Abstract
A new route for obtaining calcium-deficient apatites with a Ca/P ratio lower than 1.5 is described, in order to study their proton conduction at temperatures lower than 400 °C. The process is based on the hydrolysis of a mixed solution of Ca(NO3)2 and NH4H2PO4 in the presence of hexamethylenetetramine at a pH of approximately 5 and temperatures of 85–90 °C. The resulting spherical particles of 14 μm in average diameter were aggregates of smaller needles with approximate composition Ca8.5(HPO4)2(PO4)4OH · H2O. The effects of the reagent concentrations, pH, aging time, and temperature were studied, and the solids were characterized by x-ray diffraction, infrared absorption spectroscopy, and electron microscopy. The ionic conduction measured by alternating-current impedance spectroscopy yielded a value of 3 μSm−1 at 200 °C.
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References
R.Z. Le Geros, Calcium Phosphates in Oral Biology and Medicine, Monographs in Oral Science Vol. 15, edited by H. M. Myers (Karger, Basel, 1991).
J.A.S. Bett, L.G. Christner, and W.K. Hall, J. Am. Chem. Soc. 89, 5535 (1967).
Y. Imizu, M. Kadoya, H. Abe, H. Itoh, and A. Tada, Chem. Lett. 415 (1982).
T. Suzuki, T. Hatsushika, and Y. Hayakawa, J. Chem. Soc. Faraday Trans. 1 77, 1059 (1981).
T. Suzuki, T. Hatsushika, and M. Miyake, J. Chem. Soc. Faraday Trans. 1 78, 3605 (1982).
M. Nagai, T. Nishino, and T. Saeki, Sens. Actuators 15, 145 (1988).
K. Yamashita, H. Owada, T. Umegaki, T. Kanazawa, and T. Futagami, Solid State Ionics 28–30, 660 (1988).
K. Yamashita, K. Kitagaki, and T. Umegaki, J. Am. Ceram. Soc. 78, 1191 (1995).
S. Chandra, in Proton Conductors in Superionic Solids and Solid Electrolites, edited by A. Laskar and S. Chandra (Academic Press, Boston, 1990), p. 185.
S.J. Joris and C.H. Amberg, J. Phys. Chem. 75, 3167 (1971).
S.J. Joris and C.H. Amberg, J. Phys. Chem. 75, 3172 (1971).
W.E. Brown, M. Mathew, and L.C. Chow, in Roles of Octacalcium Phosphate in Surface Chemistry of Apatites in Adsorption on/in Surface Chemistry of Hydroxyapatite, edited by D.N. Misra (Plenum Press, New York, 1984).
M. Andrés-Vergés, C. Fernández-González, and M. Martínez-Gallego, J. Eur. Ceram. Soc. 18, 1245 (1998).
K. Matsuda, Y. Kaneko, H.J. Fei, K. Fujita, and S. Mitsuzawa, Proc. Fac. Sci. Tokai Univ. 27, 73 (1992).
B.O. Fowler, E.C. Moreno, and W.E. Brown, Arch. Oral Biol. 11, 477 (1966).
E.E. Berry and C.B. Baddiel, Spectrochim. Acta, Part A 23, 1781 (1967).
R.Z. LeGeros, G. Daculsi, I. Orly, T. Abergas, and W. Torres, Scanning Microscopy 3, 129 (1989).
C.B. Baddiel and E.E. Berry, Spectrochim. Acta 22, 1407 (1966).
B.O. Fowler, Inorg. Chem. 13, 194 (1974).
P.F. González-Díaz and A. Hidalgo, Spectrochim. Acta, Part A 32, 631 (1976).
V. Privman, D.V. Goia, and E.Matijević, J. Colloid Interface Sci. 213, 36 (1999).
D.V. Goia and E. Matijević, Colloids Surf. 146, 139 (1999).
R.H. Kretsinger and D.J. Nelson, Coord. Chem. Rev. 18, 29 (1976).
F. Cachadiña, J.D. Solier, and A. Dominguez-Rodriguez, Bol. Soc. Esp. Ceram. Vid. 37, 238 (1998).
J.R. Macdonald, Impedance Spectroscopy (Wiley, New York, 1987).
G. Williams, D.C. Watts, S.B. Dev, and A.M. North, Trans. Faraday Soc. 67, 1323 (1970).
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Andrés-Vergés, M., Fern´andez-González, C., Martínez-Gallego, M. et al. A new route for the synthesis of calcium-deficient hydroxyapatites with low Ca/P ratio: Both spectroscopic and electric characterization. Journal of Materials Research 15, 2526–2533 (2000). https://doi.org/10.1557/JMR.2000.0362
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DOI: https://doi.org/10.1557/JMR.2000.0362