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作 者:马澜 齐鹏远[2] 马雷 戴时雨 徐晓辰[2] 刘杨 MA Lan;QI Peng‑Yuan;MA Lei;DAI Shi‑Yu;XU Xiao‑Chen;LIU Yang(Shenyang Urban Planning&Design Institute Co.,Ltd.,Shenyang 110004,China;School of Materials Science and Engineering,Yingkou Institute of Technology,Yingkou,Liaoning 115014,China;School of Materials Science and Engineering,Shenyang University of Chemical Technology,Shenyang 110142,China)
机构地区:[1]沈阳市规划设计研究院有限公司,沈阳110004 [2]营口理工学院材料科学与工程学院,营口115014 [3]沈阳化工大学材料科学与工程学院,沈阳110142
出 处:《无机化学学报》2021年第6期968-976,共9页Chinese Journal of Inorganic Chemistry
基 金:辽宁省自然科学基金(No.20180550516);辽宁省教育厅科学研究(No.L2019005)资助。
摘 要:以不同沉淀剂的反向共沉淀法制备了SrZrO_(3)∶Ce纳米粒子;采用X射线衍射(XRD)、扫描电镜(SEM)、热重-差热分析(TGDTA)测试方法,对样品物相、形貌、发光强度及烧结致密化进行了分析,讨论了不同前驱体的热分析动力学。结果表明:用单相和复相沉淀剂制备的前驱体在1000℃煅烧2 h分别获得分散性良好的棱柱形和近球形SrZrO_(3)∶Ce粒子,粒径约80和60 nm。利用Doyle‑Ozawa积分法和Kissinger微分法分别求出用单相和复相沉淀剂制备的前驱体在不同反应阶段的表观活化能平均值为94.18、69.39、255.72 kJ·mol^(-1)和90.46、51.03、232.35 kJ·mol^(-1),晶体生长活化能为E_(单相)=27.97 kJ·mol^(-1)和E_(复相)=22.53 kJ·mol^(-1),后者的表观活化能和晶体生长活化能都小于前者,表明复合沉淀剂的引入降低了合成能量,提高了粒子活性,所制备样品的发光强度明显优于用单相沉淀剂制备的样品,经1760℃真空烧结保温4 h后用复相沉淀剂制备的样品的晶粒尺寸均一并达到了致密化。SrZrO_(3)∶Ce nanoparticles were prepared by reverse coprecipitation method with different precipitants.The phase,morphology,luminescence intensity and sintering densification of the samples were analyzed by X‑ray diffraction(XRD),scanning electron microscopy(SEM),thermogravimetry‑differential thermal analysis(TG‑DTA).The thermal analysis kinetics of different precursors were discussed.The results showed that the prismatic and nearly spherical SrZrO_(3)∶Ce particles with good dispersion were obtained by calcining the precursors prepared with single phase and multiphase precipitants at 1000℃for 2 h,with the particle sizes of about 80 and 60 nm,respectively.Using Doyle Ozawa integral method and Kissinger differential method,the average apparent activation energies in different reaction stages of precursors prepared with single phase and multiphase precipitants were 94.18,69.39,255.72 kJ·mol^(-1) and 90.46,51.03,232.35 kJ·mol^(-1),respectively.The activation energies of crystal growth:E_(single phase)=27.97 kJ·mol^(-1) and E_(multiphase)=22.53 kJ·mol^(-1),respectively.The apparent activation energy and grain growth activation energy of the latter were lower than those of the former,which indicates that the sample prepared with multiphase precipitant reduces the synthesis energy and improves the particle activity,and its luminous intensity was obviously better than that of the sample prepared with single phase precipitant.After vacuum sintering at 1760℃for 4 h,the sample prepared with multiphase precipitant had uniform grain size and achieved densification.
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