高温自加压制备纳米WS_2
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摘要
本文采取高温自加压方法,合成了不同形貌的纳米WS_2。利用X-射线衍射仪对合成产物进行了结构表征;利用扫描电子显微镜观察了合成产物的形貌。
研究了反应温度、分散剂二甲基亚砜(DMSO)的加入量、硫的过硫系数(ESC)和保温时间对合成产物结构和形貌的影响,结果表明:当二甲基亚砜与钨酸体积比为3:1、过硫系数为2、保温时间2h时,在不同的反应温度下制备出的纳米材料的形貌各不相同,反应温度为650℃时,制备得到的是花形纳米晶;随着温度的升高变成片状晶体,当反应温度为850℃时,制备得到球形颗粒。
The nano WS_2 with different morphology were synthesized by RAPET(Reaction under Autogenic Pressure at Elevated Temperature) method.The micro structure of WS_2 synthesized was characterized by using XRD,and the morphology of WS_2 synthesized was characterized by using SEM.
After researching the effect of the reaction temperature,the amount of dimethyl sulfoxide(DMSO),excessive sulfur coefficient(ESC) and temperature holding time on the structure and morphology of WS_2,it was conclued that when the ratio of volume of dimethyl sulfoxide(DMSO)and tungstic acid was 3:1,the excessive sulfur coefficient was 2 and temperature holding time was 2 hours,the different morphology of the WS_2 was got at different reaction temperatures.When the reaction temperature was 650℃, floriated nanocrystal was got,and when the reaction temperature was 850℃,the spheroidal particle was obtained.
研究了反应温度、分散剂二甲基亚砜(DMSO)的加入量、硫的过硫系数(ESC)和保温时间对合成产物结构和形貌的影响,结果表明:当二甲基亚砜与钨酸体积比为3:1、过硫系数为2、保温时间2h时,在不同的反应温度下制备出的纳米材料的形貌各不相同,反应温度为650℃时,制备得到的是花形纳米晶;随着温度的升高变成片状晶体,当反应温度为850℃时,制备得到球形颗粒。
The nano WS_2 with different morphology were synthesized by RAPET(Reaction under Autogenic Pressure at Elevated Temperature) method.The micro structure of WS_2 synthesized was characterized by using XRD,and the morphology of WS_2 synthesized was characterized by using SEM.
After researching the effect of the reaction temperature,the amount of dimethyl sulfoxide(DMSO),excessive sulfur coefficient(ESC) and temperature holding time on the structure and morphology of WS_2,it was conclued that when the ratio of volume of dimethyl sulfoxide(DMSO)and tungstic acid was 3:1,the excessive sulfur coefficient was 2 and temperature holding time was 2 hours,the different morphology of the WS_2 was got at different reaction temperatures.When the reaction temperature was 650℃, floriated nanocrystal was got,and when the reaction temperature was 850℃,the spheroidal particle was obtained.
引文
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[30]程继贵,熊二涛,将阳等.WS_2超细粉体的固相法合成[J].应用化学,2006,23(7):786-789.
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[32]尹桂林,黄平华,余 震等.MoS_2/WS_2共溅射复合薄膜的微结构及其摩擦磨损性能研究[J].摩擦学学报,2007,27(1):41-44.
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[34]万林生,张耀静,肖学友等.液相沉淀法制备WS_2超细粉体[J].中国钼业,2003,27(5):24-26.
[35]李长生,于云,刘艳清等.WS_2纳米颗粒的合成及摩擦学性能研究[J].无机化学学报,2008,24(2):275-279.
[36]马林,夏军保,陈卫祥等.WS_2纳米带的水热合成与表征[J].浙江大学学报(工学版)2006,40(5):832-835.
[37]张俐丽,涂江平,张升才等.球磨-溶剂热诱导法合成WS_2纳米棒及其摩擦性能[J].无机化学学报,2006,22(9):1591-1594.
[38]Raymond D L,Hsu K W,Fearon K P,et al.Multiwalled carbon nanotubes coated with tungsten disulfide[J].Chem Mater,2002,14:2209.
[39]黄祥平,段金霞.纳米WS_2的制备及其应用探讨[J].三峡大学学报(自然科学版)2003,25(3):282-284.
[40]王广珠,汪德良,崔焕芳.离子交换树脂使用及诊断技术[M].化学工业出版社72-73.
[41]Yagi M,Sone K,Yamada M,et al.Preparation and multicolor electrochromic performance of a WO_3/tris-(2,2-bipyridine)ruthenium(Ⅲ)/polymer hybrid film[J].Chem Eur J,2005,11:767-775.
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[45]庄琳,徐雪青,沈辉等.溶胶-凝胶法制备WO_3气致变色薄膜[J].光学仪器2001,23,(5-6);92-95
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[50]陈志刚,苏静.纳米三氧化钨的制备与应用[J].江苏大学学报(自然科学版,2005.26(1):57-60.
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