高功率磁控濺鍍氧化鋅鉭薄膜於電漿電解氧化純鈦之抗菌性及生物相容性之研究

Antibacterial properties and biocompatibility of Ta-Zn-O coatings on plasma electrolytic oxidation of pure titanium by high power impulse magnetron sputtering

林宜君(Yi-Jyun Lin)

指導教授 ： 張銀祐

國立虎尾科技大學/工程學院/機械與電腦輔助工程系碩士班/碩士(2017年)

摘要

本研究運用電漿電解氧化(Plasma Electrolytic Oxidation, PEO)在純鈦(Pure Ti)試片上形成的均勻多孔氧化鈦(TiO2)表面，再使用濺鍍系統調整不 同靶功率製備不同鋅含量的氧化鋅鉭(Ta-Zn-O)薄膜。電漿電解氧化法(PEO) 以醋酸鈣{Ca(CH3COO)2·H2O}加上甘油磷酸鈣(C3H7CaO6P·H2O)作為電解液。期使透過電漿電解氧化後，再利用高功率磁控濺鍍系統(High Power Impulse Magnetron Sputtering, HIPIMS )製備五氧化二鉭(Ta2O5)薄膜會有良好的細胞生物相容性以及抗菌性。本研究使用高功率單極脈衝濺鍍系統及射頻濺鍍系統(Radio frequency sputtering, RF)，選用之靶材有純鉭(Ta)、純 鋅(Zn)與氧化鋅(ZnO)，通以氧氣(O2)反應氣體，製備不同成分之氧化鋅鉭 薄膜。再分別以金黃色葡萄球菌(Staphylococcusaureus, S.a)、伴放線菌放線桿菌(Actinobacillusactinomycetemocomitans, A.a)、人體骨母細胞(human osteosarcoma cell, MG-63)與人體皮膚纖維母細胞(human skin fibroblast, SKF)分析薄膜之抗菌性與生物相容性。
本研究使用X光繞射儀( XRD)、X光電子光譜儀(XPS)與場發射掃描式 電子顯微鏡(FE-SEM)分析所製備之薄膜之晶相微結構與化學鍵結態。選用 體外MTT分析細胞活性，且觀察試片於人體皮膚纖維母細胞(SKF)與人體骨母細胞(MG-63)之細胞黏附形態影響以及生物相容性。抗菌性實驗藉由 Syto9螢光染色法觀察金黃色葡萄球菌(Staphylococcus aureus)及伴放線菌放 線桿菌(Actinobacillusactinomycetemocomitans)之細菌存活率。
研究結果顯示五氧化二鉭(Ta2O5)薄膜較其他試片中更具有親水性質。 MTT細胞活性測試結果顯示五氧化二鉭(Ta2O5)薄膜具有最佳之的SKF細胞 活性，抗菌實驗顯示適當Zn含量Ta-Zn-O(鋅含量=4.36 at.%)薄膜擁有最佳之抗菌性。

關鍵字

電漿電解氧化 ； 物理氣相沉積 ； 五氧化二鉭 ； 氧化鋅 ； 生物相容性

並列摘要

The surface modification of biomaterials with better biocompatibility and antibacterial feature has been a challenge for many years. Plasma electrolytic oxidation (PEO) is a rising technology which can produce porous surface for cell adhesion and improves the biocompatibility for further implantation. Tantalum pentoxides (Ta2O5) and zinc oxides (ZnO) have been used as the material of implants due to their good cell biocompatibility and antibacterial property on the microorganisms.In this study, a pre-treatment of surface modification on titanium (Ti) substrates has been made by PEO. Porous oxide layers formed, and Ta-Zn-O films were then deposited onto the porous surface of Ti substrates by using twin-gun high power impulse magnetron sputtering (HIPIMS) and Radio Frequency (RF) sputtering.This study aims to obtain Ta-Zn-O films with different zinc contents by adjusting the zinc target power through the sputtering system. Pure tantalum (Ta), zinc (Zn) and zinc oxide (ZnO) were selected as the target materials. Antibacterial properties and biocompatibilities were analyzed through Staphylococcusaureus(S.a), Aggregatibacteractinomycetemcomitans(A.a), human osteosarcoma cell (MG-63) and Human Skin Fibroblast (SKF).
The surface morphology, crystal structure, and bonding state of the films were identified by scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). An in vitro MTT method was used to analyze cell activities, where the influence of cell adhesion morphology and biocompatibility of the specimen on the human skin fibroblast and human osteosarcoma cell(MG-63) were observed. A Syto9 fluorescent staining method was used to observethe survivalrate of Staphylococcus aureus and Aggregatibacteractinomycetemcomitans in the antibacterial tests.
The results showed that the Ta2O5 film had the most hydrophilic effect among thePEO-treated and coated specimens.The MTT cell activity test results showed that the Ta2O5 film had the optimal SKF cell activity.The Ta-Zn-O film containing 4.36 at.% of Zn the best antibacterial property.

並列關鍵字

Plasma Electrolytic Oxidation ； Physical vapor deposition ； tantalum oxide ； Zinc oxide ； Biocompatibility

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