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牙种植体系统的表面改性实验研究
Experimental Study on Surface Modification of Dental Implant System
【作者】 张哲;
【导师】 蔺增;
【作者基本信息】 东北大学 , 化工过程机械, 2014, 硕士
【摘要】 目前牙种植体修复技术在口腔医学领域的应用已越来越普遍,金属钛是种植体系统最为常用的材料。钛是一种惰性金属材料,生物活性较差,在植入颌骨内后容易被一层包囊纤维膜所包绕,在骨整合过程中缺乏主动性,导致骨结合时间长,初期稳定性及长期成功率差,同时纯钛本身硬度较低、疲劳强度和耐磨性能较差,导致钛种植体在服役过程中容易出现基台紧固螺钉松动、连接螺纹点蚀、磨损和腐蚀失效,大大降低种植体系统的可靠性和服役寿命。本文的工作主要分为三部分:在真实种植体表面制备TiOx薄膜并进行动物实验,以及对经喷砂酸蚀处理的钛片进行等离子体氧化处理并进行退火处理和碱液处理,最后在医用纯钛表面制备DLC薄膜。旨在研究以上两种表面改性方法在钛种植体外螺纹表面生物活性上的可行性,以及实际改善紧固螺钉螺纹机械性能。利用RF-PECVD法,对经喷砂酸蚀处理的真实种植体进行等离子体氧化处理。动物实验扭出数据和扭出后SEM检测显示,种植体经喷砂酸蚀和等离子体氧化处理后,表面骨结合力、骨细胞黏附、生长和增殖情况良好,生物活性优于未经等离子体氧化处理的SLA种植体。利用RF-PECVD法,以表面接触角为评价依据对工艺参数进行了优化,发现在本实验条件下,以Ar/O2流量比5sccm/5sccm、射频功率200W、直流偏压-400V、氧化时间1h、工作压力6.5pa的工艺条件制备获得的样品具有接触角接近0°的超亲水表面。SEM观察样品表面形貌发现,等离子体氧化处理在原始表面原位生长了氧化薄膜,保持了由喷砂酸蚀处理获得的多孔嵌套结构。在等离子体氧化基础上进行碱液处理和退火处理,发现碱液处理能明显提高TiOx薄膜润湿性长期稳定性。本文利用RF-PECVD法在医用纯钛表面沉积了DLC薄膜。通过Raman测试数据分析了不同工艺条件制备的DLC薄膜的结构成分,发现在本实验条件下,当Ar/CH4流量比10sccm/15sccm、射频功率300W、直流偏压-300V、沉积时间1h、工作压力7pa时,薄膜中I(D)/I(G)最低;SEM观察表明薄膜致密、平滑、均匀性较好,可作为医用纯钛表面的承载抗磨涂层。
【Abstract】 The application of dental implant restoration technique has been more and more common in the field of stomatology and titanium is the most commonly used material for implant system. However, as a kind of inert metal material, pure titanium is short of initiative in the osseointegration process. These defects greatly reduce the reliability and service life of the implant system. Meanwhile, the pure titanium implant system has a higher risk of abutment screw loosening because of its own low hardness, fatigue strength and wear-resisting performance. This thesis consists of three parts:Plasma oxidation on implant and animal experiment. Depostion of plasma oxidation on SLA titanium with annealing treatment and alkali liquor. diamond-like carbon film on medical titanium. The research mainly aims at improving the mechanical properties and biological activity of the titanium used on dental implant through these two surface modification methods.In this paper, the implant deal with SLA and plasma oxidated by using RF-PECVD technology. Animal twisted into data and twisted into SEM testproved that plasma oxidation treatment can make the SLA titanium sample with better biological activity.The SLA titanium was plasma oxidated by using RF-PECVD technology and the process parameters were optimized by evaluating the surface contact angle. Super-hydrophilic surface, on which the contact angle would approach 0°, can be achieved with the optimum technology parameters as followed:Ar/O2=5sccm/5sccm,200W RF power,-400V DC bias voltage 1 hour oxidation time and 6.5 working stress. SEM observation showed that the plasma oxidation in-situ formed a layer of titanium oxide on the original surface, but didn’t change the porous morphology obtained by SLA treatment. Based on plasma oxidation on the treatment and annealing treatment, found that the alkali liquor can obviously increase the TiOx thin film wettability long-term stability.In this paper, the DLC films were diposited on surface of medical titanium. The composition of DLC films obtained by different process conditions was analyzed by contact angle test. The lowest content of I(D)/I(G) bondings was found in the film obtained with the optimum technology parameters as followed:Ar/CH4=10sccm/15sccm,300W RF power,-300V DC bias voltage,1 hour deposition time and 7pa work stress. SEM observation demonstrated that the DLC film is smooth, homogeneous and compact. Therefore, it can be used as bearing and wear-resisting coating on surface of titanium implant.
【Key words】 dental implant; medical pure titanium; animal experiment; plasma oxidation; DLC film; wettability;