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共沉淀法制备Ca_(0.6)Mg_(0.4)Zr_4(PO_4)_6纳米粉体
Synthesis of Nanocrystalline Ca_(0.6)Mg_(0.4)Zr_4(PO_4)_6 by Co-precipitation Method

作  者: ; ; ; ;

机构地区: 景德镇陶瓷学院国家日用及建筑陶瓷工程技术研究中心

出  处: 《机械工程材料》 2007年第10期44-47,50,共5页

摘  要: 采用共沉淀法,以Ca(NO3)2·4H2O、Mg(NO3)2·6H2O、ZrO(NO3)2·8H2O和NH4H2PO4为原料合成Ca0.6Mg0.4Zr4(P04)6(C0.6M0.4ZP)纳米粉体,通过TGDSC、XRD、TEM和纳米粒度/Zeta电位分析手段研究了反应过程pH值、反应物浓度配比和沉淀反应方式等对合成粉体的相组成、平均颗粒尺寸及其分布等的影响。结果表明:将Ca^2+、Mg^2+、Zr4+离子混合溶液加入到不同pH值的NH4H2PO4溶液中,并控制pH=3~11,沉淀物经900℃煅烧3h后,可合成单相的C0.6M0.4ZP纳米粉体;当Zr4十浓度为0.5mol/L、沉淀剂NH4H2PO4浓度为1.0mol/L、pH=9时,合成粉体平均颗粒尺寸和粒径分布范围最小,分别为40nm和20-70nm。 Nano-sized Ca0. 6 Mg0. 4 Zr4 (PO4)6 (C0. 6 M0. 4 ZP)powders were successfully synthesized by phosphate chemical co-precipitation method using stoichiometric Ca(NOa )2 · 4H2 O, Mg(NOa )2 · 6H2 O, ZrOCL2 · 8H2 O and NH4H2PO4 as raw materials. The effect of processing conditions such as solution pH values, reactant concentrations and adding order of reactant on phase composition, mean particle size and particle size distribution of C0. 6 M0. 4ZP nano-powders were investigated by means of TG-DSC, XRD, Nano particle size/Zeta potential analysis and TEM. The results show that single phase C0.6 M0.4 ZP nano-powders can be obtained when the mixed Ca^2+, Mge+, Zr^2+ solutions are added into NH4H2PO4 precipitation agent solutions, controlling the pH values of NH4H2PO4 solutions between 3 to 11 and after the thermal processing of precipitation at 900 ℃ for 3 h. With 0. 5 mol/L Zr4+ and 1.0 mol/L NH4 Ha PO4, the mean particle size and particle size distribution of resultant C0. 6M0. 4 ZP is smaller at pH=9 than those at other pH values, and were 40nm and 20--70 nm, respectively.

关 键 词: 共沉淀法 纳米粉体 平均粒径

领  域: [化学工程] [化学工程]

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