Hostname: page-component-cd9895bd7-8ctnn Total loading time: 0 Render date: 2024-12-26T20:56:41.810Z Has data issue: false hasContentIssue false
  • English
  • Français

Formation of Spinel from a Hydrotalcite-Like Compound at Low Temperature: Reaction between Edges of Crystallites

Published online by Cambridge University Press:  28 February 2024

Toshiyuki Hibino  and
Atsumu Tsunashima
Toshiyuki Hibino
Affiliation:
Materials Processing Department, National Institute for Resources and Environment, 16-3 Onogawa, Tsukuba, 305 Japan
Atsumu Tsunashima
Affiliation:
Materials Processing Department, National Institute for Resources and Environment, 16-3 Onogawa, Tsukuba, 305 Japan
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.

The thermal decomposition behavior of hydrotalcite-like compounds (HTlcs) prepared by reconstruction of calcined HTlcs is described. From the results of X-ray diffraction (XRD), it seems that dicarboxylate intercalates of HTlc calcined at 500 °C are completely reconstructed to Mg-Al-CO3 HTlc by exposure to aqueous Na2CO3. However, the Mg-Al-CO3 HTlc reconstructed under particular conditions yields spinel (MgAl2O4) at 400 °C. This temperature is very low, because Mg-Al-CO3 HTlc that has been reported yields spinel at 900 °C after forming a Mg-Al double oxide. The reconstructed Mg-Al-CO3 HTlc that yields spinel at 400 °C is obtained when the following conditions are fulfilled: the crystallites of the starting dicarboxylate intercalates are coagulated tightly and the calcined HTlcs and reconstructed materials are not ground. The Mg-Al-CO3 HTlc reconstructed under these conditions contains only 55–70% of carbonate anions required by stoichiometry. Therefore, we conclude that the transformation of reconstructed Mg-Al-CO3 HTlc to spinel at 400 °C is the result of a reaction occurring between edges of crystallites.

Keywords

Double HydroxideGrindingHydrotalciteReconstructionSpinelThermal Decomposition
Type
Research Article
Information
Clays and Clay Minerals , Volume 45 , Issue 6 , December 1997 , pp. 842 - 853
Copyright
Copyright © 1997, The Clay Minerals Society

References

Allmann, R., 1968 The crystal structure of pyroaurite Acta Crystallogr B24 972–977 10.1107/S0567740868003511.CrossRefGoogle Scholar
Bratton, R.J., 1969 Coprecipitates yielding MgAl2O4 spinel powders Am Ceram Soc Bull 48 759–762.Google Scholar
Brindley, G.W. and Kikkawa, S., 1979 A crystal-chemical study of Mg,Al and Ni,Al hydroxy-perchlorates and hydroxy-car-bonates Am Mineral 64 836–843.Google Scholar
Cavani, F. Trifirò, F. and Vaccari, A., 1991 Hydrotalcite-type anionic clays: Preparation, roperties and applications Catal Today 11 173–301 10.1016/0920-5861(91)80068-K.CrossRefGoogle Scholar
Chibwe, K. and Jones, W., 1989 Synthesis of polyoxometalate-pillared layered double hydroxides via calcined precursors Chem Mater 1 489–490 10.1021/cm00005a006.CrossRefGoogle Scholar
Chibwe, K. and Jones, W., 1989 Intercalation of organic and inorganic anions into layered double hydroxides J Chem Soc, Chem Commun 926–927.CrossRefGoogle Scholar
Constantino, V.R.L. and Pinnavaia, T.J., 1995 Basic properties of Mg2+,1-x Al3+ x layered double hydroxides intercalated by carbonate, hydroxide, chloride and sulfate anions Inorg Chem 34 883–892 10.1021/ic00108a020.CrossRefGoogle Scholar
Dimotakis, E.D. and Pinnavaia, T.J., 1990 New route to layered double hydroxides intercalated by organic anions: Precursors to polyoxometalate-pillared derivatives Inorg Chem 13 2393–2394 10.1021/ic00338a001.CrossRefGoogle Scholar
Drezdzon, M.A., 1988 Synthesis of isopolymetalate-pillared hydrotalcite via organic-anion-pillared precursors Inorg Chem 27 4628–4632 10.1021/ic00298a024.CrossRefGoogle Scholar
Giannelis, E.P. Nocera, D.G. and Pinnavaia, T.J., 1987 Anionic pho-tocatalysts supported in layered double hydroxides: Intercalation and photophysical properties of a ruthenium complex anion in synthetic hydrotalcite Inorg Chem 26 203–205 10.1021/ic00248a039.CrossRefGoogle Scholar
Gusmano, G. Nunziante, P. Traversa, E. and Chiozzini, G., 1991 The mechanism of MgAl2O4 spinel formation from the thermal decomposition of coprecipitated hydroxides J Eur Ceram Soc 7 31–39 10.1016/0955-2219(91)90051-Z.CrossRefGoogle Scholar
Hibino, T. Yamashita, Y. Kosuge, K. and Tsunashima, A., 1995 De-carbonation behavior of Mg-Al-CO3 hydrotalcite-like compounds during heat treatment Clays Clay Miner 43 427–432 10.1346/CCMN.1995.0430405.CrossRefGoogle Scholar
Hibino, T. Kosuge, K. and Tsunashima, A., 1996 Synthesis of carbon-hydrotalcite complex and its thermal degradation behavior Clays Clay Miner 44 151–154 10.1346/CCMN.1996.0440114.CrossRefGoogle Scholar
Hokazono, S. Nagai, H. and Kato, A., 1991 Synthesis of spinel powder by the homogeneous precipitation method Nippon Kagaku Kaishi 275–280.CrossRefGoogle Scholar
Hudson, M.J. Carlino, S. and Apperley, D.C., 1995 Thermal conversion of a layered (Mg/Al) double hydroxide to the oxide J Mater Chem 5 323–329 10.1039/jm9950500323.CrossRefGoogle Scholar
Ingram, L. and Taylor, H.F.W., 1967 The crystal structures of sjögrenite and pyroaurite Mineral Mag 36 465–479.Google Scholar
Itaya, K. Chang, H.-C. and Uchida, I., 1987 Anion-exchanged hy-drotalcite-like-clay-modified electrodes Inorg Chem 26 624–626 10.1021/ic00251a028.CrossRefGoogle Scholar
Kodama, H. Kotlyar, L.S. and Ripmeester, J.A., 1989 Quantification of crystalline and noncrystalline material in ground kaolin-ite by X-ray powder diffraction, infrared, solid-state nuclear magnetic resonance, and chemical-dissolution analyses Clays Clay Miner 37 364–370 10.1346/CCMN.1989.0370410.CrossRefGoogle Scholar
Kristof, Juhász, A.Z. and Vassányi, I., 1993 The effect of mechanical treatment on the crystal structure and thermal behavior of kaolinite Clays Clay Miner 41 608–612 10.1346/CCMN.1993.0410511.CrossRefGoogle Scholar
MacKenzie, K.J.D. Meinhold, R.H. Sherriff, B.L. and Xu, Z., 1993 27Al and 25Mg solid-state magic-angle spinning nuclear magnetic resonance study of hydrotalcite and its thermal decomposition sequence J Mater Chem 3 1263–1269 10.1039/jm9930301263.CrossRefGoogle Scholar
Miyata, S. and Kumura, T., 1973 Synthesis of new hydrotalcite-like compounds and their physico-chemical properties Chem Lett 843–848.CrossRefGoogle Scholar
Miyata, S., 1975 The syntheses of hydrotalcite-like compounds and their structures and physico-chemical properties—I: The systems Mg2+-Al3+-NCV, Mg2+-Al3+-CL, Mg2+-Al3+-C1O4-, Ni2+-Al3+-CL and Zn2+-Al3+-CL Clays Clay Miner 23 369–375 10.1346/CCMN.1975.0230508.CrossRefGoogle Scholar
Miyata, S., 1980 Physico-chemical properties of synthetic hy-drotalcites in relation to composition Clays Clay Miner 28 50–56 10.1346/CCMN.1980.0280107.CrossRefGoogle Scholar
Narita, E. Kaviratna, P. and Pinnavaia, T.J., 1991 Synthesis of het-eropolyoxometalate pillared layered double hydroxides via calcined zinc-aluminium oxide precursors Chem Lett 805–808.CrossRefGoogle Scholar
Pesic, L. Salipurovic, S. Markovic, V. Vucelic, D. Kagunya, W. and Jones, W., 1992 Thermal characteristics of a synthetic hydrotalcite-like material J Mater Chem 2 1069–1073 10.1039/jm9920201069.CrossRefGoogle Scholar
Rey, F. Fornés, V. and Rojo, J.M., 1992 Thermal decomposition of hydrotalcites: An infrared and nuclear magnetic resonance spectroscopic study J Chem Soc, Faraday Trans 88 2233–2238 10.1039/FT9928802233.CrossRefGoogle Scholar
Rouxhet, P.G. and Taylor, H.F.W., 1969 Thermal decomposition of sjögrenite and pyroaurite Chimia 23 480–485.Google Scholar
Yun, S.K. Constantino, V.R.L. and Pinnavaia, T.J., 1995 New polyol route to keggin ion-pillared layered double hydroxides Microporous Mater 4 21–29 10.1016/0927-6513(94)00079-B.CrossRefGoogle Scholar