介孔氧化锌的制备及其抗菌性能的研究
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摘要
采用微相氨蒸发诱导自组装法成功制备了介孔氧化锌,并对其进行氮气的低温吸附和脱附测定其BET比表面积、孔容和孔径分布,结合Low-Angle XRD和TEM表征氧化锌的结构;利用Wide-Angle XRD、HRTEM,、EDS、SAED等表征方法对氧化锌孔壁的物相和晶相进行分析;讨论不同合成条件对介孔氧化锌的孔结构的影响,并探讨微相氨蒸发自组装法制备介孔氧化锌的成孔的机理。
实验结果表明:介孔氧化锌的BET比表面积和孔容分别为223.77 m~2g~(-1)和0.6930cm~3g~(-1),孔径为9.79 nm;孔壁晶型为红锌矿型氧化锌(a=3.253,c=5.213,P6_3mc,JCPDS card No.:079-0207)单晶;氧化锌形成介孔结构,其反应温度必须在70℃以上;蔗糖的量和氨的量对氧化锌介孔结构有一定影响;后处理的晶化温度对氧化锌的晶型起到至关重要的作用。
采用抑菌环法和最小抑菌浓度法,对所合成的不同BET比表面积介孔氧化锌进行抗菌性能测试。结果表明:介孔氧化锌的大肠杆菌的最小抑菌浓度能达到100μg/mL,金黄色葡萄球菌的最小抑菌浓度能达到50μg/mL,说明介孔氧化锌的具有良好的抗菌性能。
Mesoporous ZnO was synthesized successfully by using the micro-phase ammonia evaporation induced self-assembly method. And the pore structure was studied by measuring the N_2 adsorption/desorption isotherms of porous material, Low-angle XRD and TEM. Analytical methods such as XRD, HRTEM, EDS and SAED were used to investigate the compositions and structures of mesoporous ZnO. Then the effect of the various synthesis conditions on pore structure of mesoporous ZnO was studied. And the mechanism of formation of mesoporous ZnO, prepared by the micro-phase ammonia evaporation induced self-assembly method, was explored.
The results showed that, the BET special surface area, pore volume and pore size was 223.77 m~2g~(-1), 0.6930 cm~3g~(-1) and 9.79 nm, respectively. The pore wall was made up of zincite single crystal (a=3.253, c=5.213, P6_3mc, JCPDS card No.:079-0207) . Only under the situation of the Zinc ammonia/sucrose precursor solution micro-phase formed and the reaction temperature above 70℃can the ammonia evaporation induce self-assembly process and obtain meso-structured ZnO. The amount of sucrose and ammonia produce some effect on the mesoporous structure of zinc oxide, and crystallization temperature play a crucial role in crystal type of zinc oxide
The antibacterial performance of the mesoprous ZnO samples with various BET specific surface area were measured by applying Minimal Inhibitory Concentration (MIC) and Bacteriostatic Annulus method. The results indicated that, the value of MIC of mesoporous ZnO for Escherichia coli can achieve 100μg/mL, and the value of MIC of mesoporous ZnO for Staphylococcus aureus can achieve 100μg/mL. The antibacterial performance of mesoporous ZnO is quite excellent.
实验结果表明:介孔氧化锌的BET比表面积和孔容分别为223.77 m~2g~(-1)和0.6930cm~3g~(-1),孔径为9.79 nm;孔壁晶型为红锌矿型氧化锌(a=3.253,c=5.213,P6_3mc,JCPDS card No.:079-0207)单晶;氧化锌形成介孔结构,其反应温度必须在70℃以上;蔗糖的量和氨的量对氧化锌介孔结构有一定影响;后处理的晶化温度对氧化锌的晶型起到至关重要的作用。
采用抑菌环法和最小抑菌浓度法,对所合成的不同BET比表面积介孔氧化锌进行抗菌性能测试。结果表明:介孔氧化锌的大肠杆菌的最小抑菌浓度能达到100μg/mL,金黄色葡萄球菌的最小抑菌浓度能达到50μg/mL,说明介孔氧化锌的具有良好的抗菌性能。
Mesoporous ZnO was synthesized successfully by using the micro-phase ammonia evaporation induced self-assembly method. And the pore structure was studied by measuring the N_2 adsorption/desorption isotherms of porous material, Low-angle XRD and TEM. Analytical methods such as XRD, HRTEM, EDS and SAED were used to investigate the compositions and structures of mesoporous ZnO. Then the effect of the various synthesis conditions on pore structure of mesoporous ZnO was studied. And the mechanism of formation of mesoporous ZnO, prepared by the micro-phase ammonia evaporation induced self-assembly method, was explored.
The results showed that, the BET special surface area, pore volume and pore size was 223.77 m~2g~(-1), 0.6930 cm~3g~(-1) and 9.79 nm, respectively. The pore wall was made up of zincite single crystal (a=3.253, c=5.213, P6_3mc, JCPDS card No.:079-0207) . Only under the situation of the Zinc ammonia/sucrose precursor solution micro-phase formed and the reaction temperature above 70℃can the ammonia evaporation induce self-assembly process and obtain meso-structured ZnO. The amount of sucrose and ammonia produce some effect on the mesoporous structure of zinc oxide, and crystallization temperature play a crucial role in crystal type of zinc oxide
The antibacterial performance of the mesoprous ZnO samples with various BET specific surface area were measured by applying Minimal Inhibitory Concentration (MIC) and Bacteriostatic Annulus method. The results indicated that, the value of MIC of mesoporous ZnO for Escherichia coli can achieve 100μg/mL, and the value of MIC of mesoporous ZnO for Staphylococcus aureus can achieve 100μg/mL. The antibacterial performance of mesoporous ZnO is quite excellent.
引文
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[2]C. T. Kresge, M. E. Leonowicz, W. J. Roth, J. C. Vartuli, J. S. Beck Ordered mesoporous molecular sieves synthesized by a liquid-crystal template mechanism Nature [J], 1992, 359:710 - 712
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[4]Morey Mark, Davidson Anne, Eckert Hellmut, et al. Pseudotetrahedral O3/2V O Centers Immobilized on the Walls of a Mesoporous, Cubic MCM-48 Support: Preparation, Characterization, and Reactivity toward Water As Investigated by 51V NMR and UV-Vis Spectroscopies. Chemistry of Materials [J], 1996, 8(2): 486-492.
[5]Huo Qisheng, Feng Jianglin, Schuth Ferdi, et al. Preparation of Hard Mesoporous Silica Spheres. Chemistry of Materials [J], 1997, 9(1): 14-17.
[6]Lettow John S., Han Yong Jin, Schmidt-Winkel Patrick, et al. Hexagonal to Mesocellular Foam Phase Transition in Polymer-Templated Mesoporous Silicas. Langmuir [J], 2000,16(22): 8291-8295.
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[8]Stephen A. Bagshaw Eric Prouzet, Thomas J. Pinnavaia. Templating of Mesoporous Molecular Sieves by Nonionic Polyethylene Oxide Surfactants Science [J], 1995, 269:1242-1244
[9] Pinnavaia Peter T. Tanev and Thomas J. A Neutral Templating Route to Mesoporous Molecular Sieves. Science [J], 1995 267:865-867
[10] Antonelli David M., Ying Jackie Y. Synthesis and Characterization of Hexagonally Packed Mesoporous Tantalum Oxide Molecular Sieves. Chemistry of Materials [J], 1996, 8(4): 874-881.
[11] Beck J. S., Vartuli J. C., Roth W. J., et al. A new family of mesoporous molecular sieves prepared with liquid crystal templates. Journal of the American Chemical Society [J], 1992,114(27): 10834-10843.
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[13] Vartuli J. C., Schmitt K. D., Kresge C. T., et al. Effect of Surfactant/Silica Molar Ratios on the Formation of Mesoporous Molecular Sieves: Inorganic Mimicry of Surfactant Liquid-Crystal Phases and Mechanistic Implications. Chemistry of Materials [J], 1994, 6(12): 2317-2326.
[14] Chen Cong-Yan, Burkett Sandra L., Li Hong-Xin, et al. Studies on mesoporous materials II. Synthesis mechanism of MCM-41. Microporous Materials [J], 1993,2(1):27-34.
[15]Peidong Yang Dongyuan Zhao,Dacid I.Margolese,Bradley F.Chmelka,Galen D.Stucky.Generalized syntheses of large-poremesoporous metal oxideswith semicrystalline frameworks.Nature[J],1998,396:152-155.
[16]Firouzi A.,Kumar D,Bull L.M.cooperative organization of inorganic-surfactant and biomimetic assemblies Science[J],1995,267:1138-1143.
[17]Rouquerol J.,Avnir,D.,Fairbridge,Everett,et al..Recommendations for the characterization of porous solids.Pure Appl Chem[J],1994,66:1739-1758.
[18]Mann S.,Burkett,S.L.,Davis,S.A.,Fowler,C.E.,Mendelson,N.H.,Sims,S.D.,Walsh,D.Sol-gel synthesis of organized matter.Chem Mater[J],1997,9:2300-2310.
[19]徐如人,庞文琴,于吉红,等.分子筛与多孔材料[M].北京:科学出版社,2004.
[20]Lu Daling,Katou Tokumitsu,Uchida Miwa,et al.In Situ TEM Observation of Crystallization of Amorphous Ordered Mesoporous Nb,Ta and Mg/Ta Mixed Oxides.Chemistry of Materials[J],2005,17(3):632-637.
[21]Takahashi Naoyuki,Makino Masanori,Nakamura Takato,et al.Rapid Growth of Thick ZnO Films with Room-Temperature Ultraviolet Emission by Means of Atmospheric Pressure Halide Vapor-Phase Epitaxy.Chemistry of Materials[J],2002,14(9):3622-3624.
[22]Gorla C.R.,Emanetoglu N.W.,Liang S.,et al.Structural,optical,and surface acoustic wave properties of epitaxial ZnO films grown on(011-bar 2) sapphire by metalorganic chemical vapor deposition.Journal of Applied Physics[J],1999,85(5):2595-2602.
[23]Wang Debao,Song Caixia.Controllable Synthesis of ZnO Nanorod and Prism Arrays in a Large Area.The Journal of Physical Chemistry B[J],2005,109(26):12697-12700.
[24]Gao Pu-Xian,Ding Yong,Wang Zhong Lin.Electronic Transport in Superlattice-Structured ZnO Nanohelix.Nano Letters[J],0(0):
[25]Pauporte T.,Rathousky J.Electrodeposited Mesoporous ZnO Thin Films as Efficient Photocatalysts for the Degradation of Dye Pollutants.The Journal of Physical Chemistry C[J],2007,111(21):7639-7644.
[26]Rao G.S.Trivikrama,Tarakarama Rao D.Gas sensitivity of ZnO based thick film sensor to NH3 at room temperature.Sensors and Actuators B:Chemical[J],1999,55(2-3):166-169.
[27]T.Wagner,T.Waitz,J.Roggenbuck,et al.Ordered mesoporous ZnO for gas sensing.Thin Solid Fihns[J],2007,515(23):8360-8363.
[28]Jin Z.-C.,Hamberg I.,Granqvist C.G.Optical properties of sputter-deposited ZnO:Al thin films.Journal of Applied Physics[J],1988,64(10):5117-5131.
[29]Deng Ziwei,Chen Min,Gu Guangxin,et al.A Facile Method to Fabricate ZnO Hollow Spheres and Their Photocatalytic Property.The Journal of Physical Chemistry B[J],2008,112(1):16-22.
[30]Ozgur U.,Alivov Ya I.,Liu C.,et al.A comprehensive review of ZnO materials and devices.Journal of Applied Physics[J],2005,98(4):041301-041103.
[31]Service Robert F.Materials Science:Will UV Lasers Beat the Blues?Science[J],1997,276(5314):895.
[32]Wang Xudong,Ding Yong,Li Zhou,et al.Single-Crystal Mesoporous ZnO Thin Films Composed of Nanowalls.The Journal of Physical Chemistry C[J],2009,113(5):1791-1794.
[33]Lu Hongbing,Liao Lei,Li Jinchai,et al.High Surface-to-Volume Ratio ZnO Microberets:Low Temperature Synthesis,Characterization,and Photoluminescence.The Journal of Physical Chemistry B[J],2006,110(46):23211-23214.
[34]Cheng Jiping,Zhang Yunjin,Guo Ruyan.Field Emission Properties of ZnO Single Crystal Microtubes.Journal of Applied Physics[J],2009,105(3):034313-034314.
[35]Hirose Sakyo,Yamamoto Yoji,Niimi Hideaki.Effect of local electrical properties on the electrostatic discharge withstand capability of multilayered chip ZnO varistors.Journal of Applied Physics[J],2008,104(1):013701-013712.
[36]An Wei,Wu Xiaojun,Zeng X.C.Adsorption of O2,H2,CO,NH3,and NO2 on ZnO Nanotube: A Density Functional Theory Study.The Journal of Physical Chemistry C[J],2008,112(15):5747-5755.
[37]Qisheng Huo David I.Margolese,Ulrike Ciesla,Galen D.Stucky.Generalized synthesis of periodic surfactant inorganic composite materials.Nature[J],1994,368:317-319.
[38]Zhao Dongyuan,Goldfarb Daniella.Synthesis of Lamellar Mesostructures with Nonamphiphilic Mesogens as Templates.Chemistry of Materials[J],1996,8(11):2571-2578.
[39]Yang Peidong,Zhao Dongyuan,Margolese David I.,et al.Block Copolymer Templating Syntheses of Mesoporous Metal Oxides with Large Ordering Lengths and Semicrystalline Framework.Chemistry of Materials[J],1999,11(10):2813-2826.
[40]Choi Kyoung-Shin,Lichtenegger Helga C.,Stucky Galen D.,et al.Electrochemical Synthesis of Nanostructured ZnO Films Utilizing Self-Assembly of Surfactant Molecules at Solid-Liquid Interfaces.Journal of the American Chemical Society[J],2002,124(42):12402-12403.
[41]Jiu Jinting,Kurumada Ken-ichi,Tanigaki Masataka.Preparation of nanoporous ZnO using copolymer gel template.Materials Chemistry and Physics[J],2003,81(1):93-98.
[42]Luo Jia-yan,Wang Yong-gang,Xiong Huan-ming,et al.Ordered Mesoporous Spinel LiMn2O4 by a Soft-Chemical Process as a Cathode Material for Lithium-Ion Batteries.Chemistry of Materials[J],2007,19(19):4791-4795.
[43]陈学泽.无机及分析化学[M].北京:中国林业出版社,2000.
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