超声波辅助乙酸溶液球磨制备金属氧化物纳米粉末的研究

发布时间：2018-04-12 09:45

  本文选题：超声波辅助球磨 + 乙酸　； 参考：《湖南大学》2015年硕士论文

【摘要】：Sb_2O_3、SnO_2、Bi_2O_3是几种应用广泛的重要金属氧化物半导体材料,其可用作光催化剂和锂电池负极材料等方面。超声辅助球磨法是一种将球磨和超声波结合起来的方法。这种合成方法简单易行,合成的产物纯度较高,生产效率高,具有良好的产业化前景。本论文开展了超声波辅助乙酸溶液球磨制备Sb_2O_3、SnO_2、Bi_2O_3纳米粉末的研究。探讨了液体反应介质(乙酸溶液、纯水、乙醇溶液)对合成纳米粒子物相结构的影响,并进一步研究了乙酸浓度、超声波频率对合成纳米粒子的影响。采用XRD、FT-IR、TEM对制备产物进行表征。此外,对SnO_2、Bi_2O_3纳米粉末的光催化性能以及SnO_2纳米粉末的电化学性能进行了初步测试。(1)通过超声波辅助乙酸溶液球磨法成功制备了立方型的Sb_2O_3、金红石型的SnO_2、单斜晶系的Bi_2O_3纳米粉末,其平均粒径分别为:20 nm、10 nm、20 nm。(2)在乙酸溶液中球磨20 h可以合成Sb_2O_3纳米颗粒;而在水和乙醇溶液中球磨36 h,仍不能合成Sb_2O_3纳米颗粒;在乙酸溶液中球磨21 h可以合成SnO_2纳米颗粒;而在水和乙醇溶液中球磨40 h,仍不能合成SnO_2纳米颗粒。对合成Sb_2O_3、SnO_2而言:乙酸浓度越高,反应速率越快。随着乙酸浓度的升高,反应速度的增长速率越来越慢。对合成SnO_2而言:超声波频率越低,反应速率越快。(3)对Sb_2O_3纳米粒子进行在400℃下保温4 h的热处理后,可以合成Sb+3Sb+5O4,关于该物质的文献报道较少。(4)对SnO_2、Bi_2O_3纳米粉末进行光催化降解甲基橙实验发现:SnO_2纳米粉末具有良好的光催化性能;Bi_2O_3纳米粉末具有一定的光催化性能。对SnO_2纳米粉末的电化学性能进行测试发现:在三种浓度乙酸溶液中合成的SnO_2中,在25%乙酸溶液中合成的SnO_2,其电化学性能最好。它的首次充放电比容量较高,25次循环后比容量最高,库伦效率较高,循环伏安曲线的峰形最尖锐,稳定性最好。
[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，

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