 Render date: 2024-12-27T06:27:04.300Z Has data issue: false hasContentIssue false
  • English
  • Français

XRD Measurement of Mean Thickness, Thickness Distribution and Strain for Illite and Illite-Smectite Crystallites by the Bertaut-Warren-Averbach Technique

Published online by Cambridge University Press:  28 February 2024

V. A. Drits ,
D. D. Eberl  and
J. Środoń
V. A. Drits
Affiliation:
Institute of Geology RAN, Pyzhevsky 7, 109017 Moscow, Russia
D. D. Eberl
Affiliation:
U.S. Geological Survey, 3215 Marine St., Boulder, Colorado 80303-1066
J. Środoń
Affiliation:
Institute of Geological Sciences PAN, Senacka 1, 31002 Krakow, Poland
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.

A modified version of the Bertaut-Warren-Averbach (BWA) technique (Bertaut 1949, 1950; Warren and Averbach 1950) has been developed to measure coherent scattering domain (CSD) sizes and strains in minerals by analysis of X-ray diffraction (XRD) data. This method is used to measure CSD thickness distributions for calculated and experimental XRD patterns of illites and illite-smectites (I-S). The method almost exactly recovers CSD thickness distributions for calculated illite XRD patterns. Natural I-S samples contain swelling layers that lead to nonperiodic structures in the c* direction and to XRD peaks that are broadened and made asymmetric by mixed layering. Therefore, these peaks cannot be analyzed by the BWA method. These difficulties are overcome by K-saturation and heating prior to X-ray analysis in order to form 10-Å periodic structures. BWA analysis yields the thickness distribution of mixed-layer crystals (coherently diffracting stacks of fundamental illite particles). For most I-S samples, CSD thickness distributions can be approximated by lognormal functions. Mixed-layer crystal mean thickness and expandability then can be used to calculate fundamental illite particle mean thickness. Analyses of the dehydrated, K-saturated samples indicate that basal XRD reflections are broadened by symmetrical strain that may be related to local variations in smectite interlayers caused by dehydration, and that the standard deviation of the strain increases regularly with expandability. The 001 and 002 reflections are affected only slightly by this strain and therefore are suited for CSD thickness analysis. Mean mixed-layer crystal thicknesses for dehydrated I-S measured by the BWA method are very close to those measured by an integral peak width method.

Keywords

CrystalliteFundamental Illite ParticlesIlliteMite-SmectiteMacEwan CrystallitesMixed-Layer ClayThickness DistributionsWarren-Averbach Method
Type
Research Article
Information
Clays and Clay Minerals , Volume 46 , Issue 1 , February 1998 , pp. 38 - 50
Copyright
Copyright © 1998, The Clay Minerals Society

References

Árkai, P. Merriman, R.J. Roberts, B. Peacor, D.R. and Tóth, M., 1996 Crystallinity, crystallite size and lattice strain of illite-mus-covite and chlorite: Comparison of XRD and TEM data for diagenetic to epizonal pelites Eur J Mineral 8 1119–1137 10.1127/ejm/8/5/1119.CrossRefGoogle Scholar
Bertaut, M.F., 1949 Etude aux rayons X de la répartition des dimensions des cristallites dans une poudre cristalline CR Acad Sci Paris 228 492–494.Google Scholar
Bertaut, M.E., 1950 Raies de Debye-Scherrer et répartition des dimensions des domaines de Bragg dans les poudres polycristallines Acta Crystallogr 3 14–18 10.1107/S0365110X50000045.CrossRefGoogle Scholar
Drits, V.A. Srodori, J. and Eberl, D.D., 1997 XRD measurement of mean illite crystallite thickness: Reappraisal of the Kubler index and the Scherrer equation Clays Clay Miner 45 461–475 10.1346/CCMN.1997.0450315.CrossRefGoogle Scholar
Drits, V.A. and Tchoubar, C., 1990 X-ray diffraction by disordered lamellar structures Berlin Springer-Verlag 10.1007/978-3-642-74802-8.CrossRefGoogle Scholar
Eberl, D.D. Blum, A., Reynolds, R.C. Jr and Walker, J.R., 1993 Illite crystallite thickness by X-ray diffraction CMS Workshop Lectures, Vol. 5, Computer applications to X-ray powder diffraction analysis of clay minerals Boulder, CO Clay Miner Soc. 124–153.Google Scholar
Eberl, D.D. Drits, V. Srodori, J. and Nüesch, R., 1996 MudMaster: A program for calculating crystallite size distributions and strain from the shapes of X-ray diffraction peaks USGS Open File Report 96–171 .CrossRefGoogle Scholar
Eberl, D.D. and Środoń, J., 1988 Ostwald ripening and interparticle diffraction effects for illite crystals Am Mineral 73 1335–1345.Google Scholar
Eberl, D.D. Środoń, J. Kralik, M. Taylor, B. and Peterman, Z.E., 1990 Ostwald ripening of clays and metamorphic minerals Science 248 474–477 10.1126/science.248.4954.474.CrossRefGoogle Scholar
Eberl, D.D. Środoń, J. Lee, M. Nadeau, P.H. and Northrop, H.R., 1987 Sericite from the Silverton caldera, Colorado: Correlation among structure, composition, origin, and particle thickness Amer Mineral 72 914–934.Google Scholar
Gangulee, A., 1970 Separation of the α1 - α2 doublet in X-ray diffraction profiles J Appl Cryst 3 272–277 10.1107/S0021889870006179.CrossRefGoogle Scholar
Guinier, A., 1964 Théorie et technique de la radiocristallogra-phie. Chap 13: Diffraction par les réseaux cristallins imparfaits Paris Dunod 490–636.Google Scholar
James, R.W.. 1965. The optical properties of the diffraction of X-rays. Vol. II, The crystalline state. Bragg, L., series editor. Ithaca: Cornell Univ Pr. 664 p.Google Scholar
Klug, H.P. and Alexander, L.E., 1974 X-ray diffraction procedures for polycrystalline and amorphous materials 2nd ed. New York J Wiley.Google Scholar
Kodama, H., 1965 Crystal distortion of sericite Clay Sci 2 121–131.Google Scholar
Kodama, H. Gatineau, L. and Méring, J., 1971 An analysis of X-ray diffraction line profiles of microcrystalline muscovites Clays Clay Miner 19 405–413 10.1346/CCMN.1971.0190609.CrossRefGoogle Scholar
Lanson, B. and Kubler, B., 1994 Experimental determination of the coherent scattering domain size distribution of natural mica-like phases with the Warren-Averbach technique Clays Clay Miner 42 489–494 10.1346/CCMN.1994.0420418.CrossRefGoogle Scholar
Maire, J. and Mering, J., 1960 Croissance des dimensions des domaines cristallins au cours de la graphitation du carbons New York Pergamon Pr. 345–350.Google Scholar
Moore, D.M. and Reynolds, R.C. Jr., 1989 X-ray diffraction and the identification of clay minerals New York Oxford Univ Pr..Google Scholar
Nadeau, P.H. Wilson, M.J. McHardy, W.J. and Tait, J.M., 1984 Inter-stratified clay as fundamental particles Science 225 923–935 10.1126/science.225.4665.923.CrossRefGoogle Scholar
Reynolds, R.C. Jr., 1985 NEWMODÉ, a computer program for the calculation of one-dimensional diffraction patterns of mixed-layered clays .Google Scholar
Reynolds, R.C. Jr., 1986 The Lorentz-polarization factor and preferred orientation in oriented clay aggregates Clays Clay Miner 34 359–367 10.1346/CCMN.1986.0340402.CrossRefGoogle Scholar
Reynolds, R.C. Jr., Bish, D.L. and Post, J.E., 1989 Diffraction by small and disordered crystals Modern powder diffraction Washington, DC Miner Soc Am. 145–181 10.1515/9781501509018-009.CrossRefGoogle Scholar
Siemens., 1990 Diffrac 5000 powder diffraction evaluation software reference manual, release 2.2, part no. 269-00200. Siemens Analytical Instruments, Inc., 6300 Enterprise Lane, Madison, WI 53719 .Google Scholar
Środoń, J., 1980 Precise identification of illite/smectite inter-stratifications by X-ray powder diffraction Clays Clay Miner 28 401–411 10.1346/CCMN.1980.0280601.CrossRefGoogle Scholar
Środoń, J., 1984 X-ray diffraction of illitic materials Clays Clay Miner 32 337–349 10.1346/CCMN.1984.0320501.CrossRefGoogle Scholar
Środoń, J. and Elsass, F., 1994 Effect of the shape of fundamental particles on XRD characteristics of illitic minerals Eur J Mineral 6 113–122 10.1127/ejm/6/1/0113.CrossRefGoogle Scholar
Środoń, J. Elsass, F. McHardy, W.J. and Morgan, D.J., 1992 Chemistry of illite-smectite inferred from TEM measurements of fundamental particles Clay Miner 27 137–158 10.1180/claymin.1992.027.2.01.CrossRefGoogle Scholar
Środoń, J. Morgan, D.J. Eslinger, E.V. Eberl, D.D. and Karlinger, M.R., 1986 Chemistry of illite/smectite and end-member illite Clays Clay Miner 34 368–378 10.1346/CCMN.1986.0340403.CrossRefGoogle Scholar
Stokes, A.R., 1948 A numerical Fourier-analysis method for the correction of widths and shapes of lines on X-ray diffraction photographs Proc Phys Soc (London) A61 382–391 10.1088/0959-5309/61/4/311.CrossRefGoogle Scholar
Viczián, I., 1997 Hungarian investigations on the “Zempleni” illite Clays Clay Miner 45 114–115 10.1346/CCMN.1997.0450114.CrossRefGoogle Scholar
Warren, B.E. and Averbach, B.L., 1950 The effect of cold-work distortion on X-ray patterns J Appl Phys 21 595–599 10.1063/1.1699713.CrossRefGoogle Scholar