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Effects of Changes in Structural Hydration of Multiphasic Heterogeneous Calcium Phosphate Powders Created via Auto-Ignition Combustion Synthesis

  • Nina Louise Vollmer (a1), Douglas Burkes (a2), John Moore (a3) and Reed Ayers (a4)


Calcium phosphate (CaP) materials are commonly used in bone tissue engineering applications since they closely resemble the chemistry of bone and teeth. The inorganic component of mineralized tissue is multiphasic in nature-thus to better replicate those tissues, CaP materials should also be multiphasic. Combustion synthesis is a process that creates multiphasic CaP (HCaP) with low energy input over a relatively short time. The structure and chemistry of HCaP synthesized via auto-ignition combustion synthesis (AICS) varies greatly with respect to structural hydration. Product hydration was accomplished by modifying hydrogen and oxygen content in the combustion reaction by changing the amount of fuel, urea [ ] pre-reaction, and heating or sintering products post-reaction. The reaction equation for this specific system is given below. Calcium nitrate [ ], and ammonium nitrate [ ] are the components that form HCaP. Urea acts as an ignition source and fuel. Changes in the amount of urea dictate the amount of excess hydrogen to form water within the reaction. Excess products formed include water, carbon dioxide, and nitrogen. Salts of the reactants were mixed with 10 milliliters of de-ionized water in a Pyrex beaker, heated on a hot plate for 20 minutes or until the reactants began to foam, and then placed in a muffle furnace at 1000°C until the foam ignited in a combustion reaction. This was noted by the progression of a combustion wave throughout the foam. Post-AICS, products were heated at 105°C for 8 hours and 24 hours and massed to determine water content of the product. Subsequently, the products were sintered at 1000°C for 8 hours and massed again. The primary products formed using AICS are hydroxyapatite (HA), á-tricalcium calcium phosphate (TCP) and hydrated forms of tricalcium phosphate (HTCP). During low temperature heating, 105°C, water content decreases as time increases and the products began to densify. Initial results indicate that surface porosity decreases during the powder densification. XRD shows that peak intensity increases after low temperature heating, indicating an increase in crystallinity and grain orientation. XRD confirms that both crystalline and amorphous phases occur in the hydroxyapatite (HA), á-TCP and HTCP products. The amount of structural hydration has an effect on CaP, and these effects are noted by an increase in density and decrease in porosity as structurally bound water is removed from the system. Future research will be dedicated to determining hydration ratio (amount of urea in the reaction to the amount of water within the products) and a Ca:P ratio that result in optimal powder porosity, ductility and grain size generating a multiphasic HCaP implant biomaterial that accurately replicates natural bony tissue.



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Effects of Changes in Structural Hydration of Multiphasic Heterogeneous Calcium Phosphate Powders Created via Auto-Ignition Combustion Synthesis

  • Nina Louise Vollmer (a1), Douglas Burkes (a2), John Moore (a3) and Reed Ayers (a4)


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