Investigation of phase distribution in gradient HA/β-TCP/CaCO3 composite synthesized from oyster shell via hydrothermal method for bone regeneration
摘要
In this study, flake oyster shells were utilized as a natural calcium source, while diammonium hydrogen phosphate served as the phosphorus source. Through a hydrothermal process conducted at 190 °C for 48 h, the oyster shells were directly converted into a biphasic calcium phosphate composite comprising hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP), with a minor portion of unreacted oyster shell (CaCO3) remaining. Quantitative phase analysis revealed that the final composition consisted of approximately 42% HA, 44% β-TCP, and 14% CaCO3. To investigate the spatial distribution of the phases, EPMA mapping and EBSD phase analysis were performed on the cross-section of the composite. The results indicated a gradient distribution: CaCO3 and some HA were concentrated near the outer layer, the middle region was predominantly composed of HA, and β-TCP was more abundant near the inner surface layer. HRTEM further confirmed the coexistence of HA and β-TCP phases, validating the successful formation of the biphasic structure. The study demonstrates that using flake oyster shells as a calcium source enables the fabrication of HA/β-TCP/CaCO3 composite materials with a naturally developed gradient structure through a simple hydrothermal method, offering promising potential for bone repair applications.