水热法制备球花状MoS2及其热红联用分析  

Hydrothermal Preparation of Petal-like MoS2 and Its TG-DSC-FTIR Analysis

作　　者：周军[1,3] 吴雷 杨茸茸 张秋利 宋永辉[2,4] 田宇红 兰新哲[3,4] Zhou Jun;Wu Lei;Yang Rongrong;Zhang Qiuli;Song Yonghui;Tian Yu-hong;Lan Xinzhe(School of Chemistry and Chemical Engineering,Xi'an University of Architecture and Technology,Xi'an 710055,China;School of Metallurgical Engineering,Xi'an University of Architecture and Technology,Xi'an 710055,China;Shaanxi Province Metallurgical Engineering and Technology Research Centre,Xi'an 710055,China;Key Laboratory of Gold and Resources of Shaanxi Province,Xi'an 710055,China)

机构地区：[1]西安建筑科技大学化学与化工学院,陕西西安710055 [2]西安建筑科技大学冶金工程学院,陕西西安710055 [3]陕西省冶金工程技术研究中心,陕西西安710055 [4]陕西省黄金与资源重点实验室,陕西西安710055

出　　处：《稀有金属材料与工程》2020年第4期1177-1183,共7页Rare Metal Materials and Engineering

基　　金：National Natural Science Foundation of China(51774227);Natural Science Foundation Program of Shaanxi Province for Key Basic Research(2017ZDJC-33);Natural Science Foundation Program of Shaanxi Province for Joint Fund Project(2019JLP-17);International Scientific and Technological Cooperation Project of Shaanxi Province(2019KW-049)。

摘　　要：以Na2MoO4为钼源,CS(NH2)2为硫源,H2C2O4为还原剂,采用水热合成法制备了球花状MoS2微球,并利用XRD、SEM-EDS和TG-DSC-FTIR等分析手段对其晶型、微观形貌、热性能等进行分析。结果表明:Mo/S摩尔比、还原剂添加量、反应温度和反应时间均对产率产生影响。球花状微球为纯净的六角2H-MoS2,微球直径为1~2μm,微球上球花厚度为15~20 nm。球花状MoS2微球热损失大致可以分为2个阶段:MoS2转化阶段(温度区间为221.40~603.15℃)和MoO3相变阶段(温度区间为603.15~1220℃)。转化阶段MoS2转化为MoO2和MoO3,质量损失为22.3%;相变阶段主要是发生了固相MoO3转变为液相和气相的相变反应。FTIR结果表明,SO2气体在603.15℃之前全部析出,证明了MoS2在600℃左右完全转化。与常规MoS2相比,球花状MoS2微球表现出更高的活性。Petal-like MoS2 microspheres were synthesized via the hydrothermal reaction of Na2MoO4,CS(NH2)2,and H2C2O4.The crystal form and morphology of MoS2 were analyzed by XRD and SEM,and its thermogravimetric and gas precipitation properties were studied via TG-DSC-FTIR.Results indicate that product yield is influenced by the molar ratio of Mo/S,amount of reducing agent,reaction temperature,and reaction time.The crystal form of petal-like MoS2 microspheres is hexagonal 2H-MoS2;diameter of petal-like microspheres is 1~2μm,and the average thickness of petal is 15~20 nm.The thermal loss process of MoS2 can be roughly divided into two stages:transformation stage of MoS2 and phase change stage of MoO3,in which the first stage mainly occurs at 221.40~603.15℃,and the second stage occurs in the temperature range of 603.15~1220℃.MoO2 and MoO3 are generated in the first stage,with the thermal loss of 22.30%.A phase change of MoO3 from solid to liquid and gas occurs in the second stage.FTIR data show that there is no SO2 gas at 603.15℃,which proves that MoS2 is completely transformed before 600℃.Compared with common MoS2,the petal-like MoS2 microspheres have higher reaction activity.

关 键 词：球花结构 二硫化钼 水热合成 热重分析 红外分析 

分 类 号：TQ136.12[化学工程—无机化工]