本文選題：銀納米線 + 一鍋法　； 參考：《河南大學(xué)》2016年碩士論文

【摘要】：對(duì)用于制備銀納米線的多元醇法進(jìn)行了改進(jìn),探討了溫度、硝酸銀濃度、聚乙烯吡咯烷酮(PVP)分子量及濃度、鹵鹽種類(lèi)及濃度、加料速度、加料方式等參數(shù)對(duì)納米銀形貌的影響;考察了銀納米線的成核和生長(zhǎng)機(jī)理以及各影響因素之間的相互作用;進(jìn)而建立了簡(jiǎn)便、高效制備宏量銀納米線的一鍋法工藝,可望為其大規(guī)模應(yīng)用奠定實(shí)驗(yàn)和技術(shù)基礎(chǔ)。與此同時(shí),制備了銀納米線透明導(dǎo)電薄膜,評(píng)價(jià)了其光電性能,并探討了銀納米線直徑對(duì)透明導(dǎo)電薄膜光電性能的影響。本論文主要研究?jī)?nèi)容和結(jié)果如下:(1)試驗(yàn)參數(shù)對(duì)銀納米線形貌的影響選擇NiCl_2作為控制劑,利用多元醇法制備了銀納米線;考察了溫度、硝酸銀濃度、PVP與AgNO_3的摩爾比、NiCl_2與AgNO_3的摩爾比、加料速度、保護(hù)氣種類(lèi)等對(duì)銀納米線形貌的影響。與此同時(shí),采用掃描電鏡、透射電鏡、X射線衍射儀等分析了產(chǎn)物的形貌和結(jié)構(gòu),分析了銀納米線的成核和生長(zhǎng)機(jī)理。結(jié)果表明,通過(guò)合理調(diào)整試驗(yàn)參數(shù)可以有效降低銀納米顆粒制備中副產(chǎn)物的數(shù)量,得到直徑為40-100 nm的銀納米線,產(chǎn)率可高達(dá)95%以上。(2)一鍋法制備宏量銀納米線傳統(tǒng)的銀納米線制備工藝需要將反應(yīng)物逐滴加入反應(yīng)體系中,產(chǎn)物數(shù)量為毫克或克級(jí),不利于實(shí)現(xiàn)宏量制備,也無(wú)法滿(mǎn)足工業(yè)需求。因此,我們深入探究了加料方式及溫度對(duì)銀納米線產(chǎn)量的影響,并初步探討了銀納米線的純化和保存,以便為其商業(yè)化提供實(shí)驗(yàn)依據(jù)和技術(shù)支撐。結(jié)果表明,通過(guò)合理控制升溫過(guò)程可以實(shí)現(xiàn)銀納米線的一鍋法宏量制備(反應(yīng)器容積為5 L;單次反應(yīng)產(chǎn)量超過(guò)10 g)。(3)銀納米線透明電極的制備和光電性能研究將不同直徑的銀納米線作為導(dǎo)電材料,以聚對(duì)苯二甲酸乙二醇酯(PET)作為基底材料,利用旋涂方式制備出柔性透明導(dǎo)電薄膜;探究了銀納米線直徑對(duì)透明電極光電性能的影響。結(jié)果表明,通過(guò)優(yōu)化工藝條件,可以制備出透光率達(dá)90%、方阻為70?左右的高性能透明導(dǎo)電薄膜;銀納米線的直徑越細(xì)、長(zhǎng)徑比越大,則透明導(dǎo)電薄膜的光電性能越好。(4)超細(xì)銀納米線的制備銀納米線直徑對(duì)透明導(dǎo)電薄膜的光電性能具有重要影響,而直徑小于25 nm的超細(xì)銀納米線的制備是研制高性能透明導(dǎo)電薄膜的重點(diǎn)和難點(diǎn)。為此,以前述一鍋法為基礎(chǔ),通過(guò)引入NaCl、NiCl_2、NaBr作為控制劑,嘗試制備超細(xì)銀納米線。結(jié)果表明,分別以NaCl-NaBr和NiCl_2-NaBr作為控制劑,以PVP作為修飾劑,可以得到平均直徑為23 nm的超細(xì)銀納米線。
[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.
【學(xué)位授予單位】：河南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類(lèi)號(hào)】：O614.122;TB383.1

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