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超聲波輔助乙酸溶液球磨制備金屬氧化物納米粉末的研究

發(fā)布時(shí)間:2018-04-12 09:45

  本文選題:超聲波輔助球磨 + 乙酸 ; 參考:《湖南大學(xué)》2015年碩士論文


【摘要】:Sb_2O_3、SnO_2、Bi_2O_3是幾種應(yīng)用廣泛的重要金屬氧化物半導(dǎo)體材料,其可用作光催化劑和鋰電池負(fù)極材料等方面。超聲輔助球磨法是一種將球磨和超聲波結(jié)合起來(lái)的方法。這種合成方法簡(jiǎn)單易行,合成的產(chǎn)物純度較高,生產(chǎn)效率高,具有良好的產(chǎn)業(yè)化前景。本論文開(kāi)展了超聲波輔助乙酸溶液球磨制備Sb_2O_3、SnO_2、Bi_2O_3納米粉末的研究。探討了液體反應(yīng)介質(zhì)(乙酸溶液、純水、乙醇溶液)對(duì)合成納米粒子物相結(jié)構(gòu)的影響,并進(jìn)一步研究了乙酸濃度、超聲波頻率對(duì)合成納米粒子的影響。采用XRD、FT-IR、TEM對(duì)制備產(chǎn)物進(jìn)行表征。此外,對(duì)SnO_2、Bi_2O_3納米粉末的光催化性能以及SnO_2納米粉末的電化學(xué)性能進(jìn)行了初步測(cè)試。(1)通過(guò)超聲波輔助乙酸溶液球磨法成功制備了立方型的Sb_2O_3、金紅石型的SnO_2、單斜晶系的Bi_2O_3納米粉末,其平均粒徑分別為:20 nm、10 nm、20 nm。(2)在乙酸溶液中球磨20 h可以合成Sb_2O_3納米顆粒;而在水和乙醇溶液中球磨36 h,仍不能合成Sb_2O_3納米顆粒;在乙酸溶液中球磨21 h可以合成SnO_2納米顆粒;而在水和乙醇溶液中球磨40 h,仍不能合成SnO_2納米顆粒。對(duì)合成Sb_2O_3、SnO_2而言:乙酸濃度越高,反應(yīng)速率越快。隨著乙酸濃度的升高,反應(yīng)速度的增長(zhǎng)速率越來(lái)越慢。對(duì)合成SnO_2而言:超聲波頻率越低,反應(yīng)速率越快。(3)對(duì)Sb_2O_3納米粒子進(jìn)行在400℃下保溫4 h的熱處理后,可以合成Sb+3Sb+5O4,關(guān)于該物質(zhì)的文獻(xiàn)報(bào)道較少。(4)對(duì)SnO_2、Bi_2O_3納米粉末進(jìn)行光催化降解甲基橙實(shí)驗(yàn)發(fā)現(xiàn):SnO_2納米粉末具有良好的光催化性能;Bi_2O_3納米粉末具有一定的光催化性能。對(duì)SnO_2納米粉末的電化學(xué)性能進(jìn)行測(cè)試發(fā)現(xiàn):在三種濃度乙酸溶液中合成的SnO_2中,在25%乙酸溶液中合成的SnO_2,其電化學(xué)性能最好。它的首次充放電比容量較高,25次循環(huán)后比容量最高,庫(kù)倫效率較高,循環(huán)伏安曲線的峰形最尖銳,穩(wěn)定性最好。
[Abstract]:Sb2O3SnO2Bi2O3 is one of several important metal oxide semiconductor materials, which can be used as photocatalyst and cathode material for lithium battery.Ultrasonic assisted ball milling is a method that combines ball milling with ultrasonic wave.The synthetic method is simple and feasible, the product is of high purity and high production efficiency, and has a good prospect of industrialization.In this paper, ultrasonic assisted milling of acetic acid solution was carried out to prepare SB _ 2O _ 3S _ 2O _ 2S _ 2O _ 2S _ 2O _ 3 nano-powder.The effects of liquid reaction medium (acetic acid solution, pure water, ethanol solution) on the phase structure of synthesized nanoparticles were discussed. The effects of acetic acid concentration and ultrasonic frequency on the synthesis of nanoparticles were further studied.The prepared products were characterized by XRDX FT-IR TEM.In addition, the photocatalytic properties of the SnO2BiSZ _ 2O _ 3 nanometer powder and the electrochemical performance of the SnO_2 nanometer powder were preliminarily tested. (1) cubic type Bi_2O_3 nano-powders were successfully prepared by ultrasonic assisted acetic acid solution milling method, including rutile Sno _ 2, rutile Sno _ 2O _ 2 and monoclinic Bi_2O_3 nanocrystalline powders.Sb_2O_3 nanoparticles could be synthesized by ball milling in acetic acid solution for 20 h, while Sb_2O_3 nanoparticles could not be synthesized in water and ethanol solution for 36 h, and SnO_2 nanoparticles could be synthesized in acetic acid solution for 21 h.However, SnO_2 nanoparticles could not be synthesized by ball milling in water and ethanol solution for 40 h.For the synthesis of SB _ 2O _ 3SnO _ 2, the higher the acetic acid concentration, the faster the reaction rate.With the increase of acetic acid concentration, the growth rate of the reaction rate is slower and slower.For the synthesis of SnO_2, the lower the ultrasonic frequency, the faster the reaction rate.) the Sb_2O_3 nanoparticles were heat-treated at 400 鈩,

本文編號(hào):1739219

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