本文選題：多孔NiTi合金　切入點：溶膠-凝膠法　出處：《華南理工大學》2011年博士論文

【摘要】：本論文探索采用溶膠-凝膠法對多孔NiTi合金進行了生物活性涂層表面處理,并采用物相分析(XRD)和顯微表征(SEM與EDS)方法研究了涂層的基本性質;對表面涂層處理后多孔NiTi合金在Hanks’溶液(HBSS)中的腐蝕特性、在模擬體液(SBF)中的Ni離子釋放行為、涂層在Tris緩沖溶液中的穩(wěn)定性以及涂層的生物活性等進行了系統表征;研究了硫酸慶大霉素在多孔NiTi合金表面負載后藥物釋放特性;并對經HA涂層處理的多孔NiTi合金的生物相容性進行了初步的評價。 首次采用溶膠-凝膠法結合浸漬提拉工藝在多孔NiTi合金表面制備出了結構均一的銳鈦礦型TiO_2涂層,并在溶膠中添加聚乙二醇(PEG)作為造孔劑進而在多孔NiTi合金表面制備出內層致密、外層多孔的TiO_2復合涂層。SEM分析結果表明,TiO_2涂層均勻地覆蓋了多孔NiTi合金基體的外表面以及孔的內表面。Hanks’溶液中的陽極極化曲線結果表明,與未處理的多孔NiTi合金相比,具有致密TiO_2涂層的多孔NiTi合金的耐腐蝕性能有了顯著提高;而多孔TiO_2復合涂層進一步增大了多孔NiTi合金的實際表面積,提高了材料表面的生物活性。 以亞磷酸三乙酯和硝酸鈣為前驅體采用溶膠-凝膠法結合浸漬提拉工藝在多孔NiTi合金表面制備了均勻的羥基磷灰石(HA)涂層。涂層覆蓋了多孔NiTi基體材料的外表面以及孔的內表面,涂層厚度為幾個微米;涂層截面的SEM觀察和涂層的EDS分析結果表明,多孔NiTi合金中孔的內表面HA涂層的厚度大于外表面涂層的厚度。在Tris溶液中的浸泡實驗結果顯示溶膠-凝膠HA涂層具有良好的穩(wěn)定性。經過HA涂層處理后,不同孔隙率的多孔NiTi合金在SBF溶液中的Ni離子釋放速率大大降低。在FCS溶液中浸泡實驗結果表明,HA涂層誘導磷灰石的生長能力獲得增強,其中多孔NiTi合金中孔的內表面由于具有一定的粗糙度而使鈣磷晶體生長速度更快。 采用混合溶膠法在多孔NiTi合金表面制備出了多孔TiO_2/HA/TiO_2復合涂層,并研究了硫酸慶大霉素在多孔NiTi合金表面負載后藥物釋放特性。實驗結果表明,多孔NiTi合金中的特殊孔道結構為藥物的可控釋放創(chuàng)造了有利條件;藥物釋放分三個階段:第一階段釋放速率較快;第二階段釋放速率平穩(wěn);第三階段雖然釋放速率增大,但釋放總量并不大。 采用細胞培養(yǎng)的方法對多孔NiTi合金表面HA涂層的生物相容性進行了初步的評價。細胞相容性實驗結果表明,經過HA涂層處理后,細胞在多孔NiTi合金表面吸附良好,且合金的孔隙內部細胞粘附性能更好。與未經表面處理的多孔NiTi合金相比較,HA表面的成骨細胞的增長率更大,顯示更好的細胞相容性。與對照組純Ti試樣相比較,成骨細胞的在多孔NiTi合金表面的功能表達與其增殖率表現出不一致性,說明多孔NiTi合金的特殊孔隙結構是成骨細胞具有良好活性的根本原因。血液相容性實驗結果表明,經過HA涂層處理后多孔NiTi合金的溶血率為0.3%,血液相容性良好,不會引起急性溶血作用。
[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.

【學位授予單位】：華南理工大學
【學位級別】：博士
【學位授予年份】：2011
【分類號】：TG174.44

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