银掺杂介孔氧化铝抗菌剂的一步合成与表征

摘要

Metallic sliver-doped mesoporous Al2 O3 nanoparticles ( mesoporous Ag/Al2 O3 NPs ) were synthe-sized via hydrothermal method using AgNO3 and Al(NO3)3·9H2O as precursors. Powder X-ray diffraction (XRD), field-emission scanning electron microscopy(FE-SEM), X-ray fluorescence(XRF), energy disper-sive spectrometry( EDS) and N2 adsorption-desorption techniques were used to characterize mesoporous Ag/Al2O3 NPs, and the tests of minimum inhibitory concentration(MIC) and inhibition zone were carried out to evaluate antimicrobial efficiency of mesoporous Ag/Al2 O3 NPs. XRD analysis identified Al2 O3 as an unique crystalline phase in mesoporous Ag/Al2 O3 NPs, and the lattice parameters modified significantly after doping with silver, in the meantime, the FWHM of mesoporous Ag/Al2O3 NPs increased while the (111), (400) and (440) interplanar spacing decreased. The FE-SEM images of mesoporous Al2 O3 NPs and mesoporous Ag/Al2 O3 NPs illustrate the diameter of mesoporous Ag/Al2 O3 NPs decreased while the pore diameter increased after doping with silver. The XRF and EDX spectra of mesoporous Ag/Al2 O3 NPs confirmed that the atomic ratio of O/Al was 1. 5. Insightful analyses of XRD and XRF spectra of mesoporous Ag/Al2 O3 NPs showed that metallic silver occupied interstitial positions of Al2 O3 lattice and interstitial solid solution was achieved. N2 adsorption-desorption analysis illustrates the specific surface area, pore volume and average pore diameter of mesoporous Ag/Al2 O3 NPs increased significantly after doping with silver. The MIC of mesoporous Ag/Al2 O3 NPs was less than 80 μg/mL against Escherichia coli and Staphylococcus aureus. The diameter of inhibition zone for mesoporous Ag/Al2 O3 NPs was 26 mm against Escherichia coli and 24 mm against Staphylococcus aureus.%以Al(NO3)3·9H2O和AgNO3为原料,采用水热法制备了介孔氧化铝纳米粒子(Mesoporous Al2O3 NPs)和银掺杂介孔氧化铝纳米粒子( Mesoporous Ag/Al2 O3 NPs),通过X射线衍射( XRD)、场发射扫描电子显微镜( FE-SEM)、X射线荧光光谱( XRF)、能量分散X射线衍射( EDX)和低温N2吸附-脱附等手段对产物进行了表征,通过最低抑菌浓度和抑菌圈实验研究了材料的抗菌性能. XRD分析表明在介孔Ag/Al2 O3 NPs中Al2O3是唯一结晶相, Ag掺杂后,介孔Ag/Al2O3 NPs晶格常数和半高峰宽增大,晶面间距[(111),(400)和(440)面]减小. FE-SEM形貌分析表明掺杂后的介孔Ag/Al2O3 NPs颗粒直径减小而孔径增大. EDX和XRF分析表明介孔Ag/Al2 O3 NPs中O/Al摩尔比为1.5,与Al2 O3 NPs中O/Al摩尔比相同.综合XRD和XRF分析结果认为, Ag进入介孔Al2 O3晶格间隙形成间隙固溶体.低温N2吸附-脱附分析表明掺杂后的介孔Ag/Al2 O3 NPs比表面积、孔体积和孔径增大.曝气抗菌实验结果表明介孔Ag/Al2 O3 NPs的抗菌机理是活性氧和金属银的协同作用.介孔Ag/Al2 O3 NPs对革兰氏阴性菌(大肠杆菌)和革兰氏阳性菌(金黄色葡萄球菌)具有明显的抗菌效果,对大肠杆菌和金黄色葡萄球菌的最低抑菌浓度( MIC)均为80μg/mL,抑菌圈直径分别为26 mm和24 mm.