Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/10701
標題: 化學披覆奈米銀的二氧化矽微球與其抗菌效果之研究
Chemical Syntheses of Silver-Coated Silica Microspheres and Their Antibacterial Effects
作者: 黃俧達
Huang, Chih-Ta
關鍵字: sacrificial template;犧牲模板;hollow structure;silicate;silver;escherichia coli;中空結構;二氧化矽;奈米銀;大腸桿菌
出版社: 材料科學與工程學系所
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摘要: 
本研究分別使用水及四氯乙烯為反應溶劑,四氯化矽作為合成二氧化矽的前驅物,與有機微球作為硬質模板,藉由溶凝膠方式使四氯化矽水解形成矽化合物披覆在有機微球表面,經過鍛燒熱處理移除有機微球,獲得二氧化矽中空微球,再將此微球利用化學披覆銀原子在微球表面;本研究嘗試藉由改變反應溶劑、反應時間、以及清洗次數,將獲得之二氧化矽粉體分別利用場發射電子顯微鏡(FE-SEM)、X光繞射分析儀(XRD)、穿透式電子顯微鏡(TEM)、粒徑與界面電位分析儀(DLS & Zeta)、與比表面積分析儀(BET),分析合成粉體之表面形貌、結構、表面電性以及比表面積,並且利用感應藕荷電漿質譜儀(ICP-MS)分析其銀離子釋放效果。
由化學分析電子光譜儀(ESCA)縱深分析可以得到,矽的前驅物是藉由披覆方式附著在有機微球表面;SEM分析發現以水為溶劑所合成出之披覆有二氧化矽的有機微球表面呈現均勻披覆效果,並且當反應時間為10min時表面均勻披覆效果最好;而以四氯乙烯為溶劑的系統所合成之微球則呈現不均勻披覆。TEM證明以水為溶劑合成出之二氧化矽微球為一中空結構。另外,BET顯示中空結構二氧化矽微球比表面積高於實心結構二氧化矽微球,且中空結構二氧化矽微球具有中孔洞結構;DLS & Zeta顯示在合成步驟微球表面電性以及外徑尺寸的變化,發現在披覆矽化合物後,有機微球表面電性並未明顯改變,需藉由鍛燒移除有機微球後,中空二氧化矽微球才會顯示與文獻中的二氧化矽相同之表面電位-pH依存性;粒徑量測發現當改變溶液中的pH值時,中空結構微球的粒徑大幅下降,可以證明pH值的改變會影響到銀離子的釋放效果;XRD、Raman與UV-Vis則證明銀成功披覆在二氧化矽表面。
最後,藉由抗菌實驗以及ICP分析相同重量之披覆奈米銀的中空與實心二氧化矽微球在銀離子釋放對抗大腸桿菌的效果,披覆有奈米銀的中空二氧化矽微球明顯優於披覆有奈米銀的實心二氧化矽微球,證明中空結構增加了銀離子的釋放效果。

This research uses water and tetrachloroethylene as reactive solvent, silicon tetrachloride as precursor for silica, and polymeric microspheres as hard template for the synthesis of silver-coated silica particles with hollow interiors. At first, the silicon tetrachloride hydrolyzes, then condenses on surface of the polymeric templates via a sol-gel route. The hollow silica particles are fabricated after thermal pyrolysis of the organic templates, followed then by silver adsorption on the surface of hollow silica particles by a chemical electroplating. Process variables such as reactive solvent, reactive time, and the cycles of washing are examined. In addition, the silica particles are examined by FE-SEM, XRD, TEM, DLS, Zeta, and BET to analyze their morphology, structure, electrophoretic property, and specific surface area. Also, ICP-MS is used to analyze the release of silver ions in given solutions.
ESCA results show that silica is coated on surface of the polymeric microspheres. SEM analysis reveals that when water was used as a solvent, uniform silica coating on the surface of organic microsphere can be obtained, and when the reactive time is 10 minutes, an uniform coating layer can be prepared. But when tetrachloroethylene was used as a reactive solvent, an inhomogeneous silica coating is found on the organic microspheres. TEM shows that the silica particles prepared by use water as a reactive solvent form particles with a hollow structure. Also, BET confirms that the specific surface area of the hollow silica particles is substantially higher than that of the solid silica particles of similar size. DLS and zeta analyses show that the electrophoretic zeta potential does not change during the silica-coated process until calcination. The silica-coated particles change their size when pH alters, influencing the release of silver ions. XRD, Raman, and UV-Vis indicate that silvers are coated on the silica particles.
Finally, the antibacterial experiment and ICP analysis reveal that the hollow and solid silver-coated silica particles of the same weight would show a pronounced difference on the release of silver ions for the escherichia coli. Our results show that the hollow structure raises the release effect of silver ion both in the antibacterial experiment and ICP measurement.
URI: http://hdl.handle.net/11455/10701
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