The Effects and Interactions of Synthesis Parameters on Properties of Mg Substituted Hydroxyapatite

In this study, the effects and interactions of reaction time and capping agent assistance during sol-gel synthesis of magnesium substituted hydroxyapatite nanopowder (MgHA) on hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P ratio and mean crystallite size was examined experimentally as well as through statistical analysis. MgHA nanopowders were synthesized by sol-gel technique at room temperature using aqueous solution of calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and potassium dihydrogen phosphate as starting materials. The reaction time for sol-gel synthesis was varied between 15 to 60 minutes. Two process routes were followed with and without addition of triethanolamine (TEA) in the solutions. The elemental compositions of as-synthesized powders were determined using X-ray fluorescence (XRF) spectroscopy. The functional groups present in the assynthesized MgHA nanopowders were established through Fourier Transform Infrared Spectroscopy (FTIR). The amounts of phases present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders were determined using X-ray diffraction (XRD). The HA content in biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized MgHA nanopowders increased effectively with reaction time of sols (p<0.0001, two way ANOVA), however, these were independent of TEA addition (p>0.15, two way ANOVA). The MgHA nanopowders synthesized with TEA assistance exhibited 14 nm lower crystallite size (p<0.018, 2 sample t-test) compared to the powder synthesized without TEA assistance.




References:
[1] L. B. Hossein-Nezhad, A. Maghbooli, Z. Bandarian, F. Mortaz, S.
Soltani, Association of Bone Mineral Density and Lifestyle in Men,
Iran. J Publ Heal. Vol. 35 2007, pp. 51–56.
[2] M. H. Fathi and A. Hanifi “Evaluation and characterization of
nanostructure hydroxyapatite powder prepared by simple sol-gel
method,” Materials Letters, 2007, vol.61, pp. 3978-3983.
[3] M. M. Savalani, L. Hao, P. M. Dickens, Y. Zhang, K. E. Tanner and R.
A. Harris, “The effects and interactions of fabrication parameters on the
properties of selective laser sintered hydroxyapatite polyamide
composite biomaterials,” Rapid Prototyping Journal, 2012, vol.18, 1,
pp.16-27.
[4] M. Percival, “Bone Health & Osteoporosis”, Appl. Nutr. Sci. Rep., 1995,
vol.5, pp. 1-5.
[5] T. Ioanovici, “Influence of magnesium doping on synthesized
hydroxyapatite using the wet precipitation method”, E-Health and
Bioengineering Conference (EHB), 2011, pp. 1-4.
[6] R. Ramachandra, H. N. Roopa, T. S. Kannan, “Solid state synthesis and
thermal stability of HAP and HAP-β-TCP composite ceramic powders”.
J Mater Sci Mater Med 1997, vol.8, pp. 511-518.
[7] N. Pramanik, A. Tarafdar, and P. Pramanik, “Capping agent assisted
synthesis of nano sized hydroxyapatite comparative studies of the
physicochemical properties,” Journal of materials processing
technology, 2007, vol.184, pp. 131-138.
[8] M.H. Fathi, A. Hanifi, and V. Mortazavi, Preparation and Bioactivity
Evaluation of Bone-Like Hydroxyapatite Nano-powder, J. Mater.
Process. Technol., 2008, vol.202, pp. 536–542.
[9] R. Jenkins and R.L. Snyder, Introduction to X-ray Powder
Diffractrometry, Wiley, New York, 1996.
[10] S.V. Dorozhkin, Mechanism of solid-state conversion of nonstoichiometric
hydroxyapatite to biphasic calcium phosphate: Russ
Chem Bull Int, 2003, 52, pp. 2369-2375.
[11] B.D. Cullity and S.R. Stock, Elements of X-Ray Diffraction, 3rd ed.,
Prentice-Hall Inc., Englewood Cliffs, 2001.
[12] S. Kannan, J.M. Ventura, and J.M.F. Ferreira, Aqueous Precip- itation
Method for the Formation of Mg-Stabilized b-Tricalcium phosphate: An
X-ray Diffraction Study, Ceram. Int., 2007, vol.33, pp. 637–641
[13] I. V Fadeev, L. I. Shvorneva, S. M. Barinov, and V. P. Orlovskii,
“Synthesis and Structure of Magnesium-Substituted Hydroxyapatite,”
Inorg. Mater., 2003, vol.39, pp. 947–950
[14] S. C. Afshar A, Ghorbani M, Ehsani N, Saeri MR, “Some important
factors in the wet precipitation process of hydroxyapatite,” Mater Des.
24 (n.d.) pp.197–202.
[15] H. K. Varma, S. S. Babu, “Synthesis of calcium phosphate bioceramics
by citrate gel pyrolysis method,” Ceram Int, 2005, vol.31, pp. 109-114.
[16] Z. Aizawa, H. Ueno, K. Itatani, Synthesis of calcium-deficient apatite
fibers by a homogenous precipitation method and their characterization,
J Eur Ceram Soc., 2006, vol.26, pp. 501–507.
[17] J. H. Park, D. Y. Lee, K. T. Oh, and Y. K. Lee, “Bioactivity of calcium
phosphate coatings prepared by electrodeposition in a modified
simulated body fluid,” Materials Letters, 2006, vol.60, pp. 2573-2577.
[18] U. Vijayalakshmi, S. Rajeswari, “Preparation and characterization of
microcrystalline hydroxyapatite using sol-gel method,” Trends Mater
Artif Org, 2006, vol.19, pp. 57-62.
[19] B. J. Singh, and D. Khanduja, “Perspectives of Control Phase to manage
Six Sigma implements: A Foundry Case”, International Journal of
Business Excellence, 2014, vol.7, 1, pp. 88-111.