摘要
用甘氨酸-硝酸盐(GNP),Pechini,柠檬酸-硝酸盐(CNP)以及尿素-硝酸盐法(UNP)制备了Pr0.6Sr0.4FeO3-δ复合氧化物粉体,通过电感耦合等离子发射光谱(ICP),比表面积测试(BET),粒度分布、热重-差热分析(TG-DTA),傅立叶变换红外光谱(FT-IR)和X射线衍射(XRD)等手段对产物进行了分析和表征。结果表明:4种方法合成的粉体组成与Pr0.6Sr0.4FeO3-δ化学计量比一致;比表面积在9-27 m2.g-1之间,粒度范围35-110 nm,CNP法所得粉体的比表面积最大,UNP法最小;XRD结果证实,Pechini法制备的干凝胶粉在600℃下焙烧即可形成立方结构的钙钛矿相产物;FT-IR结果表明,GNP,CNP及UNP工艺合成的初级粉体中产物物相已基本形成;热分析结果预示,初级产物在1000℃下煅烧,均形成钙钛矿结构的单相固溶体。
Pr0.6Sr0.4FeO3-δ with perovskite-type structure composite-oxide powders were successfully synthesized using watery-chemical method such as glycine-nitrate process (GNP), Pechini process, citric acid-nitrate process (CNP) and urea-nitrate process (UNP). Metal nitrates were dissolved in de-ionized water with concentration of each solution 1 mol·L^-1 to prepare starting precursor solution. The chemical component, specific area, thermal stability and formation of the product were analyzed using ICP-AES, BET, TG-DTA and FT-IR, respectively, the crystalline phases of the Pr0.6Sr0.4FeO3-δ were studied by XRD, the microstructure of the ceramics was also investigated by AFM. The experimental results show that the stoichiometry of the samples for different methods accords with the Pr0.6Sr0.4FeO3-δ. The specific area distributes in the range of 9 ~ 27 m^2· g^- 1, and the particle size of the powders disperses in a range of 35 ~ 110 nm. The perovskitetype phases with cubic symmetry can be obtained after calcined the primary powder prepared by Pechini method at 600 ℃ for 2 h. The TG-DTA reveals that the single phase solid solutions with perovskite-type phases are formed after calcined the primary powders obtained from the four processes at 1000 ℃ for 2 h.
出处
《稀有金属》
EI
CAS
CSCD
北大核心
2007年第1期57-62,共6页
Chinese Journal of Rare Metals
基金
安徽省教育厅自然科学基金资助项目(2006kj132B)
作者简介
陈永红(1962-),男,安徽舒城人,硕士,教授;研究方向:稀土无机化合物,通讯联系人(E-mail:chenyh@hnnu.edu.cn)