JEAS  Vol.8 No.1 , March 2018
Hydrothermal Processing of Phase Pure and Doped Hydroxyapatite and its Characterization
Abstract: Hydroxyapatite (HA) is a synthetic ceramic which is used in numerous biomedical applications. However, its use is restricted in load bearing applications. A novel batch hydrothermal method is indigenously developed to synthesize fine size, crystalline hydroxyapatite (HA) and titania doped hydroxyapatite (TiO2-HA) powders with distinct phase formation. Powders were characterized using XRD, FTIR and DSC-TGA. Sharp peaks in HA XRD pattern after sintering at 1000°C indicate significant crystallinity while sharp peaks in TiO2 XRD pattern at 27°, 36° and 5° after sintering indicate anatase to rutile transformation. This fact is also confirmed by FTIR and DSC-TGA Plots.
Cite this paper: Rafique, M. (2018) Hydrothermal Processing of Phase Pure and Doped Hydroxyapatite and its Characterization. Journal of Encapsulation and Adsorption Sciences, 8, 18-37. doi: 10.4236/jeas.2018.81002.

[1]   Ashok, M., Arivuoli, D., Sundaram, N.M., et al. (2007) Growth and Characterization of Hydroxyapatite Crystals by Hydrothermal Method. Journal of Materials Science: Materials in Medicine, 18, 895-898.

[2]   Chaudhry, A.A., Kellici, S.S., Suela, H., et al. (2006) Instant Nano-Hydroxyapatite: A Continuous and Rapid Hydrothermal Synthesis. Chemical Communications, No. 21, 2286-2288.

[3]   Alby, D., Zajac, J., Prelot, B., et al. (2018) Recent Developments in Nanostructured Inorganic Materials for Sorption of Cesium and Strontium: Synthesis and Shaping, Sorption Capacity, Mechanisms, and Selectivity—A Review. Journal of Hazardous Materials, 344, 511-530.

[4]   Mohseni-Salehi, M.S., Taheri-Nassaj, E. and Hosseini-Zori, M. (2018) Effect of Dopant (Co, Ni) Concentration and Hydroxyapatite Compositing on Photocatalytic Activity of Titania towards Dye Degradation. Journal of Photochemistry and Photobiology A: Chemistry, 356, 57-70.

[5]   Prekajski Ðorđević, M., Yoshida, K., Babić, B., et al. (2018) In-Situ Immobilization of Sr Radioactive Isotope Using Nanocrystalline Hydroxyapatite. Ceramics International, 44, 1771-1777.

[6]   Stipniece, L., Stepanova, V., et al. (2018) Comparative Study of Surface Properties of Mg-Substituted Hydroxyapatite Bioceramic Microspheres. Journal of the European Ceramic Society, 38, 761-768.

[7]   Liu, D.-M., Troczynski, T. and Tseng, W.J. (2001) Water-Based Sol—Gel Synthesis of Hydroxyapatite: Process Development. Biomaterials, 22, 1721-1730.

[8]   Arends, J., Christoffersen, J., Eckert, H., et al. (1987) A Calcium Hydroxyapatite Precipitated from an Aqueous Solution: An International Multimethod Analysis. Journal of Crystal Growth, 84, 515-532.

[9]   Maity, J.P., Hsu, C.-M., et al. (2018) Removal of Fluoride from Water through Bacterial-Surfactin Mediated Novel Hydroxyapatite Nanoparticle and Its Efficiency Assessment: Adsorption Isotherm, Adsorption Kinetic and Adsorption Thermodynamics. Environmental Nanotechnology, Monitoring and Management, 9, 18-28.

[10]   Earl, J., Wood, D. and Milne, S. (2006) Hydrothermal Synthesis of Hydroxyapatite. Journal of Physics: Conference Series, 26, 268.

[11]   Zhang, X. and Vecchio, K.S. (2007) Hydrothermal Synthesis of Hydroxyapatite Rods. Journal of Crystal Growth, 308, 133-140.

[12]   Byrappa, K. and Adschiri, T. (2007) Hydrothermal Technology for Nanotechnology. Progress in Crystal Growth and Characterization of Materials, 53, 117-166.

[13]   Byrappa, K. and Yoshimura, M. (2001) Handbook of Hydrothermal Technology: A Technology for Crystal Growth and Materials Processing. Noyes Publications, Norwich, NY.

[14]   Khalil, K.M.S. and Zaki, M.I. (1997) Synthesis of High Surface Area Titania Powders via Basic Hydrolysis of Titanium(IV) Isopropoxide. Powder Technology, 92, 233-239.

[15]   Addamo, M., Augugliaro, V., Loddo, V., et al. (2004) Preparation, Characterization, and Photoactivity of Polycrystalline Nanostructured TiO2 Catalysts. The Journal of Physical Chemistry B, 108, 3303-3310.

[16]   Parra, R., Góes, M.S., Castro, M.S., et al. (2008) Reaction Pathway to the Synthesis of Anatase via the Chemical Modification of Titanium Isopropoxide with Acetic Acid. Chemistry of Materials, 20, 143-150.

[17]   Mahshid, S., Askari, M. and Ghamsari, M.S. (2007) Synthesis of TiO2 Nanoparticles by Hydrolysis and Peptization of Titanium Isopropoxide Solution. Journal of Materials Processing Technology, 189, 296-300.

[18]   Zinfer, R.I., et al. (2009) Synthesis and Stabilization of Nano-Sized Titanium Dioxide. Russian Chemical Reviews, 78, 873.

[19]   Powder Diffraction Card (PDF Card No. 74-0566). Internatioal Centre for Diffraction Data.

[20]   Powder Diffraction Card for Hydroxyapatite (PDF Card No. 9-432). Internatioal Centre for Diffraction Data.

[21]   Sadat-Shojai, M. (2009) Preparation of Hydroxyapatite Nanoparticles: Comparison between Hydrothermal and Solvo-Treatment Processes and Colloidal Stability of Produced Nanoparticles in a Dilute Experimental Dental Adhesive. Journal of the Iranian Chemical Society, 6, 386-392.

[22]   Powder Diffraction Card (PDF Card No. 88-1175, 84-1286). Internatioal Centre for Diffraction Data.

[23]   Thamaphat, K., Limsuwan, P. and Ngotawornchai, B. (2008) Phase Characterization of TiO2 Powder by XRD and TEM. Kasetsart Journal—Natural Science, 42, 357-361.

[24]   Ninsonti, H., et al. (2009) Hydrothermal Synthesis of Titanium Dioxide (TiO2) Micropowder. Journal of Microscopy Society of Thailand, 23, 91-94.

[25]   Rafique, M.M.A. (2011) Hydroxyapatite Synthesis and Its Characterization. IRCBM Internal Report (Unpublished).

[26]   Tevis, I.D. and Stupp, S.I. (2011) Patterning of Periodic High-Aspect-Ratio Nanopores in Anatase Titanium Dioxide from Titanium Fluoride Hydrolysis. Nanoscale, 3, 2162-2165.

[27]   Muslimin, M. and Sulaiman, M.Y.M. (2009) In-Situ High Temperature XRD Analysis of Synthesized Calcium Phosphate Biomaterial Using DEHPA as the Starting Material. Journal of Nuclear and Related Technologies, 6, 51-56.

[28]   Koutsopoulos, S. (2002) Synthesis and Characterization of Hydroxyapatite Crystals: A Review Study on the Analytical Methods. Journal of Biomedical Materials Research, 62, 600-612.

[29]   Stutman, J.M., Termine, J.D. and Posner, A.S. (1965) Vibrational Spectra and Structure of the Phosphate Ion in Some Calcium Phosphates. Transactions of the New York Academy of Sciences, 27, 669-675.

[30]   Fowler, B.O. (1974) Infrared Studies of Apatites. I. Vibrational Assignments for Calcium, Strontium, and Barium Hydroxyapatites Utilizing Isotopic Substitution. Inorganic Chemistry, 13, 194-207.

[31]   Gadaleta, S.J., Mendelsohn, R., Paschalis, E.L., et al. (1995) Fourier Transform Infrared Spectroscopy of Synthetic and Biological Apatites. In: Amjad, Z., Ed., Mineral Scale Formation and Inhibition, Springer, Boston, MA, 283-294.

[32]   Klee, W.E. and Engel, G. (1970) I.R. Spectra of the Phosphate Ions in Various Apatites. Journal of Inorganic and Nuclear Chemistry, 32, 1837-1843.

[33]   Baddiel, C.B. and Berry, E.E. (1966) Spectra Structure Correlations in Hydroxy and Fluorapatite. Spectrochimica Acta, 22, 1407-1416.

[34]   Rafique, M.M.A. (2012) Doped Hydroxyapatite Synthesis. IRCBM Internal Report (Unpublished).

[35]   Rafique, M.M.A. (2012) Batch Hydrotermal Synthesis of Hydroxyapatite and Metal Oxides. IRCBM Internal Report (Unpublished).

[36]   Morterra, C., Bolis, V. and Fisicaro, E. (1989) The Hydrated Layer and the Adsorption of CO at the Surface of TiO2 (Anatase). Colloids and Surfaces, 41, 177-188.

[37]   Barone, J. (1976) A Kinetic Study of the Formation of Calcium Phosphate Minerals. Ph.D. Thesis.

[38]   Freund, F. and Knobel, R.M. (1977) Distribution of Fluorine in Hydroxyapatite Studied by Infrared Spectroscopy. Journal of the Chemical Society, Dalton Transactions, No. 11, 1136-1140.

[39]   Winand, L., Dallemagne, M.J. and Duyckaerts, G. (1961) Hydrogen Bonding in Apatitic Calcium Phosphates. Nature, 190, 164-165.

[40]   Joris, S.J. and Amberg, C.H. (1971) Nature of Deficiency in Nonstoichiometric Hydroxyapatites. II. Spectroscopic Studies of Calcium and Strontium Hydroxyapatites. The Journal of Physical Chemistry, 75, 3172-3178.

[41]   Liao, C.-J., Sun, J.-S., et al. (1999) Thermal Decomposition and Reconstitution of Hydroxyapatite in Air Atmosphere. Biomaterials, 20, 1807-1813.

[42]   Li, H., Khor, K.A. and Cheang, P. (2003) Impact Formation and Microstructure Characterization of Thermal Sprayed Hydroxyapatite/Titania Composite Coatings. Biomaterials, 24, 949-957.

[43]   Sun, H.P., Xu, S.H., et al. (2006) Preparation and Characterization of Visible-Light-Driven Carbon-Sulfur-Codoped TiO2 Photocatalysts. Industrial & Engineering Chemistry Research, 45, 4971-4976.

[44]   Qiu, S. and Kalita, S.J. (2006) Synthesis, Processing and Characterization of Nanocrystalline Titanium Dioxide. Materials Science and Engineering: A, 435-436, 327-332.