Abstract
Calcium hydroxyapatite powder was prepared by sol-gel method using calcium acetate and PO(OC2H5)3 as initial compounds, and alcohol (methyl, ethyl, and propyl-alcohol) as solvent. Homogeneous solution and gels were prepared using a molar ratio of Ca/P=1.67. The evolution of the structure was detected by X-ray diffraction, IR, and FT-n(=1,2,3)D-EPR spectroscopy. The dried gels exhibit a signal characterized by a central line and two satellites. The 2D spectrum (ESEEM vs. field sweep) showed the same modulation for the central line. The FT-EPR spectrum vs. field sweep 2D-spectrum indicated that the satellites are due to an hfs splitting with water. The central region of this 2D spectrum is influenced by P and H in a concentration ratio of [H]/[P]=2.5. The ESEEM spectrum was simulated assuming the equation Vmod=Vmod(P)mVmod(H)n for two spin systems S=1/2 and I=1/2. This simulation gave form andn the values of 2 and 5, respectively. This finding suggests the structure:
for the unpaired state. It appears that one ethyl group does not hydrolyse in the gelation process. The ESEEM spectra of hydroxyapatite exhibit a modulation generated by P, H and Ca atoms.
Similar content being viewed by others
References
R.H. Doremus, J. Mat. Sci.27, 285 (1992).
L.L. Hench, J. Am. Ceram. Soc.74, 1487 (1991).
C. Laverinia, J.M. Schoenung, Ceramic Bullentin70(1), 48 (1991).
M. Jarcho, C.H. Bolen, M.B. Thomas, J.F. Kay, and R.H. Doremus, J. Mater. Sci.11, 2027 (1976).
M. Asada, K. Oukami, S. Nakamura, K. Takhashi, and Yogyio Kyokai-Shi, (The Ceram. Sos., Japan, 1987), vol. 95, p. 703.
M. Akao, H. Aoki, and K. Kat, J. Mater. Sci.16, 809 (1981).
A. Osaka, Y. Miura, K. Takeushi, M. Asada, and K. Takahashi, J. Mat. Sci.: Materials in Medicine2, 51 (1991).
Y. Masuda, K. Matubara, and S. Sakka, J. Cer. Soc. Japan, Int. Edition84, 98–1266.
A. Deptula, W. Lada, T. Olczac, A. Borello, C. Alvani, and A. di Bartolomeo, J. of Non. Cyystalline Solids147&148, 537 (1992).
T. Brendel, A. Engel, and C. Russel, J. Mat. Sci.: Materials in Medicine175 (1992).
S.P. Szu, L.C. Klein, and M. Greenblatt, J. Non-Cryst. Solids143, 21 (1992).
K. Nakamoto,Infrared Spectra of Inorganic and Coordination Compounds, (Willey, New York, 1963).
C.C. Trapalis, A. Koufoudakis, I. Dounis, M.A. Karakasides, and G. Kordas, Chimica Chronica23(2–3), 205 (1994).
A. Bues, M. Gehreke, and Z. Anorg. Chem.288, 291 (1956).
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Kordas, G., Trapalis, C.C. Fourier transform and multi dimensional EPR spectroscopy for the characterization of sol-gel derived hydroxyapatite. J Sol-Gel Sci Technol 9, 17–24 (1997). https://doi.org/10.1007/BF02439332
Received:
Accepted:
Issue Date:
DOI: https://doi.org/10.1007/BF02439332