纳米银及其复合抗菌材料的研究
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摘要
纳米银（Nano Silver）是指通过一定的化学途径或者物理手段制备的粒径在1-100nm之间的单质银粒子（Silver Nanoparticles，学界简写AgNPs），它具有表面效应、小尺寸效应和宏观量子隧道效应。纳米银在磁性材料、电子材料、光学材料以及高强、高密度材料的烧结、催化、传感等方而有广阔的应用前景，已经成为21世纪最有前途的材料之一。将纳米银掺入到其它材料之中，可以制备出许多种类的载纳米银复合抗菌材料。含银离子抗菌剂在金属离子抗菌剂研究中最受关注。
本文采用微波加热与化学催化相结合，制备出不同粒径的球形、棒状、线状纳米银粒子。结果表明：PVP有利于提高纳米Ag粉间的静电排斥作用，有利于其分散；升高反应的温度有利于反应的快速进行，增加银颗粒的形核速度，形核速度增加以后，从而降低了颗粒的粒径；延长反应的时间，粒子尺寸增大，粒径和形状易于发生不规则的变化；反应物浓度的升高造成颗粒的长大与团聚；引入Cl-，并适当控制反应的时间，可实现产物从球形纳米银到棒状纳米银的转变。
采用微波加热并掺入Cl-的还原方法，合成出直径从30-50纳米，长度50nm到数微米的纳米银棒。我们通过透射电子显微镜(TEM)观察其形貌，并利用UV-Vis谱、XRD分析、EDX等手段对其进行表征，研究了其形貌、结构及形成机理间关系。形成机理主要分为三个阶段：第一阶段，在Cl-作用下，生成粒径很小的球形纳米银晶粒；第二阶段，在PVP的模板作用下，生成大量三角形的银纳米颗粒，与此同时少量棒状结构的银纳米颗粒逐渐生成；第三阶段，三角形颗粒结合生成棒状结构的银纳米颗粒，并不断转化、结合、长大成为棒状的结构。
利用纳米银良好的抗菌性能，以明胶(Gelatin,以下简称GA)和聚乙烯醇(polyvinyl alcohol,以下简称PVA)为主要原料并采用静电纺丝的方法合成出一种含银的明胶/聚乙烯醇抗菌纤维（以下简称：Ag/GA/PVA的复合抗菌材料）。本文通过探讨纺丝条件对纤维结构的影响，制备出一种拉伸强度、弹性、吸水性能等性能优良的纤维材料，运用SEM、XRD、UV-vis等测试手段，及抗菌试验和细胞毒性试验，结果表明，该复合抗菌材料是一种安全无毒的具有良好抗菌性能的三元复合材料。
本研究还合成了一种性能良好的核壳抗菌剂，结合SEM，抗菌试验等表明，该抗菌剂是一种具有长久抗菌效果的核壳抗菌复合材料。还探讨了纳米银的导电性能和光学性能，制备出性能出色具有自抗菌功能的导电银浆，并对表面增强拉曼散射活性做了初步探讨。
Nano silver are silver nanoparticles, mainly between1nm and100nm in size,which can be prepared by chemical or physical methods. Because of its quantμm sizeeffect, small-size effect, surface effect and macroscopic quantμm tunneling effect, thenano silver has been one of the most promising materials in twenty-first century. Thenano silver has a wide application prospect in magnetic materials, electronic materials,optical materials and high strength, high density material sintering, catalysis, sensing,etc. Various nano silver composite materials with anti-bacterial property can beprepared by adding silver Nanoparticles. Silver ion is of most concern in metal ion usedas.antibacterial agent
In this study, spherical, rodlike and linear silver nanoparticles with differentdiameters were prepared by the combination of microwave heating and chemicalcatalysis. The results showed that PVP is beneficial to the dispersion of nanoparticles byimproving the electrostatic repulsion between the nano silver powders. The higherreaction temperature is beneficial to the reaction, which accelerated nucleation rate ofthe silver particle and thus reduced the particle size. Increasing the concentration of thereactants would result the increased growth and agglomeration of the particles. By theintroducing Cl-and properly controlling the reaction time, the products could transformfrom spherical to rodlike nanoparticles.
Rodlike silver nanoparticles with the diameter of30~50nm and the length of50nmwere synthesized by microwave heating method. By transmission electron microscopy(TEM), UV-Vis spectra, and XRD analysis, EDX and other methods, we observed themorphology of the nano particles and studied the relationship between structure andformation mechanism. The formation of Rodlike silver nanoparticles can be dividedinto three stages. Stage Ⅰ, spherical silver with small size were generated in thepresence of Cl-. StageⅡ, with the PVP as templates, a large nμmber of triangular silvernanoparticles were generated with a small amount of rod-like structure of silvernanoparticles. Stage Ⅲ, the triangle particles combined to form rod-like structure silver nanoparticles, which kept constantly transforming and binding, and finally grew into arodlike structure.
To evaluate the antibacterial Performance of the nano silvers, we fabricatedAg/GA/PVA composite materials by electrospinning technique. By adjusting theelectrospinning parameters, we successfully prepared nanofibrous antibacterialmaterials with high tensile strength, excellent elasticity and good water absorption.Using SEM, XR, UV-vis and other testing methods, we confirmed the goodantibacterial property of Ag/GA/PVA composite materials through antibacterial test andcytotoxicity test.
In this thesis, we produced composite material with core-shell structure, whichexhibited excellent antibacterial in long term confirmed by the SEM characterizationand antimicrobial test. Furthermore, the electrical properties and optical properties ofnano silvers were investigated. Silver paste with excellent conductive performance wasalso prepared, and the surface Raman scattering activity.was tested.
本文采用微波加热与化学催化相结合，制备出不同粒径的球形、棒状、线状纳米银粒子。结果表明：PVP有利于提高纳米Ag粉间的静电排斥作用，有利于其分散；升高反应的温度有利于反应的快速进行，增加银颗粒的形核速度，形核速度增加以后，从而降低了颗粒的粒径；延长反应的时间，粒子尺寸增大，粒径和形状易于发生不规则的变化；反应物浓度的升高造成颗粒的长大与团聚；引入Cl-，并适当控制反应的时间，可实现产物从球形纳米银到棒状纳米银的转变。
采用微波加热并掺入Cl-的还原方法，合成出直径从30-50纳米，长度50nm到数微米的纳米银棒。我们通过透射电子显微镜(TEM)观察其形貌，并利用UV-Vis谱、XRD分析、EDX等手段对其进行表征，研究了其形貌、结构及形成机理间关系。形成机理主要分为三个阶段：第一阶段，在Cl-作用下，生成粒径很小的球形纳米银晶粒；第二阶段，在PVP的模板作用下，生成大量三角形的银纳米颗粒，与此同时少量棒状结构的银纳米颗粒逐渐生成；第三阶段，三角形颗粒结合生成棒状结构的银纳米颗粒，并不断转化、结合、长大成为棒状的结构。
利用纳米银良好的抗菌性能，以明胶(Gelatin,以下简称GA)和聚乙烯醇(polyvinyl alcohol,以下简称PVA)为主要原料并采用静电纺丝的方法合成出一种含银的明胶/聚乙烯醇抗菌纤维（以下简称：Ag/GA/PVA的复合抗菌材料）。本文通过探讨纺丝条件对纤维结构的影响，制备出一种拉伸强度、弹性、吸水性能等性能优良的纤维材料，运用SEM、XRD、UV-vis等测试手段，及抗菌试验和细胞毒性试验，结果表明，该复合抗菌材料是一种安全无毒的具有良好抗菌性能的三元复合材料。
本研究还合成了一种性能良好的核壳抗菌剂，结合SEM，抗菌试验等表明，该抗菌剂是一种具有长久抗菌效果的核壳抗菌复合材料。还探讨了纳米银的导电性能和光学性能，制备出性能出色具有自抗菌功能的导电银浆，并对表面增强拉曼散射活性做了初步探讨。
Nano silver are silver nanoparticles, mainly between1nm and100nm in size,which can be prepared by chemical or physical methods. Because of its quantμm sizeeffect, small-size effect, surface effect and macroscopic quantμm tunneling effect, thenano silver has been one of the most promising materials in twenty-first century. Thenano silver has a wide application prospect in magnetic materials, electronic materials,optical materials and high strength, high density material sintering, catalysis, sensing,etc. Various nano silver composite materials with anti-bacterial property can beprepared by adding silver Nanoparticles. Silver ion is of most concern in metal ion usedas.antibacterial agent
In this study, spherical, rodlike and linear silver nanoparticles with differentdiameters were prepared by the combination of microwave heating and chemicalcatalysis. The results showed that PVP is beneficial to the dispersion of nanoparticles byimproving the electrostatic repulsion between the nano silver powders. The higherreaction temperature is beneficial to the reaction, which accelerated nucleation rate ofthe silver particle and thus reduced the particle size. Increasing the concentration of thereactants would result the increased growth and agglomeration of the particles. By theintroducing Cl-and properly controlling the reaction time, the products could transformfrom spherical to rodlike nanoparticles.
Rodlike silver nanoparticles with the diameter of30~50nm and the length of50nmwere synthesized by microwave heating method. By transmission electron microscopy(TEM), UV-Vis spectra, and XRD analysis, EDX and other methods, we observed themorphology of the nano particles and studied the relationship between structure andformation mechanism. The formation of Rodlike silver nanoparticles can be dividedinto three stages. Stage Ⅰ, spherical silver with small size were generated in thepresence of Cl-. StageⅡ, with the PVP as templates, a large nμmber of triangular silvernanoparticles were generated with a small amount of rod-like structure of silvernanoparticles. Stage Ⅲ, the triangle particles combined to form rod-like structure silver nanoparticles, which kept constantly transforming and binding, and finally grew into arodlike structure.
To evaluate the antibacterial Performance of the nano silvers, we fabricatedAg/GA/PVA composite materials by electrospinning technique. By adjusting theelectrospinning parameters, we successfully prepared nanofibrous antibacterialmaterials with high tensile strength, excellent elasticity and good water absorption.Using SEM, XR, UV-vis and other testing methods, we confirmed the goodantibacterial property of Ag/GA/PVA composite materials through antibacterial test andcytotoxicity test.
In this thesis, we produced composite material with core-shell structure, whichexhibited excellent antibacterial in long term confirmed by the SEM characterizationand antimicrobial test. Furthermore, the electrical properties and optical properties ofnano silvers were investigated. Silver paste with excellent conductive performance wasalso prepared, and the surface Raman scattering activity.was tested.
引文
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