Dupraz A, Nguyen T P, Richard M, Daculsi G, Passuti N
Laboratoire de recherche sur les Tissus Calcifíes et les Biomatériaux UPRES EA 2159, Nantes, France.
Biomaterials. 1999 Apr;20(7):663-73. doi: 10.1016/s0142-9612(98)00222-1.
An injectable composite material based on biphasic calcium phosphate (BCP) and a nonionic cellulose ether has been elaborated for use in percutaneous surgery for spine fusion. This paper reports the characterization results of this material by spectroscopic techniques including X-ray diffraction (XRD), infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) fitted with an energy dispersive X-Ray analysis system and high-resolution transmission electron microscopy (HR-TEM). From FTIR and XPS results, it was observed that the adhesion between the polymer and the ceramic might be insured by oxygen bridging developed through an ionic bonding between calcium ions and (C-O) groups of the polymer. Moreover, XPS showed attraction of Ca2+ ions in the polymer matrix, while the ceramic surface was modified in a HPO4(2-) -rich layer. These results suggest a possible dissolution/precipitation process at the interface ceramic/polymer. HR-TEM observations supported this hypothesis, showing a light contrasted fringe at the surface of the ceramic grains in the composite paste. As well, changes in the XRD spectra could indicate a small decrease in the crystal size of the BCP powder through the contact to polymer solution. In addition, SEM observation showed a decrease of the initial BCP granulometry. Aggregates of 80-200 microm seemed to be mostly dissociated in micrograins. The ceramic grains were coated with and bonded between each other by the polymer matrix, which acted as spacer in between the ceramic grains, creating a macroporous-like material structure.
一种基于双相磷酸钙(BCP)和非离子纤维素醚的可注射复合材料已被研制出来,用于脊柱融合的经皮手术。本文报道了通过光谱技术对该材料的表征结果,这些技术包括X射线衍射(XRD)、红外光谱(FTIR)、X射线光电子能谱(XPS)、配备能量色散X射线分析系统的扫描电子显微镜(SEM)和高分辨率透射电子显微镜(HR-TEM)。从FTIR和XPS结果可以观察到,聚合物与陶瓷之间的粘附可能是通过钙离子与聚合物的(C-O)基团之间的离子键形成的氧桥来保证的。此外,XPS显示聚合物基质中Ca2+离子的吸引力,而陶瓷表面在富含HPO4(2-)的层中发生了改性。这些结果表明在陶瓷/聚合物界面可能存在溶解/沉淀过程。HR-TEM观察结果支持了这一假设,显示复合糊剂中陶瓷颗粒表面有浅色对比条纹。同样,XRD光谱的变化可能表明BCP粉末通过与聚合物溶液接触,其晶体尺寸略有减小。此外,SEM观察显示初始BCP粒度减小。80-200微米的聚集体似乎大多解离成微颗粒。陶瓷颗粒被聚合物基质包覆并相互粘结,聚合物基质在陶瓷颗粒之间起到间隔作用,形成了类似大孔的材料结构。