温度对水热法合成二硫化钼结构的影响
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摘要
为了研究水热合成法中温度对制备二硫化钼(MoS2)的影响,文中以仲钼酸铵和硫脲为原料,采用水热法分别在120℃、160℃、200℃、230℃和260℃的温度下反应合成了MoS2,探究了温度对于MoS2结构和形貌的影响.通过电子天平、X射线衍射仪(XRD)、傅里叶-红外光谱(FTIR)、热失重分析仪(TGA)、扫描电子显微镜(SEM)和X射线光电子能谱(XPS)对产物进行了测试与表征.研究结果表明:反应温度对于MoS2的生长,结晶化程度和粒径,以及微观形貌有着显著的影响;反应温度为230℃时,MoS2的产量较多,热稳定性好,纯度和结晶化程度均较高,形貌规整且表面光滑圆润,微观片层结构明显,分布较为均匀.
The paper aims to study the effect of temperature on the preparation of molybdenum disulfide(MoS2)by the hydrothermal method.With ammonium molybdate and thiourea as raw materials,MoS2 was synthesized by the hydrothermal method at 120℃,160℃,200℃,230℃and 260℃,and then the influence of temperature on its structure and morphology was studied.The products were tested and characterized by using an Electronic balance,XRD,FT-IR,TGA,SEM and XPS.The results show that the reaction temperature has a significant influence on the products' growth,crystallization degree,particle size and microscopic morphology.With the reaction temperature at 230 ℃,MoS2 has a higher yield,better thermal stability,higher purity and crystallinity.The nanospheres have regular morphology,smooth surface,obvious microlayers and uniform distribution.
The paper aims to study the effect of temperature on the preparation of molybdenum disulfide(MoS2)by the hydrothermal method.With ammonium molybdate and thiourea as raw materials,MoS2 was synthesized by the hydrothermal method at 120℃,160℃,200℃,230℃and 260℃,and then the influence of temperature on its structure and morphology was studied.The products were tested and characterized by using an Electronic balance,XRD,FT-IR,TGA,SEM and XPS.The results show that the reaction temperature has a significant influence on the products' growth,crystallization degree,particle size and microscopic morphology.With the reaction temperature at 230 ℃,MoS2 has a higher yield,better thermal stability,higher purity and crystallinity.The nanospheres have regular morphology,smooth surface,obvious microlayers and uniform distribution.
引文
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[13]吴丹梅.溶剂热法制备纳米硫化物、硒化物及相关材料的摩擦学性能研究[D].青岛:青岛科技大学,2006.WU Danmei.Study on the Solvothermal Synthesis of Nano-sulfide,Nano-selenide and Application of the Related Materials[D].Qingdao:Qingdao University of Science and Technology,2006.(in Chinese)
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[15]李孟阁,刘文文,王龙飞,等.纳米二硫化钼的制备研究现状及展望[J].合成技术及应用,2016,31(1):26.LI Mengge,LIU Wenwen,WANG Longfei,et al.StudyStatus and Prospect of the Preparation of Nanoscaled Molybdenum Disulfide[J].Synthetic Technology and Application,2016,31(1):26.(in Chinese)
[16]汤国虎.纳米二硫化钼的合成与应用现状[J].无机盐工业,2009,41(6):10.TANG Guohu.Synthesis and Application of Nanosized Molybdenum Disulfide[J].Inorganic Chemicals Industry,2009,41(6):10.(in Chinese)
[17]WU D M,ZHOU X D,XUN F,et al.Synthesis and Characterization of Molybdenum Disulfide Microsized Solid Spheres[J].Journal of Materials Science,2006,41(17):5682.
[18]LI X L,LI Y D.MoS2 Nanostructures:Synthesis and Electrochemical Mg2+Intercalation[J].Journal of Physical Chemistry B,2004,108(37):13893.
[2]武存喜,杨海滨,李享,等.无机LEI富勒烯二硫化钼的减摩抗磨特性[J].润滑与密封,2007,32(7):118.WU Cunxi,YANG Haibing,LI Xiang,et al.Anti-friction and Anti-wear Properties of Inorganic Fullerencelike Molybdenum Disulfide[J].Lubrication Engineering,2007,32(7):118.(in Chinese).
[3]DUNGEY K E,CURTIS M D,PENNER-HAHN JE,et al.Behevior of MoS2Intercalation Compounds in HDS Catalysis[J].Journal of Catalysis,1998,175(1):129.
[4]WANG S Q,LI G H,DU G D,et al.Hydrothermal Synthesis of Molybdenum Disulfide for Lithium Ion Battery Applications[J].Chinese Journal of Chemical Engineering,2010,18(6):910.(in Chinese)
[5]张晓.二硫化钼电极材料的制备及电化学性能研究[D].哈尔滨:哈尔滨工业大学,2013.ZHANG Xiao.Research on Preparation of Molybdenum Disulfide Anode and Its Electrochemical Performance[D].Harbin:Harbin Institute of Technology,2013.(in Chinese)
[6]张坤杰,陈桂英,孙红.层状二硫化钼修饰电极的制备及电化学性能研究[J].科技展望,2016,26(3):78.ZHANG Kunjie,CHEN Guiying,SUN Hong.Preparation and Electrochemical Properties of Layered Molybdenum Disulfide Modified Electrode[J].Prospect of Science and Technology 2016,26(3):78.(in Chinese)
[7]FELDMAN Y,LYAKHOVITSKAYA V,TENN R.et al.Kinetics of Nested Inorganic Fullerene-likenanoparticle Formation[J].Journal of the American Chemical Society,1998,120(17):4176.
[8]董艳芳,何大伟,王永生,等.一种简单的化学气相沉积法制备大尺寸单层二硫化钼[J].物理学报,2016,65(12):128101-1.DONG Yanfang,HE Dawei,WANG Yongsheng,et al.Synthesis of Large Size Monolayer MoS2with a Simple Chemical Vapor Deposition[J].Acta Physics Sinica,2016,65(12):128101-1.(in Chinese)
[9]周伟鹏,杨飒,龚家志,等.基于化学气相沉积法的纳米二硫化钼研究进展[J].广州化工,2018,46(1):15.ZHOU Weipeng,YANG Sa,GONG Jiazhi,et al.Research Progress of Nano Molybdenum Disulfide Based on Chemical Vapor Deposition[J].Guangzhou Chemical Industry,2018,46(1):15.(in Chinese)
[10]ZELENSKI C M,DORHOUT P K.Template Synthesis of Near-Monodisperse1 Microscale Nanofibers and Nanotubules of MoS2[J].Journal of the American Chemical Society,1998,120(4):734.
[11]BISSESSUR R,WHITE W.Novel Alkyl Substituted Polyanilines/Molybdenum Disulfide Nanosomposites[J].Materials Chemistry and Physics,2006,99(2/3):214.
[12]LI X L,GE J P,LI Y D.Atmospheric Pressure Chemical Vapor Deposition:An Alternative Route to Large-Scale MoS2,and WS2,Inorganic Fullerene-like Nanostructures and Nanoflowers[J].Chemistry-AEuropean Journal,2004,10(23):6163.
[13]吴丹梅.溶剂热法制备纳米硫化物、硒化物及相关材料的摩擦学性能研究[D].青岛:青岛科技大学,2006.WU Danmei.Study on the Solvothermal Synthesis of Nano-sulfide,Nano-selenide and Application of the Related Materials[D].Qingdao:Qingdao University of Science and Technology,2006.(in Chinese)
[14]孙昂.纳米粒子的制备与摩擦学性能的研究[D].大连:大连海事大学,2002.SUN Ang.Research on Preparation and Tribological Performance of Nanoparticles[D].Dalian:Dalian Maritime University,2002.(in Chinese)
[15]李孟阁,刘文文,王龙飞,等.纳米二硫化钼的制备研究现状及展望[J].合成技术及应用,2016,31(1):26.LI Mengge,LIU Wenwen,WANG Longfei,et al.StudyStatus and Prospect of the Preparation of Nanoscaled Molybdenum Disulfide[J].Synthetic Technology and Application,2016,31(1):26.(in Chinese)
[16]汤国虎.纳米二硫化钼的合成与应用现状[J].无机盐工业,2009,41(6):10.TANG Guohu.Synthesis and Application of Nanosized Molybdenum Disulfide[J].Inorganic Chemicals Industry,2009,41(6):10.(in Chinese)
[17]WU D M,ZHOU X D,XUN F,et al.Synthesis and Characterization of Molybdenum Disulfide Microsized Solid Spheres[J].Journal of Materials Science,2006,41(17):5682.
[18]LI X L,LI Y D.MoS2 Nanostructures:Synthesis and Electrochemical Mg2+Intercalation[J].Journal of Physical Chemistry B,2004,108(37):13893.