非水解溶胶-凝胶法制备Cr掺杂α-Al_(2)O_(3)红色色料  

Preparation of Chromium-Doped α-Al_(2)O_(3) Red Pigments by Non-Hydrolytic Sol-Gel Method

作　　者：陈婷 汤惠东 邵川 张筱君 江伟辉 Chen Ting;Tang Huidong;Shao Chuan;Zhang Xiaojun;Jiang Weihui(School of Materials Science and Engineering,Jingdezhen Ceramic Institute,Jingdezhen 333004,China;Institute of Materials Science and Devices,Suzhou University of Science and Technology,Suzhou 215009,China)

机构地区：[1]景德镇陶瓷大学材料科学与工程学院,江西景德镇333004 [2]苏州科技大学材料科学与器件研究院,江苏苏州215009

出　　处：《稀有金属》2021年第8期989-997,共9页Chinese Journal of Rare Metals

基　　金：国家自然科学基金项目(52062019,51774096);景德镇科技局项目(20192GYZD008-15,20192GYZD008-18);江西省高校青蓝工程资助。

摘　　要：以无水三氯化铝(AlCl_(3))和三氯化铬(CrCl_(3))为原料,无水乙醇为溶剂和铝粉为还原剂,采用非水解溶胶-凝胶法制备Cr掺杂α-Al_(2)O_(3)红色色料,通过X射线衍射(XRD)、场发射扫描电镜(FE-SEM)、激光粒度仪和CIE-L*a*b*色度仪等测试手段研究了掺杂离子浓度、Al粉添加量、前驱体浓度和热处理温度对色料的相组成、形貌及呈色性能的影响。结果表明:在Cr^(3+)掺杂浓度为0%-5%(原子分数)范围内,随掺杂浓度增加,α-Al_(2)O_(3)的晶胞参数和晶胞体积均逐渐增大,说明Cr^(3+)成功固溶进入α-Al_(2)O_(3)晶格中。色料红度(a*)值随Cr^(3+)掺杂浓度增加呈现先增加后减少趋势,同时,提高前驱体浓度和还原剂的添加量有利于改善色料的呈色性能;随热处理温度增加,色料a*值先增加后趋于平稳,色料粒径逐渐增大;当Cr^(3+)掺杂浓度为4%(原子分数)、Al粉添加量(与CrCl_(3)摩尔比)为6∶1、前驱体浓度为0.4 mol·L^(-1)时,经1200℃热处理2 h,可制备呈色性能良好(a*=14.32)和粒径较小(平均粒度(D50)=7.85μm)的粉红色色料,其有望应用于陶瓷装饰领域。Red ceramics pigments had pure bright color and intensive tinting capacity,which had been widely applied in the decora-tion fields of ceramic body,glaze and inkjet printing. Chromium(Cr)doped α-Al_(2)O_(3) materialshad drawn great attention due to its purebright color,excellent thermal and chemical stability,which were known as"ruby"or"ruby solution"and could be used as red ceram-ics pigments. Various synthesis methods had been reported for preparing Cr doped α-Al_(2)O_(3) red pigments,which included hydrothermalmethod,Pechini method and combustion method. However,the above-mentioned methods had many disadvantages,such as poor col-or performance,complicated operation and high equipment requirements. Hence,Cr doped α-Al_(2)O_(3) red pigments were prepared bynovel non-hydrolytic sol-gel(NHSG)method using anhydrous aluminum chloride(AlCl_(3))and chromic chloride(CrCl_(3))as raw materi-als,anhydrous ethanol as solvent and Al powders as reducing agents,respectively. The effects of doping concentration,Al powders ad-dition amount,precursor concentration and heat treatment temperature on the phase composition and coloration properties of pigmentswere investigated via X-ray diffraction(XRD),the automatic whiteness meter based on Commission International de I’Elcairage(CIE)system and ultraviolet and visible spectrophotometry(UV-Vis). In addition,the morphology,structure and particle size of pre-pared Cr doped α-Al_(2)O_(3) pigments were studied via field-emission scanning electron microscope(FE-SEM),high resolution transmis-sion electron microscope(HRTEM),and laser particle analyzer. XRD patterns showed that the relative intensity of the sample diffrac-tion peak was gradually weakened,and the angle of diffraction peak was gradually decreased with the increase of doping concentrationin the range of 0%-5%(atom fraction). Further,it could be found that the cell parameters and cell volume of sample gradually en-larged with boosted of Cr^(3+)doping concentration via Rietveld refinement,indicating that Cr^(3+)were success

关 键 词：非水解溶胶-凝胶法 红色色料 铬掺杂 刚玉型(α-Al_(2)O_(3)) 

分 类 号：TK91[动力工程及工程热物理]