Abstract
Reactions between aqueous solutions of aluminum salts and ammonium terephthalate at pH 6–8 lead to the formation of a previously unknown, weakly ordered phase. It has signs of a layered compound with a unit cell parameter of 1.072–1.073 nm. Its empirical composition can be represented by the formula Al2O3 · xC8H6O4 · yH2O · δ(NH3), where x = 0.7–1.2, y = 4.4–6.0, and δ = 0–0.4. It has good structural order across the layers, whereas the order along the layers is weaker and depends on synthesis conditions. Calcination at 120°C leads to partial dehydration and changes the order along the layers, whereas the order across the layers changes little, with a slight increase in lattice strain. Heat treatment at 400°C leads to almost complete dehydration and fully eliminates the order along the layers, whereas the order across the layers is partially retained. Firing at 800°C leads to the formation of γ-Al2O3. A structural model has been proposed for the new phase.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Ferey, G., Hybrid Porous Solids: Past, Present, Future, Chem. Soc. Rev., 2008, vol. 37, no. 1, pp. 191–214.
Yaghi, O.M., O’Keeffe, M., Ockwig, N.W., et al., Reticular Synthesis and the Design of New Materials, Nature, 2003, vol. 423, pp. 705–714.
Duan, X. and Evans, D.G., Layered Double Hydroxides (Structure and Bonding), Berlin: Springer, 2006.
Deng, Z.-X., Li, L., and Li, Y., Novel Inorganic-Organic-Layered Structures Crystallographic Understanding of Both Phase and Morphology Formations of One-Dimensional CdE (E = S, Se, Te) Nanorods in Ethylenediamine, Inorg. Chem., 2003, vol. 42, no. 7, pp. 2331–2341.
Loiseau, T., Serre, C., Huguenard, C., et al., A Rationale for the Large Breathing of the Porous Aluminum Terephthalate (MIL-53) upon Hydration, Chem.—Eur. J., 2004, vol. 10, no. 6, pp. 1373–1382.
Volkringer, C., Loiseau, T., Guillou, N., et al., XRD and IR Structural Investigations of a Particular Breathing Effect in the MOF-Type Gallium Terephthalate MIL-53(Ga), Dalton Trans., 2009, vol. 12, pp. 2241–2249.
Panasyuk, G.P., Azarova, L.A, Voroshilov, I.L., et al., Hydrothermal Synthesis of Aluminum Terephthalate, Inorg. Mater., 2005, vol. 41, no. 11, pp. 1201–1205.
Roisnel, T. and Rodriguez-Carvajal, J., WinPLOTR: A Windows Tool for Powder Diffraction Patterns Analysis, Mater. Sci. Forum, 2000, pp. 118–123.
Williamson, G.K. and Hall, W.H., X-Ray Line Broadening from Filed Aluminium and Wolfram, Acta Metall., 1953, vol. 1, pp. 22–31.
Lygin, V.I., Muzyka, I.S., Zhukova, L.A., et al., Vibrational Spectrum and Structure of Hydroxyl-Containing Species on the Surface of High-Temperature Alumina Polymorphs, Zh. Fiz. Khim., 1993, vol. 67, no. 6, pp. 1246–1250.
Deacon, G.B. and Phillips, R.J., Relationships between the Carbon-Oxygen Stretching Frequencies of Carboxylato Complexes and the Type of Carboxylate Coordination, Coord. Chem. Rev., 1980, vol. 33, pp. 227–250.
Nakamoto, K., Infrared Spectra of Inorganic and Coordination Compounds, New York: Wiley, 1963. Translated under the title Infrakrasnye spektry neorganicheskikh i koordinatsionnykh soedinenii, Moscow: Mir, 1966, pp. 215–217.
Author information
Authors and Affiliations
Corresponding author
Additional information
Original Russian Text © D.G. Shabalin, G.P. Panasyuk, L.A. Azarova, 2013, published in Neorganicheskie Materialy, 2013, Vol. 49, No. 4, pp. 416–423.
Rights and permissions
About this article
Cite this article
Shabalin, D.G., Panasyuk, G.P. & Azarova, L.A. A new layered phase in the alumina-terephthalic acid-water system. Inorg Mater 49, 401–407 (2013). https://doi.org/10.1134/S0020168513030199
Received:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0020168513030199