New routes to copper sulfide nanostructures and thin films
New routes to copper sulfide nanostructures and thin films
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DOI：
10.1039/c1jm13277f
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发表时间：
2011-01-01
影响因子：
--
通讯作者：
Raftery, James
中科院分区：
文献类型：
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作者：
Abdelhady, Ahmed Lutfi;Ramasamy, Karthik;Raftery, James
合成了1，1，5，5-四异丙基-2-硫代缩二脲铜配合物[Cu（SON（（CNPr_2）-Pr_1）（2））（2）]，并测定了其单晶结构。该配合物已被用作单一来源的前体，用于通过溶液热法制备硫化铜纳米颗粒。合成的纳米颗粒具有各种形态，包括球形，六方盘，和三角形微晶;取决于反应温度，前体的浓度和生长时间。在油胺中的热处理实验产生了Cu 7S 4纳米颗粒，其为菱铁矿（单斜晶）和苯胺石（斜方晶）相的混合物。当将十八烯中的前体溶液注入热油胺中时，得到纯苯胺型Cu 7S 4纳米颗粒，而当将油胺中的前体溶液注入热十二烷醇中时，得到djurleite型Cu1.94S纳米颗粒。纯anilite Cu 7S 4相和djurleite Cu1.94S的光学性质与间接带隙材料一致。该配合物还用于气溶胶辅助化学气相沉积（AACVD）制备硫化铜薄膜。薄膜的粉末X射线衍射（p-XRD）图案显示在所有温度下的立方CuS 2和六方Cu 2S相的混合物的沉积。硫化铜膜的扫描电子显微镜（SEM）显示在280 ℃下反应的球形微晶、在320 ℃下的长方体和在360和400 ℃之间的板状微晶。从薄膜上刮下的材料的透射电子显微镜（TEM）显示出宽度为25-30 nm的硫化铜纳米片。
The copper(II) complex of 1,1,5,5-tetra-iso-propyl-2-thiobiuret [Cu(SON((CNPr2)-Pr-i)(2))(2)], has been synthesized and its single crystal X-ray structure determined. The complex has been used as a single source precursor for the preparation of copper sulfide nanoparticles by solution thermolysis. The nanoparticles synthesized had various morphologies including spherical, hexagonal disks, and trigonal crystallites; depending on the reaction temperature, concentration of the precursor and the growth time. Thermolysis experiments in oleylamine produced Cu7S4 nanoparticles as a mixture of roxbyite (monoclinic) and anilite (orthorhombic) phases. Pure anilite Cu7S4 nanoparticles were obtained when a solution of precursor in octadecene was injected into hot oleylamine whereas, djurleite Cu1.94S nanoparticles were obtained when a solution of the precursor in oleylamine was injected into hot dodecanethiol. The optical properties of the pure anilite Cu7S4 phase and the djurleite Cu1.94S are consistent with indirect band gap materials. The complex was also used for the preparation of copper sulfide thin films by aerosol assisted chemical vapour deposition (AACVD). Powder X-ray diffraction (p-XRD) patterns of the thin films showed the deposition of a mixture of cubic CuS2 and hexagonal Cu2S phases at all temperatures. Scanning Electron Microscopy (SEM) of copper sulfide films showed spherical crystallites from reaction at 280 degrees C, cuboids at 320 degrees C and plate like crystallites between 360 and 400 degrees C. Transmission Electron Microscopy (TEM) of material scratched from thin films showed nanoplates of copper sulfides with 25-30 nm in width.