Cu2O microsphere, microspherical composite of Cu2O/Cu nanocrystals and various Cu microcrystals: In situ hydrothermal conversion of Cu-aminodiphosphonate complexes
Cu2O microsphere, microspherical composite of Cu2O/Cu nanocrystals and various Cu microcrystals: In situ hydrothermal conversion of Cu-aminodiphosphonate complexes
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DOI：
10.1016/j.powtec.2013.04.046
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发表时间：
2013-09-01
影响因子：
5.2
通讯作者：
Nemati, Ahlam
中科院分区：
文献类型：
--
作者：
Dehghanpour, Saeed;Mahmoudi, Ali;Nemati, Ahlam
本文介绍了以{[环己基（磷甲乙基）氨基]甲基膦酸（dP）为络合剂和还原剂，采用复合前驱体水热法制备均匀Cu2O微球、可控尺寸和组成的Cu2O/Cu纳米晶体球形复合材料和多种新型铜微观结构的方法。值得注意的是，通过控制合成参数来改变初始形成的Cu2+-氨基二膦酸盐配合物前驱体的特性对最终产物的生长至关重要。在pH = 9条件下，纳米Cu2O聚集形成球形微观结构，纳米Cu2O在pH = 9条件下发生再结晶，形成较大粒径的球形Cu2O/Cu微观结构，随着Cu相含量的增加，纳米Cu2O/Cu微观结构的粒径逐渐增大。在pH = 14时，只得到不同形状的纯Cu微晶。考察了原料的浓度、摩尔比、反应时间和温度对铜微晶生长过程和形貌的影响。最后，提出了一种可能的生长机制。用x射线衍射、扫描电镜、透射电镜和傅里叶变换红外光谱对所得样品进行了表征。(C) 2013 Elsevier B.V.版权所有
We describe here a complex precursor hydrothermal route to prepare uniform Cu2O microsphere, spherical composite of Cu2O/Cu nanoaystals with controlled size and composition and a wide range of novel copper microstructures using {[Cyclohexyl(phosphonomethyl)amino]methyl}phosphonic acid (dP) as both the complexing and reducing agent. It is noteworthy that changing the characteristic of initially formed Cu2+-aminodiphosphonate complex precursor via manipulating synthetic parameters was crucial to the growth of the final product. Time order of growth process at pH = 9 has been revealed: (1) aggregation of Cu2O nanoparticles to form spherical microstructure, (2) recrystallization of Cu2O nanoparticles parallel to reductive transformation from Cu2O to Cu to produce spherical Cu2O/Cu microstructure consisting of larger nanoparticles and (3) increasing the nanoparticle size of Cu2O/Cu microstructure as the content of Cu phase increases. At pH = 14, only pure Cu microcrystals of different shapes were obtained. The effects of concentration and molar ratio of starting materials, reaction time and temperature on the growth process and morphology of copper microcrystals were investigated. Finally, a possible growth mechanism is proposed. The obtained samples have been characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier Transform infrared spectroscopy. (C) 2013 Elsevier B.V. All rights reserved.