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前驱体煅烧法制备CeO2颗粒及其抛光性能的研究
引用本文:陈向晖,赵东,裴文利,杨兴波.前驱体煅烧法制备CeO2颗粒及其抛光性能的研究[J].稀有金属,2021(2):251-256.
作者姓名:陈向晖  赵东  裴文利  杨兴波
作者单位:东北大学材料科学与工程学院材料各向异性与织构教育部重点实验室;德米特(苏州)电子环保材料有限公司
基金项目:国家自然科学基金项目(51871045)资助。
摘    要:以Ce(OH)3为前驱体,采用前驱体煅烧法制备CeO2抛光粉。通过调节煅烧温度、升温速率和保温时间获得的具有不同比表面积的CeO2颗粒样品,将样品球磨破碎,制备出中位粒径为(1.0±0.1)μm的CeO2抛光液。通过分析CeO2抛光液对K9玻璃的抛光切削量和表面粗糙度Ra值来评价其抛光性能,采用比表面仪(BET)、X射线衍射仪(XRD)、扫描电镜(SEM)、透射电镜(TEM)和原子力显微镜(AFM)等表征手段对样品的比表面积、物相组成、微观组织结构和抛光玻璃表面粗糙度进行分析,结果表明:前驱体Ce(OH)3煅烧可以制备具有立方萤石结构、尺寸均匀的纳米级CeO2抛光粉,煅烧温度的升高,保温时间的延长和升温速率降低均会使CeO2颗粒的比表面积减小。CeO2颗粒的比表面积是其抛光性能的关键,比表面积越小切削能力越强,本实验样品对K9玻璃的切削量最大可达900 nm·min-1,此外,比表面积对玻璃抛光质量也有重要影响,在比表面积为5 m2·g-1时,获得的玻璃表面粗糙度小,玻璃表面质量高。

关 键 词:CeO2  前驱体煅烧法  比表面积  切削量  粗糙度

Preparation and Polishing Properties of CeO2Particles Fabricated by Precursor Calcination Method
Chen Xianghui,Zhao Dong,Pei Wenli,Yang Xingbo.Preparation and Polishing Properties of CeO2Particles Fabricated by Precursor Calcination Method[J].Chinese Journal of Rare Metals,2021(2):251-256.
Authors:Chen Xianghui  Zhao Dong  Pei Wenli  Yang Xingbo
Affiliation:(Key Laboratory for Anisotropy and Texture of Materials(Ministry of Education),School of Materials Scienceand Engineering,Northeastern University,Shenyang110819,China;Demeter(Suzhou)Electronic Environmental Protection Material Co.,Ltd.,Suzhou215000,China)
Abstract:As an important rare earth oxide functional material,CeO2powder had been widely used as polishing material in recent years.The unique chemical mechanical polishing performance of CeO2provided a new idea for the global planarization of optical glass,silicon crystal and other materials,and became an important polishing product in the field of precision optics.At present,the precursor calcination method had become one of the main methods for batch production of CeO2powder because of its simple process,low production cost and large-scale application.Under different calcination process conditions,the specific surface area of CeO2particles prepared under the same calcination process conditions was quite different due to different temperature zones in roller kiln and different holding time.The effect of CeO2particles with the same specific surface area on the polishing performance was still unclear,so it was a hot research direction to study the relationship between the specific surface area and the polishing performance,and then improve the calcination process to obtain uniform CeO2particles with appropriate specific surface area to improve the polishing performance.In this paper,Ce(OH)3was used as the precursor material.During the experiment,appropriate amount of Ce(OH)3was directly calcined in muffle furnace.The calcination process was adjusted by setting different calcination temperature,heating rate and holding time.After the calcination of raw material,the powder particles of calcined product were refined.According to the material water mass ratio of 1:3 and the material ball mass ratio of 1:10,appropriate amount of calcined samples were put into YFFX16/13 QYC stirring ball mill.The ball milling was carried out in YC type stirring ball mill.The rotation speed of the ball mill was set at 35 r·min-1.The particle size distribution of CeO2was monitored by Malvern 2000 E laser particle size analyzer.When the median diameter of CeO2particles D50=(1.0±0.1)μm,the ball milling was stopped and the slurry was taken out.After that,the slurry was filtered through a 5μm filter bag,adjusted to the appropriate pH value with 0.5 mol·L-1 KOH solution,and added an appropriate amount of suspension dispersant sodium polyacrylate to prepare a polishing solution with a solid content of 5%.The K9 glass was polished by reed 9 B polishing machine.CeO2particles with different properties obtained by different calcination processes were refined,and the slurry with solid content of 5%was prepared to polish K9 glass on a double-sided polishing machine.The thickness reduction of K9 glass after 30 min was recorded.The cutting amount of polishing fluid was quantified by MRR to characterize the polishing efficiency of CeO2polishing fluid.The surface morphology of glass before and after polishing was observed by atomic force microscope(AFM),and the surface roughness was used to evaluate the surface quality of glass.The specific surface area of the particles was measured by H300-2000 A automatic nitrogen adsorption specific surface analyzer(BET);the phase of the calcined products was analyzed by Panaco X‘Pert Powder 003 diffractometer(XRD);the micro morphology of the particles was characterized by JEOL JEM-2100 F field emission transmission electron microscope(TEM)and JEOL7001 F field emission scanning electron microscope(SEM);the morphology of the particles was characterized by edge The surface roughness of polished glass was measured by AFM.The results showed that under different calcination conditions,the particle properties of CeO2powders were obviously different.When the calcination temperature of raw materials increased,the maximum temperature holding time prolonged or the heating rate slowed down,the CeO2grains would grow rapidly,the agglomeration of the grains was enhanced,the particle size became larger,and the CeO2grains were more complete,the grain defects were significantly reduced,and the specific surface area of the particles was reduced.The smaller the specific surface area was,the higher the MRR value was.However,when the specific surface area of CeO2was 5 m2·g-1,the roughness(Ra)value of K9 glass was the smallest,and the glass had a smooth surface.CeO2with CaF2 structure could be prepared by simple direct calcination method,using Ce(OH)3as precursor and calcining temperature above 700℃.The calcination process had an important influence on the structure and morphology of CeO2powder.When calcined at 900℃,the massive particles were more uniform and regular,forming more dense CeO2aggregate particles.Higher calcination delay,longer holding time and higher heating rate could obtain CeO2particles with smaller specific surface area.The specific surface area of CeO2particles was closely related to its polishing performance.When the specific surface area of CeO2particles was 5 m2·g-1,the roughness(Ra)value of K9 glass polished surface was the smallest,and the glass had a smooth surface.Therefore,CeO2powder with large specific surface area could be used for large cutting amount,and CeO2powder with reasonable specific surface area could be used for polishing when high quality surface was needed.
Keywords:CeO2  precursor calcination  specific surface area  cutting volume  roughness
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