Abstract
The chemical composition of zirconia gels precipitated from methanol solutions with excess, stoichiometric or deficient amounts of water as well, as the phase composition of fine ZrO2 powders obtained by thermal treatment of gels prepared by this method, were investigated. It was observed that both the stoichiometry and crystalline phase formation during thermal treatment of zirconia gels are strongly influenced by the amount of water added to the initial reaction mixture. Heating the hydrated zirconia gels in an inert oxygen-free atmosphere produced a black nonstoichiometric oxide. The degree of nonstoichiometry of zirconia and its microstructure are influenced by the initial conditions in the reaction mixture. The X-ray patterns of thermally treated samples prepared with a substoichiometric amount of water show power lines of monoclinic and tetragonal zirconia, while after the same thermal treatment to 700°C, those prepared with excess water in the initial methanol solution, show mainly tetragonal diffraction lines.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
C. Dall'Agnol, A. Gervasini, F. Morazzoni, F. Pinna, G. Strukul, and L. Zanderighi, J. Catal. 96(1), 106 (1985).
M.Y. He and J.G. Ekerdt, J. Catal. 90(1), 17 (1984).
T. Onishi, H. Abe, K. Maruya, and K. Domen, J. Chem. Soc. Chem. Commun 2, 103 (1986).
N.B. Jackson and J.G. Ekerdt, J. Catal. 101(1), 90 (1986).
A. Clearfield, G.H. Nancollas, and R.H. Blessing, Ion Exch. Solvent Extr. 5, 1 (1973).
J. Livage, K. Doi, and C. Mazieres, J. Am. Ceram. Soc. 51(6), 349 (1968).
T. Kosmac, R. Gopala Krisnan, V. Krasevec, and M. Kosmac, Journal de Physique, Colloque C1 47(2), 43 (1986).
M.J. Torralvo, M.A. Alario, and J. Soria, J. Catal. 86(2), 473 (1984).
T. Kokubo, Y. Teranishi, and T. Maki, J. Non-Cryst. Solids 56(1-3), 411 (1983).
C.J. Brinker and G.W. Sherer, Sol-Gel Processing (Academic Press, San Diego, 1990), p. 518.
R.C. Garvie, J. Phys. Chem. 69(4), 1238 (1965).
R.C. Garvie, J. Phys. Chem. 82(2), 218 (1978).
A. Krauth and H. Meyer, Ber. Deut. Keram. Ges. 42(3), 61 (1965).
Y. Suyama, T. Mizobe, and A. Kato, Ceramurgia Int. 3(4), 41 (1977).
M.J. Torralvo, J. Soria, and M.A. Alario, in Nonstiochiometry and the Glow Phenomenon in Zirconia Gels, Mater. Sci. Monograph, 10 (React. Solids, vol. 2) edited by K. Dyrek et al. (Elsevier, Amsterdam, 1982), p. 512.
Y. Murase, E. Kato, and H. Matsumato, Nippon Kagaku Kaishi 12, 2329 (1972).
B.H. Davis, J. Am. Ceram. Soc. 67(8), C168 (1984).
M.A. Blesa, A.J.G. Maroto, S.I. Passagio, N.E. Fizliolia, and G. Rigoti, J. Mater. Sci. 20(12), 4601 (1985).
Y. Murase and E. Kato, Ber. Dt.Keram. Ges. 57(4-5), 86 (1980).
E. Crucean and B. Randt, Trans. J. Brit. Ceram. Soc. 78(3), 58 (1979).
R. Srinivasan, L. Rice, and B.H. Davis, J. Am. Ceram. Soc. 73(11), 3528 (1990).
H.Th. Rijnten, in Formation, Preparation and Properties of Hydrous Zirconia in Physical and Chemical Aspects of Adsorbents and Catalysts, edited by B.G. Linsen (Academic Press, London, 1970), p. 315.
Handbook of Analytical Chemistry, 1st edn., edited by L. Meites, McGraw-Hill, New York, 1963), p. 5.
I.M. Kolthoff and E.B. Sandell, Textbook of Quantitative Inorganic Analysis, (Croatian Translation), ( Školska knjiga Zagreb, Zagreb, 1951), p. 427.
Z. Rant, Die Erzeugung von Soda: Nach dem Solvay-Verfahren, (Forshungsinstitut für Bergbau und Chemische Technologie Tuzla, Sarajevo, 1968), p. 504.
E. Scholz, Karl Fisher Titrations, Determination of Water Chemical Laboratory Practice (Springer-Verlag, Berlin, 1984), p. 25.
D.A. Skoog and D.M. West, Fundamentals of Analytical Chemistry, 3rd edn. (Holt, Rinehart and Winston, New York, 1976), p. 197.
R.J. Hill and C.J. Howard, J. Appl. Cryst. 20(6), 467 (1987).
J. Livage and J. Lemerle, Annu. Rev. Mater. Sci. 12, 103 (1982).
F.G.R. Gimblett, A.A. Rahman, and K.S.W. Sing, J. Chem. Techn. Biotechnol. 30(2), 51 (1980).
F.G.R. Gimblett, A.A. Rahman, and K.W. Sing, J. Colloid Interface Sci. 84(2), 337 (1981).
J. Ma?ek, D. Arzenšek, and M. Marinšek, in Proc. 22nd Int. Conf. on Microelectronics, MIEL '94 and 30th Symp. on Devices and Materials, SD '94, edited by I. Šorli, B. Kren, and M. Limpel (Terme Zre?e-Rogla, Slovenia, 1994), p. 331.
A.N. Ermakov, I.N. Marov, and V.K. Balyaeva, Zh. Neorgan. Khim. 8(7), 1623 (1963).
J. Ma?ek, M. Marinšek, and B. Novosel, J. Thermal Anal. 48, 675 (1997).
R. Srinivasan, R.V. Mureleedharan, S.K. Roy, and P.K.K. Nayar, J. Am. Ceram. Soc. 78(2), 429 (1995).
A.A. Rahman, Thermochim. Acta 85, 3 (1985).
J. Livage, K. Doi, and C. Mazieres, J. Am. Ceram. Soc. 51(6), 349 (1968).
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Marinšek, M., Maček, J. & Meden, T. Starved Water Hydrolysis of Different Precursors and its Influence on the Properties of Precipitated Zirconia. Journal of Sol-Gel Science and Technology 23, 119–127 (2002). https://doi.org/10.1023/A:1013791216164
Issue Date:
DOI: https://doi.org/10.1023/A:1013791216164