多孔NiTi合金表面溶胶凝胶法制备生物活性涂层及相关性能研究

发布时间：2018-04-08 08:02

  本文选题：多孔NiTi合金　切入点：溶胶-凝胶法　出处：《华南理工大学》2011年博士论文

【摘要】：本论文探索采用溶胶-凝胶法对多孔NiTi合金进行了生物活性涂层表面处理,并采用物相分析(XRD)和显微表征(SEM与EDS)方法研究了涂层的基本性质;对表面涂层处理后多孔NiTi合金在Hanks’溶液(HBSS)中的腐蚀特性、在模拟体液(SBF)中的Ni离子释放行为、涂层在Tris缓冲溶液中的稳定性以及涂层的生物活性等进行了系统表征;研究了硫酸庆大霉素在多孔NiTi合金表面负载后药物释放特性;并对经HA涂层处理的多孔NiTi合金的生物相容性进行了初步的评价。 首次采用溶胶-凝胶法结合浸渍提拉工艺在多孔NiTi合金表面制备出了结构均一的锐钛矿型TiO_2涂层,并在溶胶中添加聚乙二醇(PEG)作为造孔剂进而在多孔NiTi合金表面制备出内层致密、外层多孔的TiO_2复合涂层。SEM分析结果表明,TiO_2涂层均匀地覆盖了多孔NiTi合金基体的外表面以及孔的内表面。Hanks’溶液中的阳极极化曲线结果表明,与未处理的多孔NiTi合金相比,具有致密TiO_2涂层的多孔NiTi合金的耐腐蚀性能有了显著提高;而多孔TiO_2复合涂层进一步增大了多孔NiTi合金的实际表面积,提高了材料表面的生物活性。 以亚磷酸三乙酯和硝酸钙为前驱体采用溶胶-凝胶法结合浸渍提拉工艺在多孔NiTi合金表面制备了均匀的羟基磷灰石(HA)涂层。涂层覆盖了多孔NiTi基体材料的外表面以及孔的内表面,涂层厚度为几个微米;涂层截面的SEM观察和涂层的EDS分析结果表明,多孔NiTi合金中孔的内表面HA涂层的厚度大于外表面涂层的厚度。在Tris溶液中的浸泡实验结果显示溶胶-凝胶HA涂层具有良好的稳定性。经过HA涂层处理后,不同孔隙率的多孔NiTi合金在SBF溶液中的Ni离子释放速率大大降低。在FCS溶液中浸泡实验结果表明,HA涂层诱导磷灰石的生长能力获得增强,其中多孔NiTi合金中孔的内表面由于具有一定的粗糙度而使钙磷晶体生长速度更快。 采用混合溶胶法在多孔NiTi合金表面制备出了多孔TiO_2/HA/TiO_2复合涂层,并研究了硫酸庆大霉素在多孔NiTi合金表面负载后药物释放特性。实验结果表明,多孔NiTi合金中的特殊孔道结构为药物的可控释放创造了有利条件;药物释放分三个阶段:第一阶段释放速率较快;第二阶段释放速率平稳;第三阶段虽然释放速率增大,但释放总量并不大。 采用细胞培养的方法对多孔NiTi合金表面HA涂层的生物相容性进行了初步的评价。细胞相容性实验结果表明,经过HA涂层处理后,细胞在多孔NiTi合金表面吸附良好,且合金的孔隙内部细胞粘附性能更好。与未经表面处理的多孔NiTi合金相比较,HA表面的成骨细胞的增长率更大,显示更好的细胞相容性。与对照组纯Ti试样相比较,成骨细胞的在多孔NiTi合金表面的功能表达与其增殖率表现出不一致性,说明多孔NiTi合金的特殊孔隙结构是成骨细胞具有良好活性的根本原因。血液相容性实验结果表明,经过HA涂层处理后多孔NiTi合金的溶血率为0.3%,血液相容性良好,不会引起急性溶血作用。
[Abstract]:This paper explore the bioactive coating on the surface of the porous NiTi alloy by sol-gel method, and the phase analysis (XRD) and microscopic characterization (SEM and EDS) method to study the basic properties of the coating; the surface coating treatment of porous NiTi alloy in Hanks solution (HBSS) etching characteristics. In the simulated body fluid (SBF) release behavior of Ni ions, stability of coating in the Tris solution and the bioactivity of the coating were systematically studied characterization; gentamycin sulfate on the surface of porous NiTi alloy loaded drug release properties; and the porous NiTi alloy with HA coating the biocompatibility of a preliminary evaluation.
For the first time by the sol-gel method on the porous surface of NiTi alloy was prepared by anatase TiO_2 coating uniform with dip coating process, and adding polyethylene glycol in sol (PEG) as pore forming agent and the porous surface of NiTi alloy prepared by the dense inner layer of TiO_2 composite coating.SEM analysis results show that the porous outer layer, anode polarization curves of inner surface of.Hanks' TiO_2 coating evenly covering the porous NiTi alloy substrate surface and the hole in the solution. The results showed that compared with the untreated porous NiTi alloy, porous NiTi alloy with dense TiO_2 coating corrosion resistance has been improved significantly; while the porous TiO_2 composite coating to further increase the porous NiTi the actual alloy surface area, improve the surface bioactivity.
With three ethyl phosphite and calcium nitrate as used in the porous surface of NiTi alloy was prepared by dip coating process with homogeneous hydroxyapatite precursor sol gel (HA) coating. Coating on the inner surface of the porous NiTi matrix material covering the outer surface and the hole, the coating thickness is several microns; the results of EDS analysis and SEM observation the coating section shows that the inner surface of the HA coating of porous NiTi alloy in hole is greater than the thickness of the outer surface of the coating thickness. The soaking experiments in Tris solution showed that HA coating has good stability. After HA coating treatment, the release rate of Ni ion in porous NiTi alloy with different porosity in SBF the solution is greatly reduced. In FCS solution immersion test results showed that the growth ability of HA induced apatite coating was enhanced, the inner surface of porous NiTi alloy in the hole because it has a certain The roughness of the crystal makes the calcium and phosphorus crystals grow faster.
The mixed sol method on porous surface of NiTi alloy was prepared by porous TiO_2/HA/TiO_2 composite coating, and studied on the surface of porous NiTi alloy of gentamicin sulfate loaded drug release properties. The experimental results show that the special pore structure of porous NiTi alloy in creating favorable conditions for controlled drug release; drug release is divided into three stages: first the second stage stage faster release rate; stable release rate; the third stage although the release rate increased, but the total release is not large.
By the method of cell culture on the coating of porous NiTi alloy HA surface biocompatibility was evaluated. The cell compatibility experiment results show that after HA coating treatment, cells adsorbed on the surface of a porous NiTi alloy, and alloy inner pore cell adhesion performance is better. With the porous NiTi alloy surface treatment. Compared with the surface of HA osteoblast growth rate, showed better biocompatibility. Compared with control group, pure Ti samples, osteoblast function in surface expression of porous NiTi alloy and its proliferation rate showed no consistent, illustrate the special pore structure of porous NiTi alloy is the fundamental cause bone cells have good activity. The blood compatibility test results show that after HA hemolysis after coating of porous NiTi alloy was 0.3%, with good blood compatibility, does not cause acute hemolysis.

【学位授予单位】：华南理工大学
【学位级别】：博士
【学位授予年份】：2011
【分类号】：TG174.44

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