Lopes M A, Monteiro F J, Santos J D
INEB-Instituto de Engenharia Biomédica, Laboratório de Biomateriais, Rua do Campo Alegre, 823, 4150 Porto, Portugal.
J Biomed Mater Res. 1999;48(5):734-40. doi: 10.1002/(sici)1097-4636(1999)48:5<734::aid-jbm20>3.0.co;2-2.
CaO-P(2)O(5) glasses with additions of MgO and CaF(2) were used as a sintering aid of hydroxyapatite, and glass-reinforced hydroxyapatite composites obtained. Glasses promoted significant changes in the microstructure of the composites, namely with the formation of tricalcium phosphate secondary phases, beta and alpha-TCP. Quantitative phase analysis was performed by the Rietveld method using General Structure Analysis Software. Grain size measurements were carried out on SEM photomicrographs, using a planimetric procedure according to ASTM E 112-88. Flexural bending strength was determined from concentric ring-on-ring testing. Flexural bending strength (FBS) of glass-reinforced hydroxyapatite composites was found to be about twice or three times higher than that of unreinforced hydroxyapatite and tended to depend more on porosity and beta and alpha-TCP secondary phases, rather than on grain size. Traces of alpha-tricalcium phosphate significantly enhanced the strength of the composites. Using the rule of mixtures to estimate the zero porosity bending strength, the Duckworth-Knudsen model applied to the composites gave a porosity correction factor, b, with a value of 4.02. Weibull statistics were also used to analyze biaxial strength data and the level of reinforcement obtained by comparing failure probability for the composites and for the unreinforced hydroxyapatite. Lower activation energies for grain growth were observed for the composites compared to unreinforced hydroxyapatite, which should be attributed to the presence of a liquid glassy phase that promotes atomic diffusion during the sintering process.
添加了MgO和CaF₂的CaO-P₂O₅玻璃被用作羟基磷灰石的烧结助剂,并制备出了玻璃增强羟基磷灰石复合材料。玻璃促使复合材料的微观结构发生显著变化,即形成了磷酸三钙次生相,β -TCP和α -TCP。使用通用结构分析软件通过Rietveld方法进行定量相分析。根据ASTM E 112 - 88,采用面积测量法在扫描电子显微镜照片上进行晶粒尺寸测量。通过同心环环测试测定抗弯强度。发现玻璃增强羟基磷灰石复合材料的抗弯强度(FBS)比未增强的羟基磷灰石高出约两倍或三倍,并且其更倾向于取决于孔隙率以及β -TCP和α -TCP次生相,而非晶粒尺寸。痕量的α -磷酸三钙显著提高了复合材料的强度。使用混合法则估算零孔隙率抗弯强度,应用于复合材料的Duckworth - Knudsen模型得出孔隙率校正因子b的值为4.02。还使用威布尔统计分析双轴强度数据,并通过比较复合材料和未增强羟基磷灰石的失效概率来确定增强水平。与未增强的羟基磷灰石相比,复合材料的晶粒生长活化能更低,这应归因于在烧结过程中促进原子扩散的液态玻璃相的存在。