Department of Mechanical and Aerospace Engineering, North Carolina State University, Campus Box 7910, Raleigh, NC 27695, USA.
Acta Biomater. 2009 Nov;5(9):3563-72. doi: 10.1016/j.actbio.2009.05.013. Epub 2009 May 20.
A series of calcium phosphate coatings with graded crystallinity were deposited onto heated titanium substrates using ion beam assisted deposition. The microstructure of the coating was examined using transmission electron microscopy (TEM). The coating thickness was observed to be in a range of 594-694 nm. The degree of crystallinity and microstructural grain size of the coating showed a clear decrease with increasing distance from the substrate-coating interface. Fourier transform infrared spectroscopy (FTIR) confirmed the presence of PO(4)(3-), and X-ray photoelectron spectroscopy (XPS) analysis on the coating top surface showed that the atomic Ca/P ratio was in the range of 1.52+/-0.15 to 1.61+/-0.07. The biological response to the coatings was also evaluated using an osteoblast precursor cell culture test. More cells and a higher integrin expression of cell attachment sites were observed on the coating surface when compared to the control group (blank titanium surface). The pull-off test showed average adhesion strengths at the coating-substrate interface to be higher than 85.12+/-5.37 MPa. Nanoindentation tests indicated that the Young's moduli of all coatings are higher than 91.747+/-3.641 GPa and microhardness values are higher than 5.275+/-0.315 GPa. While the adhesion strength results helped us to identify the best setup for substrate temperature and processing parameters to begin the deposition, the culture test and XPS results helped identifying the optimum parameters for the last stage of deposition. TEM, X-ray diffraction, FTIR and nanoidentation results were used to further evaluate the quality of the coating and optimization of its processing parameters.
采用离子束辅助沉积法在加热的钛基体上沉积了一系列具有分级结晶度的磷酸钙涂层。采用透射电子显微镜(TEM)观察涂层的微观结构。涂层厚度观察到在 594-694nm 的范围内。涂层的结晶度和微观结构晶粒尺寸随着距基底-涂层界面的增加而明显降低。傅里叶变换红外光谱(FTIR)证实了 PO(4)(3-)的存在,并且对涂层顶表面的 X 射线光电子能谱(XPS)分析表明,原子 Ca/P 比在 1.52+/-0.15 至 1.61+/-0.07 的范围内。还通过成骨前体细胞培养试验评估了涂层的生物反应。与对照组(空白钛表面)相比,在涂层表面观察到更多的细胞和更高的细胞附着部位的整联蛋白表达。拉脱试验表明,涂层-基底界面的平均附着强度高于 85.12+/-5.37MPa。纳米压痕试验表明,所有涂层的杨氏模量均高于 91.747+/-3.641GPa,显微硬度值均高于 5.275+/-0.315GPa。虽然附着强度结果有助于确定开始沉积的最佳基底温度和处理参数设置,但培养试验和 XPS 结果有助于确定沉积最后阶段的最佳参数。TEM、X 射线衍射、FTIR 和纳米压痕结果用于进一步评估涂层的质量并优化其处理参数。