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X-Ray Diffraction Analysis of Thin Clay Films From Dilute Suspensions Using Glancing Incidence Diffraction

Published online by Cambridge University Press:  28 February 2024

Katherine Ozalas  and
Benjamin F. Hajek
Katherine Ozalas
Affiliation:
Eagan McAllister Associates, 2050 Mabelline Rd. Suite J, North Charleston, South Carolina 29406
Benjamin F. Hajek
Affiliation:
Department of Agronomy and Soils, Auburn University, Auburn, Alabama 36849
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Abstract

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X-ray diffraction (XRD) analysis of small quantities of clay mounted on glass slides using conventional Bragg-Brentano geometry generally produces unsatisfactory low-intensity reflections masked by amorphous substrate scatter. Glancing-incidence asymmetric Bragg diffraction, an alternative uncoupled geometry, uses a fixed low-incidence angle and parallel-beam optics to increase path length through the sample and decrease X-ray penetration into the substrate. To evaluate this technique on thin soil clay films, results from conventional Bragg-Brentano and glancing-incidence diffraction (GID) were compared for progressively diluted clay suspensions separated from 2 southeastern soils with typical mineral assemblages. Patterns produced by GID showed overall higher reflection intensities and reduced substrate scatter, especially at higher 2θ angles within the amorphous glass region. Using GID, positive identification of clay minerals was obtained from sample quantities as small as 0.005 mg cm−2 and suspensions as dilute as 29 mg L−1.

Keywords

GIDThin FilmsXRD
Type
Research Article
Information
Clays and Clay Minerals , Volume 44 , Issue 6 , December 1996 , pp. 811 - 817
Copyright
Copyright © 1996, The Clay Minerals Society

References

Angui, P.. 1991. Potassium fixation and structural characterization of 2: 1 phyllosilicates in clays from representative soils of the southeastern United States [dissertation]. Auburn, AL: Auburn University. 221 p.Google Scholar
Bradley, W.E. 1964. X-ray diffraction analysis of soil clays and structure of clay minerals. In: Rich, C.I., Kunze, G.W., editors. Soil clay mineralogy. p 113–124.Google Scholar
Brindley, G.W.. 1961. Quantitative analysis of clay mixtures. In: Brown, G., editor. The X-ray identification and crystal structures of clay minerals. London: Mineralogical Society. p 489–516.Google Scholar
Brown, G. and Brindley, G.W.. 1980. X-ray diffraction procedures for clay mineral identification. In: Brown, G., Brindley, G.W., editors. Crystal structures of clay minerals and X-ray identification. London: Mineralogical Society. p 305–360.CrossRefGoogle Scholar
Carroll, D.. 1970. Clay minerals: a guide to their X-ray identification: special paper 126. Boulder, CO: The Geological Society of America. 80 p.CrossRefGoogle Scholar
Cernik, R.J., Clark, S.M. and Pattison, P.. 1990. Study of thin films and multilayers using energy-dispersive diffraction of synchrotron radiation. Adv X-ray Anal 33: 101–107.Google Scholar
Cui, S.F., Mai, Z.H., Wu, L.S., Wang, C.Y. and Dai, D.Y.. 1991. A new scheme for X-ray grazing incidence diffraction. Rev Sci Instrum 62: 2419–2423.CrossRefGoogle Scholar
Cullity, B.D.. 1967. Elements of X-ray diffraction. Reading, MA: Addison-Wesley. 514 p.Google Scholar
Drever, J.I.. 1973. The preparation of oriented clay mineral specimens for X-ray diffraction analysis by a filter-membrane peel technique. Am Mineral 58: 553–554.Google Scholar
Huang, T.C.. 1990. Surface and ultra-thin film characterization by grazing-incidence asymmetric Bragg diffraction. Adv X-ray Anal 33: 91–99.Google Scholar
Huang, T.C., Segmuller, A., Lee, W., Lee, V., Bullock, D. and Karimi, R.. 1989. X-ray diffraction analysis of high Tc superconducting thin films. Adv X-ray Anal 32: 269–277.Google Scholar
Huang, T.C. and Toney, M.F.. 1987. Analysis of cobalt-doped iron oxide thin films by synchrotron radiation. Thin Solid Films 154: 439–445.CrossRefGoogle Scholar
Inyegar, S.S., Santana, M.W., Windischmann, H. and Engler, P.. 1987. Analysis of surface layers and thin films by low incident angle X-ray diffraction. Adv X-ray Anal 30: 458–464.Google Scholar
Jackson, M.L.. 1956. Soil chemical analysis—advanced course. Madison, WI: ML Jackson, Univ of Wisconsin. 894 p.Google Scholar
Jenkins, R.. 1989. Instrumentation. In: Bish, D.L., Post, J.E., editors. Modern powder diffraction. Reviews in Mineralogy 20. Washington, DC: Mineralogical Society of America. p 19–45.CrossRefGoogle Scholar
Jenkins, R. and Squires, B.. 1982. Problems in the measurement of large d-spacings with the parafocusing diffractometer. Norelco Reporter 29: 20–25.Google Scholar
Larsen, R.A., McNulty, T.F., Goehner, R.P. and Crystal, K.R.. 1989. X-ray diffraction studies of polycrystalline thin films using glancing angle diffractometry. Adv X-ray Anal 32: 311–321.Google Scholar
Lim, G., Parrish, W. and Masciochicci, N.. 1987. Grazing incidence synchrotron X-ray diffraction method for analyzing thin films. J Mater Res 2: 471–477.CrossRefGoogle Scholar
Marra, W.C., Eisenberger, P. and Cho, A.Y.. 1979. X-ray total external reflection—Bragg diffraction: A structural study of the GaAs-Al interface. J Appl Phys 50: 6927–6933.CrossRefGoogle Scholar
Moore, D.M. and Reynolds, R.C.. 1989. X-ray diffraction and the identification and analysis of clay minerals. New York: Oxford Univ Pr. 332 p.Google Scholar
Parrish, W. and Hart, M.. 1990. Parallel beam and focusing X-ray powder diffractometry. Adv X-ray Anal 32: 481–488.Google Scholar
Pietsch, U., Metzger, H., Rugel, S., Jenichen, B. and Robinson, I.K.. 1993. Depth-resolved measurement of lattice relaxation in Ga1-xAs/GaAs strained layer superlattices by means of grazing-incidence X-ray diffraction. J Appl Phys 74: 2381–2387.CrossRefGoogle Scholar
Reynolds, R.C.. 1980. Interstratified clay minerals. In: Brown, G., Brindley, G.W., editors. Crystal structures of clay minerals and their X-ray identification. Monograph No. 5. London: Mineralogical Society. p 249–303.CrossRefGoogle Scholar
Rhan, H., Pietsch, U., Rugel, S., Metzger, H. and Peisl, J.. 1993. Investigations of semiconductor superlattices by depth-sensitive X-ray methods. J Appl Phys 74: 146–152.CrossRefGoogle Scholar
Rich, C.I.. 1975. Amount of clay needed for optimum X-ray diffraction analysis. Soil Sci Soc Am Proc 39: 161–162.CrossRefGoogle Scholar
Szpunar, J.A., Ahlroos, S. and Tavernier, P.h.. 1993. Method of measurement and analysis of texture in thin films. J Mater Sci 28: 2366–2376.CrossRefGoogle Scholar
Toney, M.F. and Brennan, S.. 1989. Structural depth profiling of iron oxide thin films using grazing incidence asymmetric Bragg X-ray diffraction. J Appl Phys 65: 4763–4768.CrossRefGoogle Scholar