Wolke J G, van der Waerden J P, de Groot K, Jansen J A
University of Nijmegen, Department of Oral Function and Prosthetic Dentistry, Dental School, The Netherlands.
Biomaterials. 1997 Mar;18(6):483-8. doi: 10.1016/s0142-9612(96)00164-0.
The stability of radiofrequency (RF) magnetron sputtered calcium phosphate was studied under cyclically loaded conditions. The coatings were deposited on titanium bars and tested in either dry or wet conditions X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis and Fourier transform infrared (FTIR) spectroscopy were used to characterize the as-sputtered and tested coatings. XRD demonstrated that the amorphous structure after annealing at 650 C changed into a crystalline apatite structure. The residual stresses were determined by the XRD cos 2 i/i method. These residual film stresses were influenced by the coating conditions and the crystalline sputtered coating showed the presence of compressive stresses. SEM demonstrated that, after cyclic loading conditions in air, the crystalline sputter-coated Ti-6A1-4V bars showed a partial coating loss. Furthermore, in wet conditions (simulated body fluid) only the heat-treated sputter-coated bars appeared to be stable. On the other hand, the amorphous coating only showed signs of delamination in the more highly stressed regions, while in the less stressed regions a Ca-P precipitate was formed. On the basis of these results we conclude that calcium phosphate coatings subjected to cyclic loading conditions show an important difference in fatigue behaviour when tested in either dry or wet conditions.
在循环加载条件下研究了射频(RF)磁控溅射磷酸钙的稳定性。将涂层沉积在钛棒上,并在干燥或潮湿条件下进行测试。使用X射线衍射(XRD)、扫描电子显微镜(SEM)、能量色散X射线(EDX)分析和傅里叶变换红外(FTIR)光谱对溅射态和测试后的涂层进行表征。XRD表明,650℃退火后的非晶结构转变为结晶磷灰石结构。残余应力通过XRD cos 2ψ/ψ方法测定。这些残余薄膜应力受涂层条件影响,结晶溅射涂层显示存在压应力。SEM表明,在空气中循环加载条件后,结晶溅射涂层的Ti-6Al-4V棒出现部分涂层损失。此外,在潮湿条件下(模拟体液),只有经过热处理的溅射涂层棒似乎是稳定的。另一方面,非晶涂层仅在应力较高的区域出现分层迹象,而在应力较低的区域形成了Ca-P沉淀。基于这些结果,我们得出结论,在循环加载条件下的磷酸钙涂层在干燥或潮湿条件下测试时,疲劳行为存在重要差异。