本文選題：銀納米材料 + 快速制備��； 參考：《安徽工業(yè)大學(xué)》2017年碩士論文

【摘要】：銀納米材料具有獨(dú)特的物理化學(xué)性質(zhì),在光學(xué)、電子學(xué)、熱學(xué)以及生物醫(yī)藥等領(lǐng)域表現(xiàn)出特殊的功能,從而被廣泛應(yīng)用作抗菌材料、催化材料、電子元器件和防靜電材料等。眾所周知,銀納米材料的性能及應(yīng)用主要決定于其粒徑、形貌和穩(wěn)定性,因此,銀納米材料的可控制備,己經(jīng)成為當(dāng)今納米材料研究的熱點(diǎn)之一。本研究首先以葡萄糖(C_6H_(12)O_6)為還原劑、硝酸銀(AgNO_3)為銀源,聚乙烯吡咯烷酮(PVP)為分散劑,采用液相還原法在室溫水體系中快速制備了不同濃度的銀納米膠體,借助于紫外-可見光分析(UV-Vis)、X-射線分析(XRD)和透射電子顯微鏡(TEM)對(duì)銀納米粒子(Ag nanoparticles,AgNPs)的尺寸、結(jié)構(gòu)和形貌進(jìn)行了表征,結(jié)果表明:當(dāng)反應(yīng)體系中AgNO_3與C_6H_(12)O_6摩爾比為1:2,AgNO_3與NaOH的摩爾比為2:(3-4),AgNO_3與PVP的質(zhì)量比為3:1-4:1,可制得穩(wěn)定性良好、粒徑為30-55 nm、具有面心立方結(jié)構(gòu)(FCC)不同濃度的球形銀納米膠體。同時(shí)將制備的AgNPs用于痕量過氧化氫(H_2O_2)的檢測(cè),檢測(cè)表明:銀納米膠體表面等離子共振峰強(qiáng)度變化與H_2O_2濃度呈線性關(guān)系,H_2O_2的檢測(cè)靈敏度高,檢測(cè)限為5.0′10-7mol/L。其次以高化學(xué)活性的鋁粉(Al)作為還原劑,氧化銀(Ag2O)作為氧化劑,利用燃燒合成法制備了AgNPs,采用場(chǎng)發(fā)射掃描電子顯微鏡(FE-SEM)、XRD和TEM對(duì)AgNPs的尺寸、形貌和結(jié)構(gòu)進(jìn)行了表征,并對(duì)AgNPs的形成機(jī)理和表面增強(qiáng)拉曼效應(yīng)進(jìn)行了研究。結(jié)果表明:利用該法可快速制備出具有FCC結(jié)構(gòu)、平均粒徑為40nm球形AgNPs。高速攝像測(cè)試(HSVR)和密閉爆發(fā)器測(cè)試(CBT)表明燃燒合成法制備AgNPs的形成機(jī)制為:瞬間釋放的大量能量使反應(yīng)以484-840 m/s的速度快速進(jìn)行并迅速蔓延,且在此過程中銀的成核速率大于生長速率。同時(shí)以結(jié)晶紫(CV)作為探針分子,對(duì)AgNPs作為基底的表面增強(qiáng)拉曼效應(yīng)(SERS)進(jìn)行了研究,結(jié)果證實(shí),CV在AgNPs表面吸附均一,其表面增強(qiáng)拉曼因子平均達(dá)到9.35×103。最后以AgNO_3為銀源,水熱合成的片狀二氧化鈦(TiO_2)為載體,環(huán)三亞甲基三硝胺(RDX)為高能物質(zhì),采用爆燃法制備了Ag/TiO_2納米復(fù)合物。XRD、X射線光電子能譜分析(XPS)、TEM和UV-Vis測(cè)試結(jié)果表明:該法可以實(shí)現(xiàn)在TiO_2界面上一步負(fù)載5-10 nm的純相AgNPs。同時(shí)考察了其作為催化劑,光催化降解羅丹明B(RhB)的催化活性,結(jié)果表明Ag/TiO_2納米復(fù)合物比TiO_2納米片具有更強(qiáng)的光催化性能,其光催化動(dòng)力學(xué)常數(shù)隨著AgNPs含量的增加而增大,當(dāng)AgNO_3與TiO_2納米片質(zhì)量比為0.1、0.2和0.3時(shí),光催化動(dòng)力學(xué)常數(shù)分別為0.326,0.437和0.511 min-1,是TiO_2納米片的9.48,12.70和14.85倍。進(jìn)一步研究表明Ag/TiO_2納米復(fù)合物的光催化機(jī)理為納米銀粒子的高導(dǎo)電性和Ag/TiO_2界面的構(gòu)建使得TiO_2激發(fā)產(chǎn)生的電子可以迅速的遷移到銀顆粒上,實(shí)現(xiàn)光生電子空穴的有效分離并減少其復(fù)合機(jī)率。
[Abstract]:Due to its unique physical and chemical properties, silver nanomaterials are widely used as antibacterial materials, catalytic materials, electronic components and antistatic materials for their special functions in the fields of optics, electronics, thermodynamics and biomedicine. As we all know, the properties and applications of silver nanomaterials are mainly determined by their particle size, morphology and stability. Therefore, the controllable preparation of silver nanomaterials has become one of the hotspots in the research of nanomaterials. In this study, silver nanoparticles of different concentrations were prepared by liquid phase reduction method with glucose (C _ 6H _ (12) O _ (6) O _ (6) as reductant, silver nitrate (Agno _ 3) as silver source and polyvinylpyrrolidone (PVP) as dispersant. The size, structure and morphology of silver nanoparticles were characterized by UV-Vis X-ray analysis (XRD) and transmission electron microscopy (TEM). The results show that when the molar ratio of AgNOSTAL _ 3 to C _ 6H _ (12) O _ 6 is 1: 2Agno _ 3 to NaOH is 2: (3-4) the mass ratio of Agno _ 3 to PVP is 3: 1-4: 1, the spherical silver nanoparticles with FCC structure (FCC) of different concentrations can be prepared with good stability. At the same time, the AgNPs were used for the determination of trace hydrogen peroxide (H _ 2O _ 2). The results showed that there was a linear relationship between the change of surface plasmon resonance peak intensity of silver nanoparticles and the concentration of H _ 2O _ 2. The detection sensitivity of H _ S _ 2O _ 2 was high, and the detection limit was 5.0 ~ (-7) mol / L. Secondly, Ag-NPs were prepared by combustion synthesis with highly chemically active aluminum powder (Al) as reducing agent and silver oxide (Ag2O) as oxidant. The size, morphology and structure of AgNPs were characterized by field emission scanning electron microscopy (FE-SEM) and TEM. The formation mechanism and surface enhanced Raman effect of AgNPs were studied. The results show that 40nm spherical AgNPs with average particle size can be prepared rapidly by this method. High speed camera test (HSVR) and closed burst test (CBT) showed that the formation mechanism of agNPs prepared by combustion synthesis method was that the reaction was carried out at 484-840 m / s and spread rapidly because of a large amount of energy released instantly. In this process, the nucleation rate of silver is higher than the growth rate. At the same time, the surface enhanced Raman effect (SERS) of AgNPs as substrate was studied with crystal violet (CV) as the probe molecule. The results showed that the adsorption of CV on AgNPs was uniform, and the average surface-enhanced Raman factor was 9.35 脳 103. Finally, Agno _ 3 was used as silver source, TIO _ 2 as carrier and cyclotrimethylene trinitramine (RDX) as high energy substance. The results of X-ray photoelectron spectroscopy (XPS), TEM and UV-Vis measurements of Ag/ TiO-2 nanocomposites prepared by deflagration method show that the pure phase AgNPs with 5-10 nm loading can be realized by this method at the TiOStap2 interface. The photocatalytic degradation of Rhodamine B (RhB) was also investigated. The results showed that Ag- / TiO2 nanocomposites had stronger photocatalytic properties than TiO-2 nanochips, and their photocatalytic kinetic constants increased with the increase of AgNPs content. When the mass ratio of Agno _ 3 to TIO _ 2 is 0.10.2,0.3, the photocatalytic kinetic constants are 0.3260.37 and 0.511 min-1, respectively, which is 9.48% 12.70 and 14.85 times of that of TIO _ 2. Further studies show that the photocatalytic mechanism of Ag- / TiO2 nanocomposites is the high conductivity of Ag nanoparticles and the construction of Ag- / TiO2 interface so that the electrons excited by TiO2 can migrate to the silver particles rapidly. The effective separation of photogenerated electron holes is realized and the recombination probability is reduced.
【學(xué)位授予單位】：安徽工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TB383.1;TQ131.22

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本文編號(hào)：2061381