電漿電解氧化與高功率脈衝磁控濺鍍氧化鉭及氧化鋅薄膜之細胞相容性與抗菌性研究

Biological characteristic of Ta2O5 and ZnO coated titanium pretreated by plasma electrolytic oxidation

林毅柔(Yi-Jou 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

近年來電漿電解氧化(Plasma Electrolytic Oxidation, PEO)技術由於它可以利用不同的配方在鈦金屬上製備多孔的氧化鈦表面又可以提升耐腐蝕性，所以被廣泛研究用在骨骼、關節、牙科植入物等生物醫學方面，能有效提高植入物與人體的結合。 本研究先以電漿電解氧化技術在生醫級純鈦試片上形成多孔二氧化鈦(TiO2)表面，再使用濺鍍 (Sputtering)沉積氧化鋅(ZnO)、五氧化二鉭(Ta2O5)薄膜在電漿電解氧化前處理的多孔表面上，藉以獲得更好的抗菌性及細胞生物相容性。
本研究使用磷酸鉀(K3PO4)加上氫氧化鉀(KOH)作為電解液來製備多孔氧化鈦(TiO2)層，並運用高功率單極脈衝濺鍍系統(High Power Impulse Magnetron Sputtering, HIPIMS )雙靶濺射，靶材分別為純鉭(Ta)、純鋅(Zn)，通以氧氣(O2)反應氣體在電漿電解氧化處理之二氧化鈦(TiO2)層上沉積氧化二鉭(Ta2O5)薄膜。另運用射頻濺鍍系統(Radio frequency sputtering, RF)使用氧化鋅(ZnO)靶沉積氧化鋅(ZnO)薄膜。再分別以金黃色葡萄球菌(Staphylococcus aureus, 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)分析試片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。以體外MTT分析細胞活性，並觀察試片對人體皮膚纖維母細胞(SKF)與人體骨母細胞(MG-63)之細胞貼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。
　　研究結果顯示經過電漿電解氧化(PEO)前處理的表面會形成多孔二氧化鈦，使薄膜親水性提升，PEO-Ta2O5在所有薄膜試片中最具有親水性質。MTT細胞活性測試結果顯示擁有多孔氧化鈦層之五氧化二鉭試片(PEO-Ta2O5)比單純五氧化二鉭試片(Ta2O5)更具有優異的MG-63細胞相容性。另外抗菌實驗顯示PEO-ZnO試片比未經過PEO前處理之ZnO試片更具有優良之抗菌性。

關鍵字

電漿電解氧化 ； 物理氣相沉積 ； 氧化鉭 ； 氧化鋅 ； 生物相容性

並列摘要

In recent years, plasma electrolytic oxidation (PEO) technology has been widely used in biomedical sciences for bones, joints, and dental implants because it can utilize different formulations for preparation of porous titanium surfaces and increase its corrosion resistance.Thisprocess can effectively increase the fusion of implants and the body. This study hopes to use plasma electrolytic oxidation to form a porous titanium oxide (TiO2) surface on pure titanium samples before deposition of antibacterial oxide films. A sputtering technique (a type of physical vapor deposition method) was used to deposit zinc oxide (ZnO) and tantalum pentoxide (Ta2O5) as films on the porous surface that has been processed with PEO. By this process, we study the mechanical properties and aim to achieve better anti-bacterial properties and cellular biocompatibility.

This study used potassium phosphate (K3PO4) and potassium hydroxide (KOH) as electrolyte solutions for preparation of the porous titanium oxide (TiO2) surface. High Power Impulse Magnetron Sputtering(HIPIMS) was used for the deposition of tantalum pentoxide (Ta2O5) on the PEO treated titanium surface. Radiofrequency sputtering (RF) was used to deposit zinc oxide films. Staphylococcus aureus, Actinobacillusactinomycetemcomitans, human osteosarcoma cells (MG-63), and human skin fibroblasts (SKF) were used to analyze the anti-bacterial properties and biocompatibility of the samples.

　　This study used X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and field emission scanning electron microscopy (FE-SEM) to analyze the crystal microstructure and chemical bonds in the film produced. In vitro MTT assays was used to analyze cellular activities, the effects of the test samples on cell adhesion morphology and biocompatibility of SKF and MG-63 cells were observed. The anti-bacterial experiments were carried out using Syto9 fluorescent dyes to measure the bacterial survival rate of Staphylococcus aureus and Actinobacillusactinomycetemcomitans.

　　Results of this study showed that a porous titanium oxide surface was formed after the PEO process which increased the hydrophilicity of the film. The most hydrophilic sampleis the PEO-Ta2O5 samples. Results of MTT cellular activity assays showed that porous titanium oxide surfaces with PEO-Ta2O5 have greater MG-63 cellular biocompatibility compared with films with only tantalum pentoxide (Ta2O5). In addition, anti-bacterial experiments showed that the PEO-ZnOsample have better anti-bacterial properties compared with ZnO test pieces without PEO processed.

並列關鍵字

Plasma Electrolytic Oxidation ； PVD ； Tantalum oxide ； Zinc oxide ； Biocompatibility

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