气相爆轰合成纳米TiO_2粉末的实验研究
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摘要
以H_2/Air预混气体为爆炸源,在自制爆炸反应管中通过气相爆轰制备纳米TiO_2粉末。探讨了不同初始条件(初始温度25~200℃;H_2/Air混合比0.2~0.8)下管内爆轰压力的变化规律,同时借助XRD和TEM对不同初始温度下爆轰合成及高温煅烧的纳米TiO_2粉末的晶粒尺寸、晶相成分、形貌特征等进行表征。结果表明:以化学当量比预混的H_2/Air为爆炸源时,管末端的爆压最大;随着H_2含量的增加,管末端的爆压最终提高了39.03%,且增长速率先增后减;初始温度的上升使管末端的爆压最终降低了36.86%。气相爆轰合成的纳米TiO_2粉末(锐钛矿和金红石混晶),其晶粒尺寸随初始温度的升高先增后减,且其锐钛矿相含量逐渐减少;爆轰产物在高温煅烧过程中,锐钛矿相向金红石相转变的相变温度在700~900℃左右,且产物晶粒尺寸随煅烧温度的上升而逐渐增加。
Using the premixed H_2/Air as explosion source,TiO_2 nanoparticles were prepared by gaseous detonation in a self-made explosion reaction tube.The variation law was discussed of the detonation pressure in the tube under different initial conditions(initial temperature of 25~200℃and H2/Air mixing ratio of 0.2~0.8).Particle size,composition of crystal phase and morphologies of TiO_2 nanoparticles synthesized by detonation at different initial temperature and calcinated at high temperature were characterized by means of XRD and TEM.The results show that the end of the explosion reaction tube has the largest detonation pressure when the premixed H2/Air with the chemical equivalent ratio is employed as explosion source.The detonation pressure at the tube end is increased eventually increased by 39.03% with the increase of H_2/Air mixing ratio,and the increasing rate firstly increases and then decreases.However,the detonation pressure at the tube end is reduced eventually by 36.86% with the initial environmental temperature increasing.The prepared TiO_2 nanoparticles are mixed crystals of anatase and rutile,their grain size increases at first and then decreases with the increase of initial temperature,and the anatase phase is gradually reduced.The phase-transition temperature from anatase to rutile is 700~900 ℃ during high temperature calcination of detonation products,and the grain size is gradually increased with the rise of calcination temperature.
Using the premixed H_2/Air as explosion source,TiO_2 nanoparticles were prepared by gaseous detonation in a self-made explosion reaction tube.The variation law was discussed of the detonation pressure in the tube under different initial conditions(initial temperature of 25~200℃and H2/Air mixing ratio of 0.2~0.8).Particle size,composition of crystal phase and morphologies of TiO_2 nanoparticles synthesized by detonation at different initial temperature and calcinated at high temperature were characterized by means of XRD and TEM.The results show that the end of the explosion reaction tube has the largest detonation pressure when the premixed H2/Air with the chemical equivalent ratio is employed as explosion source.The detonation pressure at the tube end is increased eventually increased by 39.03% with the increase of H_2/Air mixing ratio,and the increasing rate firstly increases and then decreases.However,the detonation pressure at the tube end is reduced eventually by 36.86% with the initial environmental temperature increasing.The prepared TiO_2 nanoparticles are mixed crystals of anatase and rutile,their grain size increases at first and then decreases with the increase of initial temperature,and the anatase phase is gradually reduced.The phase-transition temperature from anatase to rutile is 700~900 ℃ during high temperature calcination of detonation products,and the grain size is gradually increased with the rise of calcination temperature.
引文
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[16]闫鸿浩,吴林松,李晓杰,等.颗粒长大模型在气相爆轰合成纳米材料中的应用[J].稀有金属材料与工程,2015,44(5):1 144-1 148.
[2]曲艳东,孔祥清,李晓杰,等.热处理对爆轰合成的纳米TiO2混晶的结构相变的影响[J].物理学报,2014,63(3):384-389.
[3]文潮,金志浩,关锦清,等.炸药爆轰法制备纳米石墨粉[J].稀有金属材料与工程,2004,33(6):628-631.
[4]QU Y D,SUN C H,SUN G L,et al.Preparation,characterization,and kinetic and thermodynamic studies of mixed-phase TiO2 nanoparticles prepared by detonation method[J].Results in Physics,2016,6:100-106.
[5]LUO N,JING H W,Ma Z G,et al.Growth characteristics of spherical titanium oxide nanoparticles during the rapid gaseous detonation reaction[J].Particuology,2016,26(3):102-107.
[6]韩志伟,解立峰,邓吉平,等.爆轰法合成纳米氧化铈粒径的控制[J].高压物理学报,2014,28(5):585-590.
[7]闫鸿浩,王胜杰,李晓杰,等.初始压力对气相爆轰制备纳米SnO2的影响[J].功能材料,2013,44(20):3 016-3 019.
[8]欧阳欣,闫鸿浩,刘津开,等.纳米二氧化钛粉体的气相爆轰制备[J].高压物理学报,2007,21(4):379-382.
[9]SPURR R A,MYERS H.Quantitative analysis of anatase-rutile mixtures with an X-ray diffractometer[J].Analytical Chemistry,1957,29(5):760-762.
[10]田诗雅,刘剑,高科.密闭管道瓦斯爆炸冲击波冲量及压力上升速率的实验研究[J].中国安全生产科学技术,2015,11(8):16-21.
[11]李润之,黄子超,司荣军.环境温度对瓦斯爆炸压力及压力上升速率的影响[J].爆炸与冲击,2013,33(4):415-419.
[12]赵衡阳.气体和粉尘爆炸原理[M].北京:北京理工大学出版社,1996:161-185.
[13]王华,邓军,葛岭梅.初始压力对矿井可燃性气体爆炸特性的影响[J].煤炭学报,2011,36(3):423-428.
[14]李晓杰,欧阳欣,闫鸿浩,等.气相爆轰压力及环境温度对制备纳米TiO2粉末的影响[J].稀有金属材料与工程,2007,36(Z3):371-373.
[15]曲艳东,李晓杰,刘元.纳米氧化钛团聚结构的研究[J].高压物理学报,2010,24(6):438-442.
[16]闫鸿浩,吴林松,李晓杰,等.颗粒长大模型在气相爆轰合成纳米材料中的应用[J].稀有金属材料与工程,2015,44(5):1 144-1 148.