ZnAl_2O_4纳米颗粒的固相合成及其机理研究  

Solid state synthesis and reaction process analysis of ZnAl_2O_4 nanoparticles

作　　者：王骏[1] 徐波[1] 李生娟[2] 

机构地区：[1]上海理工大学能源与动力工程学院,上海200093 [2]上海理工大学材料科学与工程学院,上海200093

出　　处：《电子元件与材料》2016年第12期21-25,共5页Electronic Components And Materials

基　　金：国家自然科学基金资助项目(No.51402192)

摘　　要：结合机械力化学与声化学反应,固相合成尖晶石型Zn Al_2O_4纳米颗粒。借助于X射线衍射仪（XRD）、扫描电子显微镜（SEM）和透射电子显微镜（TEM）,分析样品的表面形貌、晶体结构、化学成分及反应过程。研究结果表明：振动研磨2 h后,Al颗粒尺寸大约为0.5μm,颗粒内部存在大量的位错缺陷,有利于机械力化学反应。将研磨后的Al颗粒超声水解3 h制备出Al（OH）_3白色乳胶液,经干燥、焙烧后得到多孔、片状、活性γ-Al_2O_3纳米颗粒,颗粒尺寸分布在30～150 nm之间。将Zn O/γ-Al_2O_3固相合成制备出尖晶石型Zn Al_2O_4纳米颗粒,在温度为200～600℃范围内,Zn O/γ-Al_2O_3完成了晶核成型、晶体生长和颗粒成型过程,600℃时颗粒尺寸为30～50 nm,且具有良好的分散性。随着温度升高,颗粒尺寸增大,结晶度提高。Combined mechanochemical reaction and sonochemical reaction, Zn Al_2O_4 spinel nanoparticles were synthesized by a solid state reaction route. By means of X-ray diffraction（XRD）, scanning electron microscope（SEM） and transmission electron microscope（TEM）, the surface morphology, crystal structure, chemical composition and reaction process of the sample were analyzed. The research results show that the particles size of the Al powder milled for 2 h is about 0.5 μm, and there are a large number of dislocation defects in the interior of the particles, which is advantageous to the mechanochemical reaction. The Al particles milled for 2 h are hydrolyzed by the ultrasonic to obtain the Al（OH）_3emulsion, and the chemical reaction is quickly completed in a short time because of the synergistic action of mechanochemistry and sonochemistry. Next, the active γ-Al_2O_3 nanoparticles, which are porous and flake, are obtained by drying and roasting, whose particle size distribution is in the range of 30-150 nm. As a result, the Zn O and γ-Al_2O_3 nanoparticles are synthesized to prepare Zn Al_2O_4 spinel nanoparticles by the solid phase reaction. In the temperature range of 200 ℃ to 600 ℃, the Zn O/γ-Al_2O_3 completes the process of crystal nucleation, crystal growth and particle formation, and the particle size is 30-50 nm at 600 ℃. In addition, it has good dispersity. Further research shows that the particle size and crystallinity gradually increases with the increase of roasting temperature.

关 键 词：ZNAL2O4 纳米材料 机械力化学 声化学 固相合成 振动研磨 

分 类 号：TB34[一般工业技术—材料科学与工程] TB321