以硝酸铜、钼酸钠及氢氧化钠为原料, 采用简单的水相沉淀法, 在60℃下合成出钼铜矿(Cu3(MoO4)2(OH)2). 通过X射线衍射、扫描电镜、透射电镜、热重与差热分析、红外光谱及荧光光谱等测试手段对材料的微观结构、形貌、热稳定性及谱学特性进行表征分析. 结果显示, 制备的产物为结晶性良好的、至少一维是纳米的片状结构材料, 属于单斜型(晶胞参数a=0.53863nm, b=1.40006nm, c=0.56003nm), 其元素摩尔含量比约为3:2:10, 与推测的分子式完全吻合.热重与差热分析数据表明Cu3(MoO4)2(OH)2纳米晶具有很好的热稳定性且起始分解温度为320℃. 通过软件测得的d(021)面与d(ī21)面的晶间面距分别为0.435nm与0.358nm, 与理论值基本相符. 经测量,Cu3(MoO4)2(OH)2纳米晶具有强的荧光性质,在激发波长369nm的作用下在530nm表现为强发射峰. 此外,还探讨了Cu3(MoO4)2(OH)2纳米晶的形成机理.
Lindgrenite (Cu3(MoO4)2(OH)2) nanocrystals were synthesized by simple aqueous precipitation at 60 ℃ , using Cu(NO3)2·6H2O, Na2MoO4·2H2O and NaOH as the starting materials. X-ray Diffraction ( XRD) patterns confirm the formation of pure Cu3(MoO4)2(OH)2 nano crystals, which belongs to the monoclin ic phase with calculated crystal parameters a = 0.53863 nm, b = 1.40006 nm, c = 0.56003 nm, β = 98.47°, α = γ = 90° . The e nergy d ispersive X-ray spectrum (ED X ) analysis gives an approximate atomic ratio of 3 : 2 : 10 for Cu : Mo: O. The scanning electron microscope(SEM) and transmission electron microscop e (TEM) studies show that the as-prepared nanoparticles are well crystallized with tabular structure and t he interplanar distances of d 021 and dī 2 1 measured are 0. 435 nm and 0.358 nm , coinciding with the theoretical value. It can also be seen that the Cu3(MoO4)2(OH)2 has a good thermal stability and starts decomposing at 320 ℃ through thermogravimetric- differential thermal analysis (TG-DTA) . Moreover, the strong fluorescent property of the Cu3(MoO4)2(OH)2 is measured, with green emission peak at ca. 530 nm upon excitation at ca. 369 nm. Finally, a possible m e ch a nism for the formation of Cu3(MoO4)2(OH)2 nanocrysta ls is proposed.
参考文献
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