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中文题名:

 Ti6Al4V合金表面Si-N(O)薄膜的制备及性能研究    

姓名:

 黄菊    

学号:

 0000063270    

论文语种:

 中文    

公开时间:

 公开    

学校:

 西南交通大学    

院系:

 材料科学与工程学院    

专业:

 材料科学与工程学院    

第一导师姓名:

 杨苹    

第一导师单位:

 西南交通大学    

完成日期:

 2008-11-10    

答辩日期:

 2008-11-18    

外文题名:

 SYNTHESIS AND PROPERTY INVESTIGATION OF Si-N(O) THIN FILMS ON THE SURFACE OF Ti6Al4V ALLOY    

中文关键词:

 Si-N(O) 薄膜 ; XPS ; 力学性能 ; 血液相容性    

中文摘要:

随着人口老龄化日益加速,心血管疾病发生率不断上升,对人工心脏瓣膜、血管支架等的需求量不断增加。而心血管植入材料的耐用性和抗血栓能力一直是研究者研究开发新材料面临的关键问题。表面改性(表面覆膜)技术是改善金属生物材料血液相容性的常用方法。前期研究表明Si-N(O)系薄膜的抗凝血性能可与低温热解碳(LTIC)相比,可尝试将该薄膜用作生物医用金属材料的表面改性。
本论文较为系统地研究了Si-N(O)系薄膜的成分、结构、力学性能及血液相容性,并探讨了设备优化和沉积控制对薄膜成分、结构及薄膜性能的影响。最后还对Si-N(O)系薄膜改性钛合金的抗凝血性能做了体内评价。
本文采用脉冲非平衡磁控溅射法,通过设备优化和沉积控制,在Ti6Al4V合金和单晶硅片上制备出具有不同成分、结构和性能的Si-N(O)薄膜。使用X射线光电子能谱(XPS)和傅立叶变换红外吸收光谱(FTIR)对薄膜的成分结构进行了表征。利用AMBIOS XP-2台阶仪测量薄膜厚度,JP-82接触角测量仪检测薄膜亲疏水性。采用HXD-1000 knoop显微硬度仪、WS-97划痕试验机和CSEM球盘摩擦磨损试验机研究了薄膜的机械性能。血小板试验及动物试验用以评价薄膜的抗凝血性能。
通过四轮优化,排除真空室内附件析氧等不利因素,提高本底真空度,明显降低了薄膜中O原子含量。薄膜中N原子含量随N2流量的增加和本底真空度的提高而增加。XPS结构分析表明,N原子含量较低时,Si的键合结构以Si和SiOx(x≤2)键合结构为主,随着N原子含量增加,Si3N4键合结构所占比例明显增加,形成以Si3N4键合结构为主的薄膜。
Si-N(O)薄膜的力学性能结果表明:含氧量低的覆膜样品硬度更大,相应地耐磨性更好。随着N原子含量的增加,薄膜中Si的键合结构逐渐过渡到以Si3N4键合结构为主,有利于覆膜样品硬度的提高,从而改善了薄膜样品的耐磨性。Si-N(O)系薄膜的抗凝血性能与LTIC相当,薄膜差异不大。体内试验证实本试验制备的Si-N(O)薄膜具有一定的抗凝血性能。

外文摘要:

With the population aging accelerated day by day, the incidence of cardiovascular diseases increased and the demand quantity of the artificial heart valve,stent, etc. increased continuously. However, the key problem to be solved is the durability and the anti-thrombus capability of the cardiovascular implant materials to be developed. Surface modification technology is the common method to improve the bloodcompatibility of metallic biomaterials. The preliminary result showed that the anti-thrombus capability of Si-N(O) films was equivalent to Low Temperature Isotropic Pyrolitic Carbon(LTIC), so researchers attempt to use the Si-N(O)films to modify the biomedical metallic materials.
In this paper, the chemical composition, structure, mechanical properties and the blood compatibility of Si-N(O) films were systematical studied, and the effect of equipment optimization and deposition condition on the chemical composition, structure and properties of the films was evaluated. In addition, the in vivo test of the titanium alloy modified by the Si-N(O) films was performed。
Si-N(O) films with different composition, microstructure, mechanical properties were synthesized on Ti6Al4V alloy and  monocrystalline silicon wafer by unbalanced magnetron sputtering technique, by optimazing the equipment and deposition condition. The chemical composition and structure were characterized with X-ray photoelectron spectrometry (XPS) and Fourier transform infrared spectroscopy (FTIR). The films thickness was tested by AMBIOS XP-2 profile meter and the hydrophilic-hydrophobic property was tested by JY-82 contact angle measurement. The mechanical properties were characterized with HXD-1000 microhardness meter, CSEM pin-on-disk wear test apparatus and WS-97 scratch tester. Platelet adhesion and animal experiments were used to evaluate the anticoagulation property of the films.
After four rounds optimization, the O atom content was reduced effectively by taking out the unnecessary accessories and improving vacuum degree. The N atom content was increased with the increasing of N2 flow rate and the decreasing of the background pressure. The analysis of microstructure showed that the bonding structure of Si was dominated by Si and SiO x(x≤2) bonding structure when N atom content was lower and Si3N4 bonding structure in the films was increased significantly to the dominant bonding structure with the increasing of N atom content.
The mechanical result of Si-N(O) films showed that: the films with lower oxygen atom content had bigger composite hardness, and better wear resistance accordingly.. With the increasing of N atom content, more and more Si3N4 bonding structure formed in the films. The formation of Si3N4 bonding structure was beneficial to the film composite hardness, and improved the films wear resistance. The blood compatibility of Si-N(O) films was equivalent to LTIC, but some difference existed among the films. The in vivo test indicated that the Si-N(O) films had certain anticoagulation property.

分类号:

 TB43    

总页码:

 78    

参考文献总数:

 76    

馆藏位置:

 TB43 S 2008    

开放日期:

 2008-12-01    

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