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钛及钛合金表面多孔结构的构建与润湿性研究
Study of Porous Structure Preparation and Wettability on Titanium and Titanium Alloy Surfaces
【作者】 王永;
【导师】 李建昌;
【作者基本信息】 东北大学 , 流体机械及工程, 2011, 硕士
【摘要】 润湿性是固体材料和薄膜表面的一个重要的性质,由表面材料的化学组成和微观结构共同决定。具有超疏水和超亲水性能的特殊润湿性表面是目前研究领域的研究热点。钛及钛合金种植体的生物相容性与其表面润湿性有着直接的关系,多孔钛种植体表面不仅能增强与骨组织的机械嵌合,其表面的氧化层还具有良好的防腐蚀和生物活性高等优点。本文首先用喷砂酸蚀法(SLA)对钛及钛合金表面进行了粗化处理,制备出具有微米-纳米双微观孔洞结构的超亲水表面,并对酸腐蚀工艺进行了对比研究,发现H2SO4/HCl酸蚀和HF/HNO3与H2SO4/HC1的双重酸腐蚀均能得到微米-纳米级的多孔表面,而TA4较TC4更容易腐蚀。在SLA法粗化处理的钛及钛合金表面,用等离子体氧化的工艺,制备具有超亲水性能的氧化钛表面。发现表面亲水性能随自偏压的增加先减小后增加,随处理时间的增加而减小,未发现与气体流量的改变有关。在360V自偏压、20min处理时间和1sccm氧气流量时能到超亲水效果的锐钛矿二氧化钛表面。成骨细胞黏附和增殖实验表明等离子体氧化工艺相对于氧化后退火处理具有更好的生物活性。最后尝试用十二烷基三氯硅烷和分子自组装法在粗糙的氧化钛表面生长疏水表面,最大角度可达120°,并利用等离子体处理和紫外光照射成功实现了表面由超亲水到疏水之间的转换。总之,本文从构建对表面润湿性具有直接影响的微观结构开始,重点研究SLA法,等离子体处理与钛及钛合金表面超亲水性能的关系,并简单尝试了疏水表面的制备以及润湿类型的控制。得出了一些有益的经验与结果,为后续的深入研究奠定了一定的基础。
【Abstract】 Wettability is an important property of the solid material and film surfaces and it is well known that surface wettability is not only dependent upon their chemical compositions but also closely related to the micro/nano-structures on their surfaces. Surface with special wettability including superhydrophobic and superyhydrophilic surfaces is a new hotspot at present. Furthermore, there was direct relation between the biocompatibility of titanium and titanium alloy implant and its surfaces wettability. Titanium implant surface with porous structure both have high mechanical interlocking strength and biological activity.Firstly, micro/nano-structures surfaces with superyhydrophilic on TC4and TA4are achieved by using sandblast-acid etching. By comparatively study on different processes we find that porous surface micro/nano-structures with superyhydrophilic can achieved by etching in H2SO4/HCl solution or HF/HNO3&H2SO4/HCl double solution. TA4is more corrosive rather than TC4.Secondly, titanium oxide surfaces are achieved on SLA surfaces by using plasma oxidation base on PECVD vacuum film-plating machine. The water contact angle (CA) of this surfaces begin to increase and then decrease with increasing the self-bias voltage, and decrease with increasing treat time but no relation to the change of oxygen flow. Suphyhydrophilic TiO2(Anatase) surface can achieved while the self-bias voltage is360V, treat time is20min and oxygen flow is1sccm. Ahesion and proliferation experiments of osteogenic cells showed that biological of plasma treated sample is more activie than annealing sample.Finally, we attempt to prepare superhydrophobic surface by using self-assembled monolayers (SAMs), the maximal CA is120°while superyhydrophilic titanium oxide surfaces with micro/nano-structures as substrate and dodecyltrichlorosilane as film material. Superhydrophilic and hydrophobic surface can under control transform by UV light, plasma treat and darkroom placed. Above all, this paper begins in creating micro/nano-structures which is very important to surface with special wettability. Mainly research is the effects of the SLA and plasma oxidation on wettability of titanium and titanium alloys surfaces. hydrophobic surface is achieved and the types of wettability can be control. We obtain some interesting and useful results.It laid the some foundation for subsequent in-depth study.
【Key words】 wettability; superyhydrophilic; SLA; plasma oxidation; titanium implant;