微波法快速合成納米銀及影響因素研究
發(fā)布時(shí)間：2019-02-24 15:35
【摘要】：納米銀材料由于顯示出獨(dú)特的性能,如小尺寸效應(yīng)、表面效應(yīng)和量子隧道效應(yīng)等,成為現(xiàn)階段科學(xué)研究的熱點(diǎn),并且在催化、消費(fèi)電子、醫(yī)學(xué)等領(lǐng)域有著廣泛的應(yīng)用。銀納米材料的性能主要取決于銀粒子的大小和形貌,因此制備高性能納米銀的關(guān)鍵是精確控制顆粒尺寸和形貌。作為一種合成納米材料的新方法,微波輔助法與傳統(tǒng)方法相比,具有巨大的優(yōu)點(diǎn),如微波的穿透能力比較強(qiáng),加熱更均勻,清潔高效、污染小。本課題主要采用微波輔助合成法,在微波輔助加熱條件下,以硝酸銀(AgNO3)為銀源,乙二醇(EG)作為溶劑和還原劑,聚乙烯吡咯烷酮(PVP)作為表面活性劑,氯化鈉(NaCl)或者硫化鈉(Na2S)作為形貌控制劑,通過調(diào)整反應(yīng)條件及反應(yīng)物配比,并運(yùn)用紫外-可見吸收光譜儀(UV-Vis)、X射線衍射儀(XRD)、透射電鏡(TEM)和場(chǎng)發(fā)射掃描電鏡(SEM)等儀器觀察分析產(chǎn)物的形狀與尺寸,探討影響納米銀形貌和粒徑大小的因素。全文主要內(nèi)容包括以下三部分:(1)納米銀線的制備:采用微波輔助加熱,以NaC l為形貌控制劑,探討反應(yīng)時(shí)間、溫度、反應(yīng)物配比、微波功率和氯化鈉濃度等因素對(duì)納米銀線形貌和尺寸的影響。最終取得最佳的制備工藝:微波功率為300 W,AgNO3與PVP質(zhì)量比為1:2.5,NaCl濃度為2.5 mM,反應(yīng)時(shí)間4 min,溫度控制為190oC。在此基礎(chǔ)上合成了直徑約40 nm、長(zhǎng)度約15μm、形貌均一的高純納米銀線,并進(jìn)一步探討納米銀線的生長(zhǎng)機(jī)制。(2)納米銀立方塊的制備:利用微波法,以Na2S作為形貌控制劑,通過改變Na2S濃度、PVP與硝酸銀的質(zhì)量比、反應(yīng)溫度和時(shí)間等條件得出銀立方塊的最佳生成條件:微波功率為300 W,PVP質(zhì)量為0.68 g,AgNO3質(zhì)量為0.17 g,Na2S濃度為375mM,反應(yīng)時(shí)間4 min,反應(yīng)溫度180oC。并且成功制備出完整形貌的納米銀立方塊,并進(jìn)一步探討了納米銀立方塊的生長(zhǎng)機(jī)理。(3)高濃度球形納米銀顆粒的制備:利用多元醇的弱還原性和微波輔助法的高反應(yīng)效率,將多元醇法和微波輔助法結(jié)合制備納米銀顆粒,詳細(xì)分析了反應(yīng)時(shí)間、溫度、反應(yīng)物配比和硫化鈉濃度等條件對(duì)產(chǎn)物的影響并在10 min內(nèi)制備出了高濃度(0.5M)、小粒徑(10 nm)、窄粒徑分布(2-6 nm)的納米銀顆粒。
[Abstract]:Due to their unique properties, such as small size effect, surface effect and quantum tunneling effect, silver nanocrystalline materials have been widely used in the fields of catalysis, consumer electronics, medicine and so on. The properties of silver nanoparticles mainly depend on the size and morphology of silver particles, so the key to the preparation of high performance silver nanoparticles is to accurately control the size and morphology of silver nanoparticles. As a new method of synthesizing nanomaterials, microwave assisted method has great advantages compared with traditional methods, such as strong penetrating ability of microwave, more uniform heating, clean and efficient, and less pollution. In this paper, microwave-assisted synthesis was carried out under the condition of microwave-assisted heating, silver nitrate (AgNO3) as silver source, ethylene glycol (EG) as solvent and reductant, polyvinylpyrrolidone (PVP) as surfactant, and polyvinylpyrrolidone (PVP) as surfactant. Sodium chloride (NaCl) or sodium sulfide (Na2S) were used as morphology control agents. By adjusting reaction conditions and reactants ratio, UV-Vis absorption spectrometer (XRD),) was used. The shape and size of the products were observed by transmission electron microscope (TEM) and field emission scanning electron microscopy (SEM), and the factors affecting the morphology and particle size of silver nanoparticles were discussed. The main contents of this paper are as follows: (1) preparation of nanocrystalline silver wire: microwave assisted heating, NaC l as morphology control agent, reaction time, temperature, reactant ratio, etc. Effects of microwave power and concentration of sodium chloride on the morphology and size of silver nanowires. The optimal preparation process was obtained as follows: microwave power of 300W Agno _ 3 to PVP was 1: 2.5 mM, reaction time was 2.5 mM, reaction time was 4 min, and the temperature was 190oC. On this basis, high purity silver nanowires with a diameter of about 40 nm, about 15 渭 m in length and uniform morphology were synthesized, and the growth mechanism of nanocrystalline silver nanowires was further discussed. (2) preparation of silver nanocrystalline cubes: Na2S was used as the morphology control agent by microwave method. By changing the concentration of Na2S, the mass ratio of PVP to silver nitrate, the reaction temperature and time, the optimum conditions for the formation of silver cubic block were obtained: microwave power of 300WN PVP, mass of 0.68g / Agno _ 3, mass of 0.17 g / na _ 2S, concentration of 375mM, etc. The reaction temperature was 180oC at 4 min,. And successfully prepared nano-silver square with complete morphology, The growth mechanism of nanocrystalline silver cube was also discussed. (3) preparation of high concentration spherical silver nanoparticles: the weak reduction of polyols and the high reaction efficiency of microwave-assisted method. The effects of reaction time, temperature, ratio of reactants and concentration of sodium sulfide on the preparation of silver nanoparticles were analyzed in detail, and a high concentration (0.5 M) of silver nanoparticles was prepared in 10 min. Silver nanoparticles with small particle size (10 nm), narrow particle size distribution (2-6 nm).
【學(xué)位授予單位】：華中科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB383.1;O614.122
本文編號(hào)：2429682
[Abstract]:Due to their unique properties, such as small size effect, surface effect and quantum tunneling effect, silver nanocrystalline materials have been widely used in the fields of catalysis, consumer electronics, medicine and so on. The properties of silver nanoparticles mainly depend on the size and morphology of silver particles, so the key to the preparation of high performance silver nanoparticles is to accurately control the size and morphology of silver nanoparticles. As a new method of synthesizing nanomaterials, microwave assisted method has great advantages compared with traditional methods, such as strong penetrating ability of microwave, more uniform heating, clean and efficient, and less pollution. In this paper, microwave-assisted synthesis was carried out under the condition of microwave-assisted heating, silver nitrate (AgNO3) as silver source, ethylene glycol (EG) as solvent and reductant, polyvinylpyrrolidone (PVP) as surfactant, and polyvinylpyrrolidone (PVP) as surfactant. Sodium chloride (NaCl) or sodium sulfide (Na2S) were used as morphology control agents. By adjusting reaction conditions and reactants ratio, UV-Vis absorption spectrometer (XRD),) was used. The shape and size of the products were observed by transmission electron microscope (TEM) and field emission scanning electron microscopy (SEM), and the factors affecting the morphology and particle size of silver nanoparticles were discussed. The main contents of this paper are as follows: (1) preparation of nanocrystalline silver wire: microwave assisted heating, NaC l as morphology control agent, reaction time, temperature, reactant ratio, etc. Effects of microwave power and concentration of sodium chloride on the morphology and size of silver nanowires. The optimal preparation process was obtained as follows: microwave power of 300W Agno _ 3 to PVP was 1: 2.5 mM, reaction time was 2.5 mM, reaction time was 4 min, and the temperature was 190oC. On this basis, high purity silver nanowires with a diameter of about 40 nm, about 15 渭 m in length and uniform morphology were synthesized, and the growth mechanism of nanocrystalline silver nanowires was further discussed. (2) preparation of silver nanocrystalline cubes: Na2S was used as the morphology control agent by microwave method. By changing the concentration of Na2S, the mass ratio of PVP to silver nitrate, the reaction temperature and time, the optimum conditions for the formation of silver cubic block were obtained: microwave power of 300WN PVP, mass of 0.68g / Agno _ 3, mass of 0.17 g / na _ 2S, concentration of 375mM, etc. The reaction temperature was 180oC at 4 min,. And successfully prepared nano-silver square with complete morphology, The growth mechanism of nanocrystalline silver cube was also discussed. (3) preparation of high concentration spherical silver nanoparticles: the weak reduction of polyols and the high reaction efficiency of microwave-assisted method. The effects of reaction time, temperature, ratio of reactants and concentration of sodium sulfide on the preparation of silver nanoparticles were analyzed in detail, and a high concentration (0.5 M) of silver nanoparticles was prepared in 10 min. Silver nanoparticles with small particle size (10 nm), narrow particle size distribution (2-6 nm).
【學(xué)位授予單位】：華中科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB383.1;O614.122
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