不同碳源对纳米锌铝尖晶石合成及颗粒粒径的影响  

Effect of Carbon Source on Synthesis and Particle Size of Nano-ZnAl_2O_4

作　　者：文钰斌 刘新红[1] 顾强 陈晓雨[1] 贾全利[1] 杨林[1] 马腾[1] WEN Yubin LIU Xinhong GU Qiang CHEN Xiaoyu JIA Quanli YANG＇Lin MA Teng(Henan Key Laboratory of High Temperature Functional Ceramics, Zhengzhou University, Zhengzhou 45005)

机构地区：[1]郑州大学河南省高温功能材料重点实验室,郑州450052

出　　处：《材料导报》2017年第18期109-113,118,共6页Materials Reports

基　　金：国家自然科学基金面上项目(51672253);河南省重点科技攻关项目(152102410014);河南省科技厅基础研究项目(162300410044)

摘　　要：以硝酸铝、硝酸锌和柠檬酸为原料,以炭黑和酚醛树脂为碳源,采用溶胶-凝胶法制备了纳米锌铝尖晶石粉体,研究了高温还原气氛下不同碳源对纳米锌铝尖晶石合成及颗粒粒径的影响,并以高温氧化气氛热处理、无碳引入的试样作对比。研究表明:在还原气氛下,引入碳源的试样在600℃热处理后,锌铝尖晶石峰不明显,主要是因为碳起空间位阻作用,阻碍了离子传质;800℃热处理后可合成锌铝尖晶石,且纳米颗粒尺寸较小(20~30nm);热处理温度升高至1 000℃时,纳米锌铝尖晶石颗粒尺寸变化不大,碳的空间位阻作用抑制了颗粒长大和烧结。与炭黑相比,酚醛树脂抑制锌铝尖晶石颗粒长大的效果更好,可能因为树脂碳化后呈玻璃态,空间阻隔作用更强。但热处理温度不低于1 200℃时,纳米锌铝尖晶石易被CO或C还原,锌以Zn(g)的形式逸出,只有α-Al2O3相。然而,在空气气氛下,600℃热处理后即可合成纳米锌铝尖晶石,但热处理温度从600℃升至800℃时,锌铝尖晶石颗粒长大较明显,颗粒尺寸从27.5nm增至54.6nm,并呈烧结状。Nano ZnAl2O4 powders were prepared by sol-gel method with aluminum nitrate,zinc nitrate and citric acid as starting material,carbon black and phenolic formaldehyde resin as carbon source.Effect of different carbon source on synthesis and particle size of nano-ZnAl2O4 were studied in reducing atmosphere at high temperature,comparing with samples which conducted heat treatment in air without carbon addition.The results showed that XRD peaks of samples with carbon addition were not detected after heat treatment at 600 ℃in reducing atmosphere.The reason was that carbon acts as steric hindrance,which inhibited ions movement.Nano ZnAl2O4 with fine particles（20—30 nm）could be synthesized at 800℃ with carbon addition,and nano-ZnAl2O4 particle size was almost no change when the temperature increased from 800 ℃ to 1 000 ℃.Carbon surrounding the ZnAl2O4 particles prevented effectively the growth and sintering of the particles.Phenolic resin was better than carbon black for inhibiting ZnAl2O4 particle growth,which might be phenolic resin carbonized with some glassy carbon,leading to better retarding effect.But when the temperature was no less than 1 200℃,ZnAl2O4 was easy to react with CO or C to form volatile Zn（g）,there was only single crystal phaseα-Al2O3.However,nano-ZnAl2O4 particles could be synthesized at 600℃in air without carbon addition,but the particles increased noticeably（from 27.5 nm to 54.6 nm）with temperature increasing from 600 ℃ to 800 ℃,and the particles exhibited sintered state.

关 键 词：溶胶-凝胶法 锌铝尖晶石 酚醛树脂 炭黑 纳米颗粒 

分 类 号：TB35[一般工业技术—材料科学与工程]