NaSn_2(PO_4)_3纳米晶的低热固相合成及表征

Preparation and Characterization of Nanometer Crystalline NaSn_2(PO_4)_3 from Low Heat Solid-state Reaction

以Na2HPO4.12H2O和SnCl4.5H2O为原料,在适量表面活性剂聚乙二醇(PEG)-400的存在下,先在室温下研磨反应混合物进行固相反应,然后将反应混合物在80℃下保温2h,接着用水洗去混合物中的可溶性无机盐后在80℃下烘干,即得磷酸锡钠纳米晶前驱体。将前驱体在600℃下保温使其转变成高纯NaSn2(PO4)3纳米晶。采用TG/DTA,IR,XRD和SEM对产品进行表征。结果表明,前驱体在600℃下保温1h得到结晶良好、空间群为R-3(148)、平均粒径约为49.6 nm的球形NaSn2(PO4)3。

Precursor of nanometer crystalline NaSna （PO4）3 is prepared in the presence of surfactant PEG-400 with fully ground Na2HPO4· 12H2O and SnCl4 5H2O as raw materials by solid-state reaction at room temperature, the product mixture is heated at 80℃ for 2h, and washed with water to remove soluble inorganic salts and dried. Nanometer crystalline NaSn2 （PO4）3 with high purity is obtained by thermal crystallization of precursor at 600℃ for lh. Precursor and product are characterized by TG/DTA, IR, XRD and SEM. The results Show that the well crystalline spherical NaSn2 （PO4）3 with average particle size 49.6nm and consonant with space group R -3（148） is derived at 600℃ from heating precursor.