Hostname: page-component-cd9895bd7-mkpzs Total loading time: 0 Render date: 2024-12-28T16:08:16.808Z Has data issue: false hasContentIssue false
  • English
  • Français

Solid State NMR Characterization of the Thermal Transformation of an Illite-Rich Clay

Published online by Cambridge University Press:  28 February 2024

G. E. Roch ,
M. E. Smith  and
S. R. Drachman
G. E. Roch
Affiliation:
School of Physical Sciences, University of Kent, Canterbury, Kent, CT2 7NR, United Kingdom
M. E. Smith*
Affiliation:
School of Physical Sciences, University of Kent, Canterbury, Kent, CT2 7NR, United Kingdom
S. R. Drachman
Affiliation:
RBB Research and Development, Graylands, Langhurstwood Road, Horsham, West Sussex, RH12 4QG, United Kingdom
*
†Present address and correspondence to: M. E. Smith, Department of Physics, University of Warwick, Coventry, CV4 7A1, United Kingdom.
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.

Lode, a dioctahedral illite-rich clay from Latvia belonging to the mica group of clay minerals, undergoes thermal transformation via a series of structurally disordered intermediate phases. Despite containing high levels of paramagnetic Fe substituted into the octahedral sites, 29Si and 27Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectra of sufficient quality are obtained to resolve different structural units, showing clearly defined structural changes which occur in the sample during calcination to 1200 °C. However, Fe plays a significant role in broadening the Al signal, with integrated peak intensities decreasing as temperature increases. Significant differences are revealed in the thermal decomposition process by NMR spectra between pyrophyllite, Ca-montmorillonite and illite clays, possibly due to the different cations present in the interlayer. It has also been shown for illite that no structural differences at the atomic level occur when the dwell time at a particular temperature is varied and no difference is observed between samples that have different thermal histories; however, a minor effect of particle size and surface area is visible in the NMR data.

Keywords

IlliteIronParamagnetic CenterSolid-State NMRThermal Transformation
Type
Research Article
Information
Clays and Clay Minerals , Volume 46 , Issue 6 , December 1998 , pp. 694 - 704
Copyright
Copyright © 1998, The Clay Minerals Society

References

Brown, I.W.M. MacKenzie, K.J.D. and Meinhold, R.H., 1987 The thermal reactions of montmorillonite studied by high resolution solid state Si-29 and Al-27 NMR J Mater Sci 22 3265–3275 10.1007/BF01161191.CrossRefGoogle Scholar
Deer, W.A. Howie, R.A. and Zussman, J., 1992 An introduction to the rock-forming minerals Hong Kong Longman.Google Scholar
Drachman, S.R. Roch, G.E. and Smith, M.E., 1997 Solid state NMR characterisation of the thermal transformation of fuller’s earth Solid State NMR 9 257–267 10.1016/S0926-2040(97)00069-6.CrossRefGoogle ScholarPubMed
Drits, V.A. Besson, G. and Muller, F., 1995 An improved model for structural transformations of heat-treated aluminous dioc-tahedral 2:1 layer silicates Clays Clay Miner 43 718–731 10.1346/CCMN.1995.0430608.CrossRefGoogle Scholar
Earley, J.W. Milne, I.H. and McVeagh, W.J., 1953 Thermal dehydration and X-ray studies on montmorillonite Am Mineral 38 770–783.Google Scholar
Earnest, C.M., 1991 Thermal analysis of selected illite and smectite clay minerals part 1: Mite clay specimens Lecture notes in earth sciences Berlin Springer-Verlag 270–286.Google Scholar
Engelhardt, G. and Michel, D., 1987 General aspects of Si-29 and Al-27 NMR of the silicate and aluminosilicate framework High resolution solid-state NMR of silicates and zeolites New York J. Wiley 106–155.Google Scholar
Fitzgerald, J.J. and Hamza, A.I., 1996 Solid-state 27-Al and 29-Si NMR and 1-H CRAMPS studies of the thermal transformation of the 2:1 phyllosilicate pyrophyllite J Phys Chem 100 17351–17360 10.1021/jp961499f.CrossRefGoogle Scholar
Greene-Kelly, R., 1955 Dehydration of the montmorillonite minerals Mineral Mag 30 604–615.Google Scholar
Grim, R.E. and Bradley, W.F., 1940 Investigation of the effect of heat on the clay minerals illite and montmorillonite I Am Ceram Soc 22 242–248 10.1111/j.1151-2916.1940.tb14263.x.CrossRefGoogle Scholar
Malathi, N. Puri, S.P. and Saraswat, I.P., 1971 Mossbauer studies of iron in illite and montmorillonite. II. Thermal treatment J Phys Soc Jpn 31 117–122 10.1143/JPSJ.31.117.CrossRefGoogle Scholar
Massiot, D. Dion, P. Alcover, J. and Bergaya, E., 1995 Al-27 and Si-29 MAS NMR study of kaolinite thermal decomposition by controlled rate thermal analysis J Am Ceram Soc 78 2940–2944 10.1111/j.1151-2916.1995.tb09067.x.CrossRefGoogle Scholar
Michael, P.J. and McWhinnie, W.R., 1989 Mossbauer and ESR studies of the thermochemistry of illite and montmorillonite Polyhedron 8 2709–2718 10.1016/S0277-5387(00)80443-X.CrossRefGoogle Scholar
Morris, H.D. Bank, S. and Ellis, P.D., 1990 Al-27 spectroscopy of iron-bearing montmorillonite clays J Phys Chem 94 3121–3129 10.1021/j100370a069.CrossRefGoogle Scholar
Murad, E. and Wagner, U., 1996 The thermal behaviour of an Fe-rich illite Clay Miner 31 45–52 10.1180/claymin.1996.031.1.04.CrossRefGoogle Scholar
Ogloza, A.A. and Malhotra, V.M., 1989 Dehydroxylation induced structural transformations in montmorillonite: An isothermal FTIR study Phys Chem Miner 378–385.CrossRefGoogle Scholar
Sanchez-Soto, P.J. and Perez-Rodriguez, J.L., 1997 Influence of grinding in pyrophyllite-mullite thermal transformation assessed by 29-Si and 27-A1 MAS NMR spectroscopies Chem Mater 9 677–684 10.1021/cm960224+.CrossRefGoogle Scholar
Sanz, J. Madani, A. and Serratosa, J.M., 1988 Al-27 and Si-29 MAS NMR study of the kaolinite-mullite transformation J Am Ceram Soc 71 C418 C421 10.1111/j.1151-2916.1988.tb07513.x.CrossRefGoogle Scholar
Schroeder, P.A. and Pruett, R.J., 1996 Fe ordering in kaolinite: Insights from Si-29 and Al-27 MAS NMR spectroscopy Am Mineral 81 26–38 10.2138/am-1996-1-204.CrossRefGoogle Scholar
Smith, M.E., 1993 Application of Al-27 NMR techniques to structure determination in solids Appi Magn Res 4 1–64 10.1007/BF03162555.CrossRefGoogle Scholar
Smith, M.E. Neal, G. Trigg, M.B. and Drennan, J., 1993 Structural characterization of the thermal transformation of halloysite by solid state NMR Appl Magn Res 4 157–170 10.1007/BF03162561.CrossRefGoogle Scholar
Wardle, R. and Brindley, G.W., 1972 The crystal structures of pyrophyllite, ITc and of its dehydroxylate Am Mineral 57 732–750.Google Scholar
Woessner, D.E., 1989 Characterization of clay minerals by Al-27 NMR spectroscopy Am Mineral 74 203–215.Google Scholar
Worrall, W.E., 1986 Clays and ceramic raw materials London Elsevier.Google Scholar