单晶CuS纳米线的电沉积合成及结构表征
王裕希,吴 幸,徐 峰,孙立涛*
(东南大学-FEI纳皮米中心,MEMS教育部重点实验室,东南大学,江苏 南京 210096)
摘 要:采用多孔AAO模板辅助的有机溶剂电化学沉积技术,制备出尺寸均匀,平均直径30nm的单晶CuS纳米线。利用透射电子显微技术研究了纳米线的晶体结构和元素成分,分析了不同沉积电流密度对CuS纳米晶形核及生长过程的影响。研究结果表明,电流密度过小,容易导致S单质向S2-还原速度竞争不过Cu2+与S2-反应成核的速度,从而出现Cu34S32(即CuS0.95);电流密度过大,则会导致成核过程抑制生长过程,得到的CuS纳米晶均为多晶形态。
关键词:硫化铜纳米线;电化学沉积;单晶生长;高分辨透射电子显微技术
中图分类号:TB383;O646;O78;TG115.21+5.3 文献标识码:A
doi:10.3969/j.1000-6281.2014.01.003
Preparation and characterization of single crystal CuS nanowires using electro-deposition method
WANG Yu-xi, WU Xing, XU Feng, SUN Li-tao*
(SEU-FEI Nano-Pico Center,Key laboratory of MEMS of Ministry of education,Southeast University,Nanjing Jiangsu 210096,China)
Abstract:Using organic electro-chemical deposition technique with porous aluminum anodic oxide template, single-crystalline CuS nanowires with uniform size and average 30 nm in diameter were synthesized. The crystal phase information and chemical composition of CuS nanowires were characterized by transmission electron microscopy. Process of crystal nucleation and growth of CuS nano-crystals under different deposition current density were studied in detailed. The results show that: (1) if the current density was too small, rate of reduction of sulfur can't satisfied the reaction between Cu2 + and S2 - , and then Cu34S32 (namely CuS0.95) appeared;(2) if current density was excessive, the rate of nucleation would inhibit the rate of crystal growth process, and then poly-crystalline CuS was synthesized.
Keywords:copper monosulfide nanowire;electrochemical deposition;nucleation and growth; high resolution transmission electron microscopy
下载全文请到同方知网、万方数据或万维等数据库网站中下载
[1]Choi S H, An K, et al.Simple and generalized synthesis of semiconducting metal sulfide nanocrystals [J].Advanced Functional Materials, 2009, 19 (10): 1645-1649.
[2]Eijsbouts S, Mayo S W, et al. Unsupported transition metal sulfide catalysts: From fundamentals to industrial application [J]. Applied Catalysis A: General, 2007, 322: 58-66.
[3]Zheng N F, Bu X H, et al. Open-framework chalcogenides as visible-light photocatalysts for hydrogen generation from water [J]. Angewandte Chemie, 2005, 117 (33): 5433–5437.
[4]Lee H, Yoon S W, et al.In-situ growth of copper sulfide nanocrystals on multiwalled carbon nanotubes and their application[J]. Nano Letters, 2007, 7(3): 779-784.
[5]Dhasade S, Patil J S, Han S H, et al. Copper sulfide nanorods grown at room temperature for photovoltaic application [J].Materials Letters, 2013, 90 (1):138–141.
[6]Sagade A, SharmaetR. Copper sulphide (CuxS) as an ammonia gas sensor working at room temperature [J]. Sensors and Actuators B: Chemical, 2008, 133 (1): 135–143.
[7]岳永海, 周晓亮, 王立华,等. Cu纳米线的制备及其力学性能的研究[J]. 电子显微学报, 2011, 30 ( 3): 175-180.
[8]齐阔, 马传生, 李兴华, 等. NiCu / Cu 多层纳米线微、纳结构及成份研究[J]. 电子显微学报, 2012, 31(2): 97-103.
[9] Routkevitch D, Bigioni T, Moskovits M,et al. Electrochemical fabrication of CdS nanowire arrays in porous anodic aluminum oxide templates [J]. The Journal of Physical Chemistry, 1996, 100 (33): 14037-14047.
[10]Xu D, Xu Y, Chen D, et al.Preparation and characterization of CdS nanowire arrays by dc electrodeposit in porous anodic aluminum oxide templates [J]. Chemical Physics Letters, 2000, 325 (4): 340-344.
[11]Wu C, Shi J B, Chen C J, et al. Synthesis and optical properties of CuS nanowires fabricated by electrodeposition with anodic alumina membrane [J]. Materials Letters, 2008, 62 (6): 1074-1077.
[12]Qian X, Liu H, Chen N, et al. Architecture of CuS/PbS heterojunction semiconductor nanowire arrays for electrical switches and diodes [J]. Inorganic Chemistry, 2012, 51 (12): 6771-6775.
[13]Rickerby D, Valdrè Giovanni, Valdrè Ugo. Impact of Electron and Scanning Probe Microscopy on Materials Research [M]. Italy:Kluwer Academic Publishers, 1998:81-83.