Hostname: page-component-586b7cd67f-dsjbd Total loading time: 0 Render date: 2024-11-28T02:29:55.071Z Has data issue: false hasContentIssue false
  • English
  • Français

Thickness Distribution of Illite Crystals in Shales. I: X-Ray Diffraction vs. High-Resolution Transmission Electron Microscopy Measurements

Published online by Cambridge University Press:  01 January 2024

Teresa Dudek ,
Jan Środoń ,
Dennis D. Eberl ,
Françoise Elsass  and
Peter Uhlik
Teresa Dudek*
Affiliation:
Institute of Geological Sciences, Polish Academy of Sciences, Senacka 1, 31-002 Kraków, Poland
Jan Środoń
Affiliation:
Institute of Geological Sciences, Polish Academy of Sciences, Senacka 1, 31-002 Kraków, Poland
Dennis D. Eberl
Affiliation:
US Geological Survey, Suite E-127, 3215 Marine St., Boulder, Colorado 80303-1066, USA
Françoise Elsass
Affiliation:
Science du Sol INRA, Versailles, France
Peter Uhlik
Affiliation:
Department of Mineral Deposits, Comenius University, Bratislava, Slovakia
*
*E-mail address of corresponding author: [email protected]
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.

Two independent methods of crystal-size distribution analysis were compared: the Bertaut-Warren-Averbach XRD technique (MudMaster computer program) and high-resolution transmission electron microscopy (HRTEM). These techniques were used to measure thickness distributions of illite crystals (fundamental particles) from sets of illite-smectites from shales and bentonites that had expandabilities ranging from 86%S to 6%S. The illite-smectites were treated with a polymer (polyvinylopyrolidone, PVP) to separate them into fundamental particles for XRD and HRTEM investigations.

A systematic difference between XRD and HRTEM results was observed: XRD (area-weighted distributions) detected a larger fraction of thick (>4 nm) and a smaller fraction of thin crystals as compared to HRTEM (number-weighted distributions). As a result, XRD-determined distributions have larger mean thickness values and larger distribution parameters (α and β2). The measurements performed by the two techniques were verified by modeling XRD patterns of the PVP-illites, using the measured distributions as inputs. The modeling indicated that the XRD-determined distributions are very accurate. Selecting broader thickness distributions in MudMaster further improved the modeling results. The HRTEM measurements underestimate the proportion of coarse particles, in particular in shale samples, and this inaccuracy is attributed to the effect of using number-weighted (rather than area-weighted) distributions and to inaccurate counting statistics for thick crystals.

Keywords

BWA AnalysisCrystal Size DistributionFundamental ParticlesHRTEMIllite-smectiteLognormal DistributionMudMasterXRD
Type
Research Article
Information
Clays and Clay Minerals , Volume 50 , Issue 5 , October 2002 , pp. 562 - 577
Copyright
Copyright © 2002, 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-muscovite and chlorite: comparison of XRD and TEM data for diagenetic to epizonal pelites European Journal of Mineralogy 8 1119–1138 10.1127/ejm/8/5/1119.CrossRefGoogle Scholar
Drits, V. Środoń, J. and Eberl, D.D., (1997) XRD measurement of mean crystallite thickness of illite and illite/smectite: reappraisal of the Kübler index and the Scherrer equation Clays and Clay Minerals 45 461–475 10.1346/CCMN.1997.0450315.CrossRefGoogle Scholar
Drits, V. Eberl, D.D. and Środoń, J., (1998) XRD measurement of mean thickness, thickness distribution and strain for illite and illite-smectite crystallites by the Bertaut-Warren-Averbach technique Clays and Clay Minerals 46 38–50 10.1346/CCMN.1998.0460105.Google Scholar
Dudek, T. (2001) Diagenetic evolution of illite-smectite in the Miocene shales from the Przemyśl area (Carpathian Foredeep). PhD thesis, Institute of Geological Sciences, Polish Academy of Sciences, 155 pp.Google 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 American Mineralogist 72 914 934.Google Scholar
Eberl, D.D., Drits, V.A., Środoń, J. and Nuesch, R. (1996) MUDMASTER: A program for calculating crystallite size distributions and strain from the shapes of X-ray diffraction peaks. U.S. Geological Survey, Open-File Report 96–171.Google Scholar
Eberl, D.D. Drits, V. and Środoń, J., (1998) Deducing growth mechanisms for minerals from the shapes of crystal size distributions American Journal of Science 298 499–533 10.2475/ajs.298.6.499.Google Scholar
Eberl, D.D. Nuesch, R. Šucha, V. and Tsipursky, S., (1998) Measurement of fundamental illite particle thicknesses by X-ray diffraction using PVP-10 intercalation Clays and Clay Minerals 46 89–97 10.1346/CCMN.1998.0460110.CrossRefGoogle Scholar
Elsass, F. Beaumont, A. Pernes, M. Jaunet, A.-M. and Tessier, D., (1998) Changes in layer organization of Na-and Ca- exchanged smectite materials during solvent exchanges for embedment in res in The Canadian Mineralogist 36 1475 1483.Google Scholar
Jackson, M.L. (1975) Soil Chemical Analysis — Advanced Course (Jackson, M. editor). University of Wisconsin, Madison, USA.Google Scholar
Kile, D.E. Eberl, D.D. Hoch, A.R. and Reddy, M.M., (2000) An assessment of calcite crystal growth mechanism based on crystal size distributions Geochimica et Cosmochimica Acta 64 2937–2950 10.1016/S0016-7037(00)00394-X.Google Scholar
Lanson, B. and Kübler, B., (1994) Experimental determination of coherent scattering domain size distribution of natural mica-like phases with the Warren-Averbach technique Clays and Clay Minerals 42 489–494 10.1346/CCMN.1994.0420418.Google Scholar
Merriman, R.J. Roberts, B. and Peacor, D.R., (1990) A transmission electron microscope study of white mica crystallite size distribution in a mudstone to slate transitional sequence, North Wales, UK Contributions to Mineralogy and Petrology 106 27–40 10.1007/BF00306406.Google Scholar
Moore, D.M. and Reynolds, R.C. Jr, (1997) X-ray Diffraction and the Identification and Analysis of Clay Minerals New York Oxford University Press.Google Scholar
Nadeau, P.H. Tait, J.M. McHardy, W.J. and Wilson, M.J., (1984) Interstratified XRD characteristics of physical mixtures of elementary clay particles Clay Minerals 19 67–76 10.1180/claymin.1984.019.1.07.Google Scholar
Nieto, F. and Sanchez-Navas, A., (1994) A comparative XRD and TEM study of the physical meaning of the white mica ‘crystallinity’ index European Journal of Mineralogy 6 611–622 10.1127/ejm/6/5/0611.Google Scholar
Reynolds, R.C. Jr, Brindley, G.W. and Brown, G., (1980) Interstratified clay minerals Crystal Structures of Clay Minerals and their X-ray Identification London Mineralogical Society 249 304.Google Scholar
Reynolds, R.C. Jr, (1985) NEWMOD © a computer program for the calculation of one-dimensional diffraction patterns of mixed-layered clays 8 Brook Dr., Hanover, New Hampshire, USA R.C. Reynolds.Google Scholar
Spurr, A.R., (1969) A low viscosity epoxy resin embedding medium for electron microscopy Journal of Ultrastructural Research 26 31–43 10.1016/S0022-5320(69)90033-1.Google Scholar
Środoń, J., (1984) X-ray powder diffraction identification of illitic materials Clays and Clay Minerals 32 337–349 10.1346/CCMN.1984.0320501.Google 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 and Clay Minerals 34 368–378 10.1346/CCMN.1986.0340403.Google Scholar
Środoń, J. Andreoli, C. Elsass, F. and Robert, M., (1990) Direct high-resolution transmission electron microscopic measurements of expandability of mixed-layer illite/smectite in bentonite rock Clays and Clay Minerals 38 373–379 10.1346/CCMN.1990.0380406.Google Scholar
Środoń, J. Eberl, D.D. and Drits, V., (2000) Evolution of fundamental particle size during illitization of smectite and implications for the illitization mechanism Clays and Clay Minerals 48 446–459 10.1346/CCMN.2000.0480405.Google Scholar
Tessier, D. (1984) Etude experimentale de l’organisation des materiaux argileux. Dr Science thesis, University of Paris VII, Paris, INRA publisher, pp. 125–130.Google Scholar
Uhlik, P. (1999) Evolution of illite-smectite particles during diagenesis. PhD thesis, Comenius University, 101 pp. (in Slovak).Google Scholar
Uhlik, P. Šucha, V. Eberl, D.D. Puskelova, L. and Čaplovičova, M., (2000) Evolution of pyrophyllite particle sizes during dry grinding Clay Minerals 35 423–432 10.1180/000985500546774.Google Scholar
Uhlik, P. Šucha, V. Elsass, F. and Čaplovičova, M., (2000) High-resolution transmission electron microscopy of mixed-layer clays dispersed in PVP-10: A new technique to distinguish detrital and authigenic illitic material Clay Minerals 35 781–789 10.1180/000985500547232.Google Scholar
Vali, H. and Köster, H.M., (1986) Expanding behaviour, structural disorder, regular and random irregular interstratification of 2:1 layer-silicates studied by high-resolution images of transmission electron microscopy Clay Minerals 21 827–859 10.1180/claymin.1986.021.5.01.Google Scholar
Warr, L.N. and Nieto, F., (1998) Crystallite thickness and defect density of phyllosilicates in low-temperature metamorphic pelites: a TEM and XRD study of clay mineral crystallinity index standards The Canadian Mineralogist 36 1453 1474.Google Scholar