Gd^3+、Ca^2+共掺氧化铈纳米粉体的制备  

Preparation of Gd^3+、Ca^2+ Co-Doped CeO2 Based Solid Electrolyte

作　　者：贺素姣 张予新 付大勇 HE Su-jiao;ZHANG Yu-xin;FU Da-Yong(Henan Vocational College of Applied Technology,Zhengzhou 450042,China)

机构地区：[1]河南应用技术职业学院,河南郑州450042

出　　处：《盐科学与化工》2020年第5期33-35,47,共4页Journal of Salt Science and Chemical Industry

摘　　要：以Ce(NO3)3·6H2O、Gd(NO3)3·5H2O和Ca(NO3)2·4H2O为原料,采用草酸盐沉淀法制备一系列Ce0.8Gd0.2-xCaxO2-δ(x=0.00~0.20)粉体。运用TG/DSC、EA、TEM、XRD等实验手段对粉体的前驱体和煅烧粉体进行了表征。结果表明:前驱体沉淀物其组成为Ce0.8Gd0.15Ca0.05(C2O4)1.475·4.8H2O,煅烧后产物组成为Ce0.8Gd0.15Ca0.05O1.875。前驱体经400℃,600℃,700℃和800℃煅烧后的粉体皆为立方萤石结构,其晶粒度分别为14.2 nm,22.5 nm,29.3 nm和38.1 nm。样品在1 200℃,1 300℃和1 400℃烧结2 h的相对密度分别达到92.5%,95.3%和96.6%;晶粒度从1 200℃的0.5μm^1μm增加到1 400℃的1μm^2μm,与相对密度的测定结果吻合;烧结体XRD测定表明,Ce0.8Gd0.2-xCaxO2-δ样品经过1 400℃高温煅烧,仍然保持立方萤石结构,没有新物相的形成。Powders of Ce0.8Gd0.2-xCaxO2-δ(x=0.00~0.20) were prepared by co-precipitation method using cerium nitrate,gadolinium nitrate and calcium nitrate as the raw material,and ammonium oxalate as precipitator.The powder precursor and powders have been characterized by TG/DSC、EA、TEM and XRD.The results indicated that:the powder precursor was identified as Ce0.8Gd0.15Ca0.05(C2O4)1.475·4.8 H2O.The sintered powders were Ce0.8Gd0.15Ca0.05O1.875.The crystal sizes of the powders calculated with Scherrer’s equation are 14.2 nm,22.5 nm,29.3 nm and 38.1 nm for Ce0.8 Gd0.15 Ca0.05O2-δcalcined at 400 ℃,600 ℃ 700 ℃ and 800 ℃ for 4 h,respectively.The relative densities of the typical Ce0.8 Gd0.1 Ca0.1O2-δsamples sintered at 1 200 ℃,1 300 ℃ and 1 400 ℃ for 2 h are measured to be 92.5%,95.3% and 96.6%,respectively.The average grain sizes in the sintered pellets increased with increasing sintering temperature and the average grain sizes were about 0.5 μm ~ 1 μm at 1 200 ℃ and 1 μm ~ 2 μm at 1 400 ℃ .No impurity phases appeared in the XRD patterns of Ce0.8Gd0.2-xCaxO2-δ sintered at 1 400 ℃ .

关 键 词：草酸盐沉淀法 掺杂氧化铈 固体电解质 纳米粉体 

分 类 号：O614[理学—无机化学]