Yoshinari M, Hayakawa T, Wolke J G, Nemoto K, Jansen J A
Department of Dental Materials Science and Oral Health Science Center, Tokyo Dental College, Japan.
J Biomed Mater Res. 1997 Oct;37(1):60-7. doi: 10.1002/(sici)1097-4636(199710)37:1<60::aid-jbm8>3.0.co;2-h.
This study evaluated the effect of rapid heating with infrared radiation on the physico-chemical and morphological properties of radio frequent (RF) magnetron-sputtered calcium phosphate (Ca-P) coatings. About 2.5 microm thick Ca-P coatings were deposited on titanium disks and cylinders. These specimens were left untreated or were heat treated by infrared radiation at 300, 400, 500, 600, and 700 degrees C for 4, 7, 11, 17, and 24 s. Subsequently, the specimens were immersed in simulated body fluid (SBF) for 1 day, 1 week, and 5 weeks. X-ray diffraction measurements showed that heating at 500 degrees C or higher resulted in an increase of coating crystallinity. In addition, FT-IR measurements revealed the appearance of OH peaks in the spectra of samples treated at 500-700 degrees C. Electron probe microanalysis showed that after 5 weeks of immersion about 40-50% of the coatings heat treated at 500 and 600 degrees C was maintained. The coatings heat treated at 700 degrees C showed no dissolution at all. On the other hand, as-coated and 300 degrees C treated films were dissolved within 1 day. Scanning electron microscopy of the samples showed that directly after heat treatment no apparent cracks were present in the coatings. On the basis of these findings, we conclude that rapid heating with infrared radiation around 600 degrees C is the best heat treatment for RF magnetron-sputtered coatings.
本研究评估了红外辐射快速加热对射频(RF)磁控溅射磷酸钙(Ca-P)涂层的物理化学和形态学性能的影响。在钛盘和圆柱上沉积了约2.5微米厚的Ca-P涂层。这些样品未经处理,或在300、400、500、600和700摄氏度下用红外辐射热处理4、7、11、17和24秒。随后,将样品浸入模拟体液(SBF)中1天、1周和5周。X射线衍射测量表明,在500摄氏度或更高温度下加热会导致涂层结晶度增加。此外,傅里叶变换红外光谱(FT-IR)测量显示,在500-700摄氏度下处理的样品光谱中出现了OH峰。电子探针微分析表明,浸泡5周后,在500和600摄氏度下热处理的涂层约有40-50%得以保留。在700摄氏度下热处理的涂层完全没有溶解。另一方面,未处理和在300摄氏度下处理的薄膜在1天内就溶解了。对样品的扫描电子显微镜观察表明,热处理后涂层中没有明显的裂纹。基于这些发现,我们得出结论,对于RF磁控溅射涂层,600摄氏度左右的红外辐射快速加热是最佳的热处理方式。