周军,吴雷,梁坤,周晶晶,张秋利,宋永辉,田宇红.水热法制备球花状MoS2及其热红联用分析[J].稀有金属材料与工程,2020,49(4):1177~1183.[zhou jun,wu lei,liang kun,zhou jing jing,zhang qiu li,song yong hui,tian yu hong.Hydrothermal Preparation of Petal-like MoS2 and its TG-DSC-FTIR Analysis[J].Rare Metal Materials and Engineering,2020,49(4):1177~1183.]
水热法制备球花状MoS2及其热红联用分析
投稿时间:2019-08-24  修订日期:2020-03-02
中文关键词:  二硫化钼  水热合成  形貌分析  热重分析  红外分析
基金项目:国家自然科学基金项目(面上项目,重点项目,重大项目)
中文摘要:
      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。研究结果表明:Mo/S比、还原剂添加量、反应温度和反应时间均对产物收率产生影响。球花状微球为纯净的六角2H-MoS2,微球直径约为1-2 um,微球上球花厚度约为15-20 nm。球花状MoS2微球热损失大致可以分为两个阶段:MoS2转化阶段(温度区间为221.40 °С~603.15 °С)和MoO3相变阶段(温度区间为603.15 °С~1220 °С)。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。
Hydrothermal Preparation of Petal-like MoS2 and its TG-DSC-FTIR Analysis
英文关键词:Molybdenum disulfide  Hydrothermal synthesis  Morphology analysis  thermal analysis  FTIR analysis
英文摘要:
      Petal-like MoS2 microspheres were synthesized via the hydrothermal reaction of Na2MoO4, CS(NH2)2, and H2C2O4. The crystal form and micro morphology of MoS2 were analyzed by XRD and SEM, and its thermogravimetric and gas precipitation properties were studied via TG–DSC–FTIR. Results indicated that product yield was 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 was hexagonal 2H-MoS2, which petal-like microspheres diameter was about 1-2 μm with 15-20 nm average thickness of petal. The thermal loss process of MoS2 could roughly be divided into two stages: transformation stage of MoS2 and phase change stage of MoO3, wherein, first stage mainly focused in 221.40 °С~603.15 °С, and second stage occurred in the temperature range of 603.15 °С~1220 °С. MoO2 and MoO3 were generated in the first stage which thermal loss decreased by 22.30%. A phase change of MoO3 from solid to liquid and gas appeared in the second stage. FTIR data showed that there was no SO2 gas at 603.15 °С, which proved MoS2 completely transformation before 600 °С. Compared with common MoS2, the petal-like MoS2 microsphere acted out high reaction activity.
作者单位E-mail
周军 西安建筑科技大学化学与化工学院 xazhoujun@126.com 
吴雷 西安建筑科技大学冶金工程学院  
梁坤 西安建筑科技大学化学与化工学院  
周晶晶 西安建筑科技大学化学与化工学院  
张秋利 西安建筑科技大学化学与化工学院  
宋永辉 西安建筑科技大学冶金工程学院  
田宇红 西安建筑科技大学化学与化工学院  
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