高等学校化学学报 ›› 2016, Vol. 37 ›› Issue (6): 1036-1041.doi: 10.7503/cjcu20160111

• 研究论文: 无机化学 • 上一篇    下一篇

银掺杂介孔氧化铝抗菌剂的一步合成与表征

陈华军(), 席晓晶, 丁梧秀   

  1. 洛阳理工学院环境工程与化学学院, 洛阳 471023
  • 收稿日期:2016-02-25 出版日期:2016-06-10 发布日期:2016-05-26
  • 作者简介:联系人简介: 陈华军, 男, 副教授, 主要从事无机功能材料的合成与应用研究. E-mail:chj790118@163.com
  • 基金资助:
    国家自然科学基金(批准号: 51279073)和河南省科技厅科技攻关计划项目(批准号: 132102310367)资助

One-pot Synthesis and Antimicrobial Performance of Metallic Silver-doped Mesoporous Al2O3 Nanoparticles

CHEN Huajun*(), XI Xiaojing, DING Wuxiu   

  1. Department of Environmental Engineering and Chemistry,Luoyang Institute of Science and Technology, Luoyang 471023, China
  • Received:2016-02-25 Online:2016-06-10 Published:2016-05-26
  • Contact: CHEN Huajun E-mail:chj790118@163.com
  • Supported by:
    † Supported by the National Natural Science Foundation of China(No;51279073) and the Science and Technology Project of Institue of Science and Technology Department of Henan Province, China(No.132102310367)

摘要:

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/Al2O3 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/Al2O3 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/Al2O3 NPs中O/Al摩尔比为1.5, 与Al2O3 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Al2O3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/Al2O3 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/Al2O3 NPs的抗菌机理是活性氧和金属银的协同作用. 介孔Ag/Al2O3 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80 μg/mL, 抑菌圈直径分别为26 mm和24 mm.

关键词: 银掺杂, 介孔氧化铝, 革兰氏菌, 抗菌性能

Abstract:

Metallic sliver-doped mesoporous Al2O3 nanoparticles(mesoporous Ag/Al2O3 NPs) were synthesized 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 dispersive 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/Al2O3 NPs. XRD analysis identified Al2O3 as an unique crystalline phase in mesoporous Ag/Al2O3 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 Al2O3 NPs and mesoporous Ag/Al2O3 NPs illustrate the diameter of mesoporous Ag/Al2O3 NPs decreased while the pore diameter increased after doping with silver. The XRF and EDX spectra of mesoporous Ag/Al2O3 NPs confirmed that the atomic ratio of O/Al was 1.5. Insightful analyses of XRD and XRF spectra of mesoporous Ag/Al2O3 NPs showed that metallic silver occupied interstitial positions of Al2O3 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/Al2O3 NPs increased significantly after doping with silver. The MIC of mesoporous Ag/Al2O3 NPs was less than 80 μg/mL against Escherichia coli and Staphylococcus aureus. The diameter of inhibition zone for mesoporous Ag/Al2O3 NPs was 26 mm against Escherichia coli and 24 mm against Staphylococcus aureus.

Key words: Silver doping, Mesoporous Al2O3, Gram, Antimicrobial efficiency

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