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Evolution of the microstructure of interstratified Ca-saturated clays during dehydration: SAXS and HRTEM analysis

Published online by Cambridge University Press:  09 July 2018

H. Ben Rhaiem
Affiliation:
LPM, Faculté des Sciences de Bizerte, 7021Jarzouna, Tunisia
D. Tessier
Affiliation:
Station de Recherche du Sol, INRA, 78026 Versailles, France
C. H. Pons
Affiliation:
CRMD Université d'Orléans, 45067 Orléans cedex2, France
A. Ben Haj Amara
Affiliation:
LPM, Faculté des Sciences de Bizerte, 7021Jarzouna, Tunisia

Abstract

This paper aims at characterizing the structural and textural evolution of three mixed-layered clays in Ca-form from Southern and Central Tunisia, These samples contain various amounts of mixed-layer smectite-illite associated with crystallites of kaolinite. The clay fractions were prepared in the Ca-form and submitted to suction pressures increasing from 3.2 up to 1000 kPa. The structural and textural changes of the pastes obtained were studied by TEM and SAXS. The TEM observations and SAXS quantitative analysis on samples at low stress (3.2 kPa) showed that the thickness of the particles (number of layers per particle) and their lateral extension (in the plane of layers) decrease with increasing illite content. The textural evolution during drying, as described by SAXS, is controlled by the geometry of particles which is determined by the mineralogy of the structural units. With increasing illite content, the particles became shorter, rigid and had flat surfaces. This geometry increases their ability to associate face-to-face during dehydration. When the 2:1 fraction contains a high proportion of smectite, the architecture of the clay-water system at high water content (low stress) seems to be analogous to that of smectites. However, contrary to the behaviour of pure smectites reported in the literature, desiccation led first to a rupture of particles and a reorganization of the geometry of the pore system. This behaviour is due to the rigidity of particles caused by the presence of non-exchangeable K. The structural evolution showed that for an illite-rich sample a transition from the three-water layer to the one-water layer state occurred at 1000 kPa, whereas for smectite-rich materials, the hydration state of layers, i.e. three water layers, was not affected.

Type
Research Article
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 1998

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References

Ben Rhaiem, H. (1983) Etude du comportement hydrique des montmorillonites calciques et sodiques par analyse de la diffi∼sion des rayons X aux petits angles. Thesis, Univ. Orléans, France.Google Scholar
Ben Rhaiem, H., Pons, C.H. & Tessier, D. (I987) Factors affecting the microstmcture of smectite: role of cation and applied stress. Proc. Int. Clay Conf., Denver, 292-297.Google Scholar
Ben Rhaiem, H., Tessier, D. & Pons, C.H. (1986) Comportement hydrique et évolution structurale et texturale des montmorillonites au cours d'un cycle de dessiccation-humectation. Partie I: cas des montmorillonites calciques. Clay Miner. 21, 9–29.Google Scholar
Burchill, S. & Hayes, M.H.B, (1980) Adsorption of poly (vinyl) alcohol by clay minerals. Pp. 109–121 in: Agrochemicals in Soils (Banin, A. & Kafkafi, U., editors). Pergamon, Oxford.Google Scholar
Drits, V.A. (1975) The structural and crystallochemical features of layer-silicates. Pp. 35–51 in: Crystallochemistry of Minerals and Geological Problems (Kossovskaya, A.G., editor). Nauka, Novosibirsk.Google Scholar
Drits, V.A. & Tchoubar, C. (1990) X-ray Diffraction by Disordered Lamellar Structures: Theory and Application to Microdivided Silicates and Carbons. Springer Verlag, New York, Berlin, Heidelberg.CrossRefGoogle Scholar
Goldberg, S. & Glaubig, R.A. (1987) Effect of saturating cation, pH, and aluminum and iron oxide on the floculation of kaolinite and montmorilloni﹜e. Clays Clay Miner. 35, 220227.Google Scholar
Hetzel, F. & Doner, H.E. (1993) Some colloidal properties of beidellite: comparison with low and high charge montmorillonites. Clays Clay Miner. 41, 453460.CrossRefGoogle Scholar
Hetzel, F., Tessier, D., Jaunet, A.M. & Doner, H.E. (1994) The microstructure of three Na+ smectites: the importance of the particle geometry on dehydration and rehydration. Clays Clay Miner. 42, 242–248.CrossRefGoogle Scholar
Kakinoki, J. & Komura, Y. (1952) Intensity of X-ray diffraction by one dimensionally disordered crystal. J. Phys. Soc. Japan, 7, 30-35.Google Scholar
MacEwan, D.M.C. (1956) Fourier transform methods for studying scattering from lamellar system. I. A direct method for analysing interstratified mixtures. Koloidzeitschr. 149, 96108.Google Scholar
MacEwan, D.M.C. (1958) Fourier transform methods for studying scattering from lamellar system. II. The calculation of X-ray diffraction effects for various types of interstratification. Koloidzeitschr. 156, 6167.Google Scholar
Mering, J. (1949) Interférences des rayons X dans les systémes á interstratification désordonnée. Acta Crystallogr. 2, 371377.Google Scholar
Moore, D.M. & Reynolds, R.C. (1989) X-Ray Diffraction and the Identification and Analysis of Clay Minerals. Oxford University Press, Oxford, New York.Google Scholar
Plançon, A. (1981) Diffraction by layer containing different kinds of layers and stacking faults. J. Appl. Cryst. 14, 300304.Google Scholar
Pons, C.H., Ben Rhaiem, H., Tessier, D. & Clinard, C. (1987) Apport de la diffusion aux petits angles de rayons X á l‘étude de la microstructure des mathéiaux argileux. Pp. 37–4 2 in: Micromorphologie des Sols/Soil Micromorphology. (Fedomff, N., Bresson, L.M. & Courty, M.A., editors). AFES, Plaisir, France.Google Scholar
Pons, C.H., de la Callc, C. & Martin de Vidales, J.L. (1995) Quantification curves for XRD analysis of mixed-layer 14 Å/10 Å clay minerals. Clays Clay Miner. 43, 246254.Google Scholar
Pons, C.H., Tessier, D., Ben Rhaiem, H. & Tchoubar, D. (1982) A comparison between X-ray studies and electron microscopy observations of smectite fabric. Proc. Int. Clay. Conf., Bologna-Pavia, 165-186.Google Scholar
Reynolds, R.C. (1980) Interstratified clay minerals. Pp. 249-303 in: Crystal Structures of Clay Minerals and their X-ray Identification. (Brindley, G.W. & Brown, G., editors). Mineralogical Society, London.Google Scholar
Richards, L.A. (1941) A pressure-membrane extraction apparatus for soil solution. Soil Sci. 51, 377–386.Google Scholar
Saez-Aunon, J., Pons, C.H., Iglesias, J.E. & Rausell- Colom, J.M. (1983) Etude du gonflement des vermiculites-ornithine en solution saline par analyse de la diffusion des rayons X aux petits angles. Méthode d'interprétation et recherche des paramètres d'ordre. J. Appl. Crystallogr. 16, 439–448.Google Scholar
Soljic, Z. & Marjanovic-Krajovan, V. (1968) Methode rapide de dosage de SiO2, Fe2O3, Al2O3, TiO2, CaO et MgO dans une bauxite. Analyse rapide de calcaire et de dolomite. Chimie Analytique, 50, 122.Google Scholar
Środoń, J. & Elsass, F., (1994) Effect of the shape of fundamental particles on XRD characteristics of illitic minerals. Eur. J.. Miner. 6, 113–122.Google Scholar
Swartzen-Allen, S.L. & Matijevic, E. (1976) Colloid and surface properties of clay suspensions. III. Stability of montmorillonite and kaolinite. J. Coll. Interf. Sci. 56, 159167.Google Scholar
Tessier, D. (1984) Etude expérimentale de l'organisation des matériaux argileux. Hydratation, gonflement et structuration au cours de la dessiccation et de la réhumectation. Doc. Sci. thesis, Univ. Paris VII, France.Google Scholar
Tessier, D. (1990) Behaviour and microstmcture of clay minerals. Pp. 387–415 in: Soil Colloids and their Associations in Aggregates (De Boodt, M.F., Hayes, M.H.B. & Herbillon, A., editors). Plenum Press, New York.Google Scholar
Tessier, D. & Berrier, J. (1979) Utilisation de la microscopie électronique á balayage dans l'étude des sols. Observations des sols humides soumis á différents pF. Science du Sol, 1, 6782.Google Scholar
Touret, O., Ports, C.H., Tessier, D. & Tardy, Y. (1990) Etude de la répartition de l'eau dans les argiles saturées Mg2+ aux fortes teneurs en eau. Clay Miner. 25, 217233.Google Scholar