水相沉淀法制备纳米片状钼铜矿 (Cu3(MoO4)2(OH)2)

doi:10.3724/SP.J.1077.2010.10750

无机材料学报 ›› 2011, Vol. 26 ›› Issue (4): 438-442.DOI: 10.3724/SP.J.1077.2010.10750

水相沉淀法制备纳米片状钼铜矿 (Cu₃(MoO₄)₂(OH)₂)

蒋文俊 ¹,²,³ , 方劲 ² , 范仲勇 ¹ , 杨绪杰 ² , 陆企亭 ³ , 侯一斌 ³

1. 复旦大学材料科学系 , 上海 200433; 2. 南京理工大学软化学与功能材料教育部重点实验室 , 南京 210094; 3. 上海康达化工新材料股份有限公司 , 上海 201201

收稿日期:2010-11-04 修回日期:2010-12-13 出版日期:2011-04-20 网络出版日期:2011-04-22
作者简介:JIANG Wen-Jun(1980 - ), male, PhD.

Synthesis of Nano-sized Tabular Lindgrenite (Cu₃(MoO₄)₂(OH)₂) by Aqueous Precipitation

JIANG Wen-Jun¹,²,³,FANG Jin²,FAN Zhong-Yong¹,YANG Xu-Jie²,LU Qi-Ting³,HOU Yi-Bin³

1 . Department of Materials Science, Fudan University, Shanghai 200433, China ; 2. Key Laboratory for Soft Chemistry and Functional Materials, Ministry of Education, Nanjing University of Science and Technology, Nanjing 210094, China ; 3. Shanghai Kangda Chemical Co., LTD, Shanghai 201201, China

Received:2010-11-04 Revised:2010-12-13 Published:2011-04-20 Online:2011-04-22
Supported by:
Foundation item : High Technical Foundation of Jiangsu Province (BG2007047); National Natural Science Foundation of China (50772048)

摘要/Abstract

摘要： 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.

关键词: 钼铜矿(Cu₃(MoO₄)₂(OH)₂), 水相沉淀法, 纳米晶, 表征, 热稳定性, 荧光特性

Abstract: 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 = 0.53863nm, b = 1.40006nm, c = 0.56003nm, 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 ₀₂₁and d_ī ₂₁measured are 0. 435nm and 0.358nm , 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. 530nm upon excitation at ca. 369nm. Finally, a possible m e ch a nism for the formation of Cu₃(MoO₄)₂(OH)₂ nanocrysta ls is proposed.

Key words: lindgrenite (Cu₃(MoO₄)₂(OH)₂), aqueous precipitation, nanocrystals, characterization, t hermal stability, fluorescent property

中图分类号:

O782

蒋文俊, 方劲, 范仲勇, 杨绪杰, 陆企亭, 侯一斌. 水相沉淀法制备纳米片状钼铜矿 (Cu₃(MoO₄)₂(OH)₂)[J]. 无机材料学报, 2011, 26(4): 438-442.

JIANG Wen-Jun,FANG Jin,FAN Zhong-Yong,YANG Xu-Jie,LU Qi-Ting,HOU Yi-Bin. Synthesis of Nano-sized Tabular Lindgrenite (Cu₃(MoO₄)₂(OH)₂) by Aqueous Precipitation[J]. Journal of Inorganic Materials, 2011, 26(4): 438-442.

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水相沉淀法制备纳米片状钼铜矿 (Cu₃(MoO₄)₂(OH)₂)

Synthesis of Nano-sized Tabular Lindgrenite (Cu₃(MoO₄)₂(OH)₂) by Aqueous Precipitation

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