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Synthesis of bioactive TiO2 thick films on titanium substrates by plasma electrolytic oxidation
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電漿電解氧化法（plasma electrolytic oxidation, PEO）是自1930年代就有的技術，但是近年來，隨著輕金屬材料在工業界、航太工程與生醫材料上的應用越來越廣，電漿電解氧化法成為越來越常被應用在輕金屬表面改質的技術。電漿電解氧化法是一種設備簡便、成膜迅速的製程，在適當的電解溶液環境中，加上數百伏特的外加電壓，金屬的表面會產生局部的電漿與火花反應，短時間內，金屬的表面便形成緻密且多孔的氧化層，同時也能將溶液中的元素併入氧化層當中。此氧化層具有極佳的接合強度、大的接觸面積、耐高溫、高強度、高磨耗、抗腐蝕等優良的特性，相當適合生醫上的使用。
在鈦金屬上以醋酸鈣（Ca(CH3COO)2）、β-甘油磷酸鈉（C3H7Na2O6P•5H2O）為電解液進行電漿電解氧化反應，可以在試片上迅速的被覆二氧化鈦膜，且膜層當中有鈣與磷的併入，經過適當的熱處理，可以成為具有高度生醫活性的試片。本實驗使用田口實驗法，以電解液組成、反應時間、反應電壓為因子，各因子在三種水準下分別執行電漿電解氧化試驗，然後量測試片的粗糙度與銳鈦礦相的相對強度，使用田口實驗法的L9直交表找出以生醫適用性為目的的優選反應參數。以此參數進行電漿電解氧化反應，反應後的試片不需要經過高溫水熱處理，室溫下，將試片浸泡在2M的K2HPO4水溶液下10分鐘，再以此浸泡過的試片進行活體外試驗。活體外試驗是使用模擬人體體液（Simulate body fluid, SBF）浸泡試片1-15天，再分析其性質；試片浸泡SBF 3天後，在試片的表面即有氫氧基磷灰石的生成，7天後試片的表面覆滿氫氧基磷灰石。以FE-SEM、XRD分析試片的微結構與組成，並以傅立葉轉換紅外線光譜儀（FT-IR）分析試片的化學組成。
Titanium, a kind of light metal material, is widely applicated in biomedical field, mainly because of good bio-compatibility and chemical stability. Generally various applications of titanium depend on the characteristic such as surface property, oxide structure, thickness of oxide layer and chemical composition. The oxide layer of the material surface or coated hydroxyapatite of titanium often was modifies for the purpose of usage in implantation. By this kind modification, not only the bonding process could be strength between the titanium materials and also speed up the osteointegration of bone tissue.
Plasma electrolytic oxidation (PEO) is an oxidation technology that was developed since the 1930s. Light metal material was more and more broadly used in the different industries, including material industry, aerospace engineering and biomedical industry. Thus the application of PEO in light metal surface modification technology was widely used recently.
PEO is a fast film-forming process with simple device. Metal surface could induce local spark and plasma reactions by hundreds voltage in suitable electrolytic solution. Under this condition, the formation of dense and porous oxide layer was induced shortly on metal surface. This oxide layer has excellent characteristics of good bonding strength, large contact area, high temperature tolerance, high durability, better corrosion resistance and so on. It is very suitable in biomedical field due to its excellent properties.
Titanium metal using the calcium acetate (Ca(CH3COO)2), β-glycerophosphate (C3H7Na2O6P • 5H2O) as the electrolyte for plasma electrolytic oxidation, and we can rapidly get specimens which coated with titanium dioxide films dope calcium and phosphorous. Greatly bioactivite materials will complete after suitable thermal process. In this study, we perform PEO process under three levels of each factor (electrolyte composition, reaction time, reaction voltage factor) by using Taguchi method, and measured roughness of the sample and the relative intensity of anatase. We implement PEO reaction by some optimal reaction parameters which from L9 orthogonal array table in Taguchi method and is for the purpose of applicability of biomedical. Specimen after the reaction without under hydrothermal treatment, the sample immersed in 2 M of K2HPO4 solution for 10 minutes, and then soaked specimen is performed some in vitro tests. In vitro studies are analyzing the specimens immersed in Simulate body fluid (SBF) for 1-15 days. Hydroxyapatite-containing coatings on titanium substrates were formed after 3 days' immersion. And the sample surface covered with hydroxyapatite after 7 days' immersion. The microstructures and compositions of the obtained films were analyzed by field-emission scanning electron microscopy and X-ray diffraction. The chemical states were also analyzed by Fourier transform infrared spectroscopy.
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