發(fā)布時(shí)間：2018-04-15 03:30

  本文選題：多孔陽極氧化鋁(PAA) + 電化學(xué)沉積�。� 參考：《浙江理工大學(xué)》2017年碩士論文

【摘要】：模板法操作容易,設(shè)備簡單,并且可以通過調(diào)節(jié)所用模板的孔徑大小和厚度來控制合成材料的直徑和長度,這一特點(diǎn)為納米器件的制備及應(yīng)用提供了基礎(chǔ)。本論文選用模板多孔陽極氧化鋁模板與電化學(xué)沉積相結(jié)合,通過控制反應(yīng)中的化學(xué)條件成功合成了保持本征特性的單晶銀納米線、鐵納米線一維材料,并研究了其形貌及結(jié)構(gòu)。通過溶劑熱與超聲方法相結(jié)合將一維金屬納米材料轉(zhuǎn)化為零維納米顆粒,制備了具有本征特性的納米粒子,成功實(shí)現(xiàn)了金屬納米線的低維化,討論了反應(yīng)時(shí)間以及反應(yīng)溫度等因素對所得產(chǎn)物形貌與結(jié)構(gòu)的影響,避免了化學(xué)法合成中為了防止納米粒子發(fā)生團(tuán)聚,在反應(yīng)體系中加入分散劑等表面活性劑而產(chǎn)生的繁雜后處理,同時(shí)保持了納米粒子的本征特性。采用掃描電鏡(SEM),透射電鏡(TEM),紫外可見吸收光譜(UV-Vis),X-射線衍射(XRD)以及能譜(EDS)對一維納米材料金屬納米線和低維化的金屬納米粒子進(jìn)行了基礎(chǔ)分析表征。本論文所做的有研究主要有以下方面的工作:銀納米線陣列的制備:首先在多孔陽極氧化鋁(PAA)模板的一側(cè)蒸鍍金屬(一般蒸鍍金屬為Ag/Au,Ag蒸鍍13 min,Au蒸鍍10 min)作為工作電極,然后再電化學(xué)恒電位(-0.8V)沉積銀納米線,銀電解液為28.7 g/L Ag電解液,至電流急劇上升時(shí)停止沉積,沉積完成后,用物理方法打磨除去Ag工作電極,然后將樣品溶解在3M NaOH中震蕩溶解PAA模板,用去離子水進(jìn)行離心洗滌3~5次,之后放入真空干燥器中干燥12 h,即得銀納米線陣列。鐵納米線陣列的制備:首先在PAA模板的一側(cè)蒸鍍金屬(一般蒸鍍金屬為Ag/Au,Ag蒸鍍13 min,Au蒸鍍10 min)作為工作電極,然后再電化學(xué)恒電位(-0.9V)沉積鐵納米線。鐵電解液:FeSO4·7H2O 120 g/L,H3BO3 45 g/L,Vc1 g/L。先沉積4 min的Ag,再沉積Fe納米線,至電流下降至0時(shí)停止沉積,沉積完成后,用物理方法打磨除去Ag工作電極和犧牲電極銀,然后將樣品溶解在3M NaOH中震蕩溶解PAA模板,用去離子水進(jìn)行離心洗滌3~5次,之后放入真空干燥器中干燥12 h,即得鐵納米線陣列。將陽極氧化鋁模板結(jié)合電化學(xué)沉積制備的納米線利用溶劑熱與超聲結(jié)合的方式將納米線低維化,首先將制備好的納米線在設(shè)定的溫度下進(jìn)行電磁攪拌或者機(jī)械攪拌攪拌,自然冷卻至室溫后,將在設(shè)定的溫度下電磁攪拌得到的樣品,進(jìn)行超聲浴或者超聲探頭進(jìn)行超聲處理,即可將納米線低維化處理成為納米顆粒。該方法可以將單晶的納米線轉(zhuǎn)化為單晶的納米粒子。結(jié)果表明,在以N-甲基吡咯烷酮為溶劑時(shí),通過改變?nèi)軇�熱反�?yīng)時(shí)間、反應(yīng)溫度或超聲時(shí)間、方式等均可生成銀納米粒子的溶膠,研究了溶劑熱反應(yīng)溫度、反應(yīng)時(shí)間,超聲時(shí)間、方式等因素對納米粒子形貌、尺寸的影響。
[Abstract]:The template method is easy to operate and the equipment is simple, and the diameter and length of the synthesized material can be controlled by adjusting the pore size and thickness of the template, which provides the basis for the fabrication and application of nanodevices.In this paper, single crystal silver nanowires and iron nanowires were successfully synthesized by using porous anodic alumina template and electrochemical deposition, and their morphology and structure were studied.One-dimensional metal nanocrystals were transformed into zero-dimensional nanoparticles by solvothermal and ultrasonic methods, and nanocrystalline nanoparticles with intrinsic properties were prepared, and the low-dimensional metal nanowires were successfully realized.The effects of reaction time and reaction temperature on the morphology and structure of the products were discussed.The complex post-treatment produced by the addition of surfactants such as dispersants in the reaction system keeps the intrinsic properties of the nanoparticles at the same time.Scanning electron microscopy (SEM), transmission electron microscope (TEM), UV-Vis absorption spectrum (UV-Vis) -X ray diffraction (XRD) and energy dispersive spectroscopy (EDS) were used to characterize one-dimensional metal nanowires and low-dimensional metal nanoparticles.The main work of this thesis is as follows: the preparation of silver nanowire array: firstly, the metal was evaporated on the side of the porous anodic aluminum oxide (PAA) template (the common metal was evaporated by Ag / Au-Ag for 13 min or 10 min) as the working electrode.The silver nanowires were deposited by electrochemical potentiostatic deposition. The silver electrolyte was 28.7 g / L Ag electrolyte. After the deposition was finished, the Ag working electrode was removed by physical method.Then the sample was dissolved in 3M NaOH and the PAA template was dissolved in 3M NaOH. The silver nanowire array was obtained by centrifugation with deionized water for 5 times and then dried in a vacuum dryer for 12 hours.Preparation of iron nanowire arrays: first, the metal was evaporated on one side of the PAA template (the general evaporation metal was Ag / Au-Ag vaporized for 13 min or 10 min) as the working electrode, and then the electrochemically constant potential (-0.9V) was used as the working electrode for the deposition of iron nanowires.Iron electrolyte: FeSO4 7H2O 120 g / L H3BO3 45 g / L Vc 1 g / L.After deposition, Ag working electrode and sacrificial electrode silver were removed by physical method, then the sample was dissolved in 3M NaOH to dissolve PAA template, and the Ag was deposited for 4 min, then Fe nanowires were deposited. After the deposition was finished, the Ag working electrode and sacrificial electrode silver were removed by physical method.Iron nanowire arrays were obtained by centrifugation with deionized water for 5 times and then dried in a vacuum dryer for 12 hours.The nanowires prepared by anodic alumina template and electrochemical deposition were prepared by solvothermal and ultrasonic methods. Firstly, the prepared nanowires were agitated by electromagnetic or mechanical stirring at a given temperature.After natural cooling to room temperature, the samples obtained by electromagnetic stirring at a given temperature were treated by ultrasonic bath or ultrasonic probe, and the nanowires were treated into nanocrystalline particles by low-dimensional treatment.This method can transform the nanowires of single crystals into single crystal nanoparticles.The results show that the sols of silver nanoparticles can be obtained by changing the solvothermal reaction time, reaction temperature or ultrasonic time when N-methylpyrrolidone is used as solvent. The solvothermal reaction temperature and reaction time are studied.The influence of ultrasonic time, mode and other factors on the morphology and size of nanoparticles.
【學(xué)位授予單位】：浙江理工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O614.123;TB383.1

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本文編號：1752343