银纳米线的宏量制备及其在柔性透明电极中的应用

发布时间：2018-06-25 20:45

本文选题：银纳米线 + 一锅法　；参考：《河南大学》2016年硕士论文

【摘要】：对用于制备银纳米线的多元醇法进行了改进,探讨了温度、硝酸银浓度、聚乙烯吡咯烷酮(PVP)分子量及浓度、卤盐种类及浓度、加料速度、加料方式等参数对纳米银形貌的影响;考察了银纳米线的成核和生长机理以及各影响因素之间的相互作用;进而建立了简便、高效制备宏量银纳米线的一锅法工艺,可望为其大规模应用奠定实验和技术基础。与此同时,制备了银纳米线透明导电薄膜,评价了其光电性能,并探讨了银纳米线直径对透明导电薄膜光电性能的影响。本论文主要研究内容和结果如下:(1)试验参数对银纳米线形貌的影响选择NiCl_2作为控制剂,利用多元醇法制备了银纳米线;考察了温度、硝酸银浓度、PVP与AgNO_3的摩尔比、NiCl_2与AgNO_3的摩尔比、加料速度、保护气种类等对银纳米线形貌的影响。与此同时,采用扫描电镜、透射电镜、X射线衍射仪等分析了产物的形貌和结构,分析了银纳米线的成核和生长机理。结果表明,通过合理调整试验参数可以有效降低银纳米颗粒制备中副产物的数量,得到直径为40-100 nm的银纳米线,产率可高达95%以上。(2)一锅法制备宏量银纳米线传统的银纳米线制备工艺需要将反应物逐滴加入反应体系中,产物数量为毫克或克级,不利于实现宏量制备,也无法满足工业需求。因此,我们深入探究了加料方式及温度对银纳米线产量的影响,并初步探讨了银纳米线的纯化和保存,以便为其商业化提供实验依据和技术支撑。结果表明,通过合理控制升温过程可以实现银纳米线的一锅法宏量制备(反应器容积为5 L;单次反应产量超过10 g)。(3)银纳米线透明电极的制备和光电性能研究将不同直径的银纳米线作为导电材料,以聚对苯二甲酸乙二醇酯(PET)作为基底材料,利用旋涂方式制备出柔性透明导电薄膜;探究了银纳米线直径对透明电极光电性能的影响。结果表明,通过优化工艺条件,可以制备出透光率达90%、方阻为70?左右的高性能透明导电薄膜;银纳米线的直径越细、长径比越大,则透明导电薄膜的光电性能越好。(4)超细银纳米线的制备银纳米线直径对透明导电薄膜的光电性能具有重要影响,而直径小于25 nm的超细银纳米线的制备是研制高性能透明导电薄膜的重点和难点。为此,以前述一锅法为基础,通过引入NaCl、NiCl_2、NaBr作为控制剂,尝试制备超细银纳米线。结果表明,分别以NaCl-NaBr和NiCl_2-NaBr作为控制剂,以PVP作为修饰剂,可以得到平均直径为23 nm的超细银纳米线。
[Abstract]:The polyol method for preparing silver nanowires was improved. The effects of temperature, concentration of silver nitrate, molecular weight and concentration of polyvinylpyrrolidone (PVP), type and concentration of halogen, feed rate and feeding mode on the morphology of silver nanoparticles were investigated, and the nucleation and growth mechanism of silver nanowires and the phases of various factors were investigated. The one pot process of simple and efficient preparation of macro silver nanowires was established, and the experimental and technical basis for its large-scale application was expected. At the same time, the silver nanowire transparent conductive film was prepared and its photoelectric properties were evaluated. The influence of the direct diameter of the silver nanowire on the photoelectric properties of the transparent conductive film was discussed. The contents and results are as follows: (1) the influence of the test parameters on the morphology of silver nanowires is selected as the control agent, and the silver nanowires are prepared by the polyol method. The influence of temperature, the concentration of silver nitrate, the molar ratio of PVP to AgNO_3, the molar ratio of NiCl_2 to AgNO_3, the feeding speed and the type of protective gas on the morphology of the silver nanowires are investigated. At the same time, the morphology and structure of the products were analyzed by scanning electron microscope, transmission electron microscope and X ray diffractometer. The nucleation and growth mechanism of the silver nanowires were analyzed. The results showed that the number of byproducts in the silver nanoparticles could be effectively reduced by adjusting the test parameters reasonably, and the silver nanowires with a diameter of 40-100 nm were obtained, with a yield of up to 95. (2) the traditional preparation process of silver nanowires with one pot method to prepare silver nanowires requires the addition of the reactants to the reaction system by dropping the reactants in the reaction system. The quantity of the products is milligram or gram level, which is not conducive to the preparation of macros and the industrial demand. Therefore, we have deeply explored the effect of the feeding mode and temperature on the production of silver nanowires, and preliminary study on the effect of the temperature on the production of silver nanowires. The purification and preservation of the silver nanowires are discussed in order to provide experimental basis and technical support for commercialization. The results show that the one pot macro amount of silver nanowires can be prepared by reasonable control of the heating process (the volume of the reactor is 5 L; the yield of the single reaction exceeds 10 g). (3) the preparation and photoelectric properties of the silver nanowire transparent electrode will be studied. The silver nanowires of different diameters are used as conductive material, with polyglycol terephthalate (PET) as the base material, and the flexible transparent conductive film is prepared by spin coating. The effect of the diameter of the silver nanowires on the photoelectric properties of the transparent electrode is explored. The results show that the transmittance of 90% and the square resistance of 70 can be prepared by the optimization process conditions. The smaller the diameter of the silver nanowires and the greater the ratio of the length to diameter, the better the photoelectric properties of the transparent conductive film. (4) the silver nanowire diameter of the ultrafine silver nanowires has an important effect on the photoelectric properties of the transparent conductive film, and the preparation of the ultrafine silver nanowires with a diameter of less than 25 nm is the development of high performance penetration. On the basis of one pot method, the ultrafine silver nanowires are prepared by introducing NaCl, NiCl_2 and NaBr as the control agent. The results show that the ultrafine silver nanowires with an average diameter of 23 nm can be obtained by using NaCl-NaBr and NiCl_2-NaBr as the control agent and PVP as the modifier respectively.
【学位授予单位】：河南大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O614.122;TB383.1

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