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. Keywords—Capping agent, hydroxyapatite, regression analysis, sol-gel, 2sample t-test, two-way ANOVA.