Faculty of Materials Science and Engineering, Hubei University, Wuhan 430062, People's Republic of China.
Acta Biomater. 2011 Mar;7(3):1387-97. doi: 10.1016/j.actbio.2010.10.008. Epub 2010 Oct 20.
Titanium hydride powders are utilized to enhance the foaming process in the formation of orthopedic NiTi scaffolds during capsule-free hot isostatic pressing. In order to study the formation mechanism, the thermal behavior of titanium hydride and hydrogen release during the heating process are systematically investigated in air and argon and under vacuum by X-ray diffraction (XRD), thermal analysis, including thermogravimetric analysis and differential scanning calorimetry, energy dispersive X-ray spectroscopy, and transmission electron microscopy. Our experiments reveal that hydrogen is continuously released from titanium hydride as the temperature is gradually increased from 300 to 700 °C. Hydrogen is released in two transitions: TiH1.924→TiH1.5/TiH1.7 between 300 °C and 400 °C and TiH1.5/TiH1.7→α-Ti between 400 °C and 600 °C. In the lower temperature range between 300 °C and 550 °C the rate of hydrogen release is slow, but the decomposition rate increases sharply above 550 °C. The XRD patterns obtained in air and under vacuum indicate that the surface oxide layer can deter hydrogen release. The pressure change is monitored in real time and the amount of hydrogen released is affected by the processing temperature and holding time. Holding processes at 425 °C, 480 °C, 500 °C, 550 °C, and 600 °C are found to significantly improve the porous structure in the NiTi scaffolds due to the stepwise release of hydrogen. NiTi scaffolds foamed by stepwise release of hydrogen are conducive to the attachment and proliferation of osteoblasts and the resulting pore size also favor in-growth of cells.
氢化钛粉末被用于增强无胶囊热等静压过程中骨科镍钛支架形成过程中的发泡工艺。为了研究其形成机制,我们通过 X 射线衍射(XRD)、热分析(包括热重分析和差示扫描量热法)、能量色散 X 射线光谱和透射电子显微镜,系统地研究了氢化钛在空气、氩气和真空中的热行为和升温过程中氢气的释放。我们的实验表明,随着温度从 300°C 逐渐升高到 700°C,氢化钛中的氢气不断释放。氢气通过两个转变释放:在 300°C 到 400°C 之间 TiH1.924→TiH1.5/TiH1.7,在 400°C 到 600°C 之间 TiH1.5/TiH1.7→α-Ti。在 300°C 到 550°C 的较低温度范围内,氢气释放速度较慢,但在 550°C 以上,分解速度急剧增加。在空气和真空中获得的 XRD 图谱表明,表面氧化层可以阻止氢气释放。实时监测压力变化,氢气的释放量受处理温度和保温时间的影响。在 425°C、480°C、500°C、550°C 和 600°C 下进行保温处理,发现由于氢气的分步释放,NiTi 支架的多孔结构得到显著改善。通过分步释放氢气形成的 NiTi 支架有利于成骨细胞的附着和增殖,并且所得的孔径也有利于细胞的向内生长。