CTAB辅助制备环状MoS_2晶体及微结构调控
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摘要
以钼酸铵为钼源硫脲为硫源,十六烷基三甲基溴化铵(CTAB)为模板剂,采用表面活性剂促助法成功制备了环状结构MoS_2,并利用X射线衍射仪(XRD)、扫描电镜(SEM)系统比较研究了CTAB添加量、p H值、钼硫比、反应时间对合成环状MoS_2微结构及晶体生长的影响,分析了环状结构生长形成的机理。研究结果表明:MoS_2形貌主要受CTAB添加量的影响,随着用量的增多MoS_2经历了球花状-不规则环状-规则环状-不规则堆积状的递变过程,最佳CTAB添加量为0.5 g。p H值对MoS_2的生长发育以及结晶性和微观形貌有显著影响,当p H=3时,所得产物晶体颗粒的圆整度、均一性较好。钼硫比对产物的结晶性和分散性有一定影响,并且影响到环状结构的生长发育,但是过高的钼硫比会造成严重的团聚现象,当钼硫比为1∶4时产物的圆整性和分散性较好。反应时间对产物的结晶度有较大影响,随着反应时间的延长结晶度增加,最佳的反应时间为36 h。
Ring-MoS_2 was successfully prepared firstly by surfactant-promoting method,in which the ammonium molybdate as Mo-source and thiourea as the S-source and the CTAB as cationic surfactant.The effects of CTAB dosage,p H value,reaction time and the ratio of Mo and S and the growth of MoS_2 were investigated systematically by the means of X-ray diffraction( XRD),scanning election microscopy( SEM). Furthermore,the ring growth mechanism was discussed. The results reveal that the morphology of MoS_2 crystal is greatly affected by the dosage of CTAB,with the increase in the concentration of CTAB,the morphology of MoS_2 changes from ball flower,irregular ring,regular ring,to irregular packing. The optimal CTAB amount was 0. 5 g. The p H of reaction system plays a crucial role on the formation of MoS_2 ring structure,degree of crystallization,when the reaction system p H = 3,the ring-MoS_2 were obtained and showed the better roundness and uniformity. The molybdenum-sulfur ratio has a great influence on the crystallization and dispersion of the ring-MoS_2,and affects the growth and development of the ring structure, however, high ratio of molybdenum-sulfur will cause serious agglomeration. When the molybdenum-sulfur ratio was 1 ∶ 4,the ring-MoS_2 showed the better roundnessand dispersibility. The reaction time influence on the crystallization of the ring-MoS_2,the crystallization increases with the reaction time,and the optimal reaction time was 36 h.
Ring-MoS_2 was successfully prepared firstly by surfactant-promoting method,in which the ammonium molybdate as Mo-source and thiourea as the S-source and the CTAB as cationic surfactant.The effects of CTAB dosage,p H value,reaction time and the ratio of Mo and S and the growth of MoS_2 were investigated systematically by the means of X-ray diffraction( XRD),scanning election microscopy( SEM). Furthermore,the ring growth mechanism was discussed. The results reveal that the morphology of MoS_2 crystal is greatly affected by the dosage of CTAB,with the increase in the concentration of CTAB,the morphology of MoS_2 changes from ball flower,irregular ring,regular ring,to irregular packing. The optimal CTAB amount was 0. 5 g. The p H of reaction system plays a crucial role on the formation of MoS_2 ring structure,degree of crystallization,when the reaction system p H = 3,the ring-MoS_2 were obtained and showed the better roundness and uniformity. The molybdenum-sulfur ratio has a great influence on the crystallization and dispersion of the ring-MoS_2,and affects the growth and development of the ring structure, however, high ratio of molybdenum-sulfur will cause serious agglomeration. When the molybdenum-sulfur ratio was 1 ∶ 4,the ring-MoS_2 showed the better roundnessand dispersibility. The reaction time influence on the crystallization of the ring-MoS_2,the crystallization increases with the reaction time,and the optimal reaction time was 36 h.
引文
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[2]胡坤宏,徐勇,徐玉福,等.不同形态的二硫化钼润滑剂在离子液体中的摩擦学性能[J].摩擦学学报,2015,35(2):167-175.
[3]张蒙蒙,谢凤,李斌,等.金属硫化物固体润滑剂简介[J].合成润滑材料,2015,42(3):27-30.
[4]李斌,冶银平,万宏启,等.水性二硫化钼基粘结固体润滑涂层制备及其摩擦学性能[J].中国表面工程,2017,30(4):142-149.
[5]王国栋,蒋丽娟,李来,等.二硫化钼润滑剂应用研究进展[J].中国钼业,2013,37(5):10-14.
[6]张淑惠,王梦岑,张伊晗.二硫化钼的制备及其复合物在光催化应用的研究进展[J].现代盐化工,2018,45(2):49-50.
[7]王楚璇,党晶晶,叶林静.二硫化钼光催化剂的改性及其在水处理的应用研究进展[J].应用化工,2017,46(9):1827-1834.
[8]程刚,徐强,桑林,等.超声处理对可充镁电池二硫化钼电极的作用[J].电源技术,2013,37(6):990-996.
[9]韩宗盈,王乃飞,张倩倩,等.二硫化钼助磨的镁基储氢材料相结构及储氢性能[J].广东化工,2013,40(15):12-25.
[10]翟英娇,李金华,楚学影,等.纳米结构Mo S2的制备及其应用[J].无机材料学报,2015,30(9):897-905.
[11]高宾,赵鹏.富勒烯结构二硫化钼纳米粒子的制备和应用[J].中国钼业,2007,31(1):49-53.
[12]高宾,赵鹏,许启明,等.气相法合成Mo S2纳米管的研究[J].中国钨业,2006,21(3):21-24.
[13]Lin H T,Chen X Y,et al.Hydrothermal Synthesis and Characterization of Mo S2Nanorods[J].Materials Letters,2010,64:1748-1750.
[14]白鸽玲,吴壮志.二硫化钼纳米球的制备及其摩擦性能研究[J].润滑与密封,2013,38(4):93-96.
[15]Luo H,Xu C,Zou Db,et al.Hydrothermal Synthesis of Hollow Mo S2Microspheres in Ionic Liquids/Water Binary E-mulsions[J].Materials Letters,2008,62(20):3558-3560.
[16]Huang W Z,Xu Z D,Liu R,et al.Tungstenic Acid Induced Assembly of Hierarchical Flower-like Mo S2Spheres[J].Materials Research Bulletin,2008,43:2799-2805.
[17]崔雅茹,饶衍冰,何江山,等.CTAB对水热合成纳米Mo S2颗粒的影响研究[J].中国钼业,2014,38(6):30-32.
[18]崔雅茹,何江山,李凯茂.不同酸度对水热法合成纳米二硫化钼的影响研究[J].热加工工艺,2013,42(6):64-66.
[19]Zhang X,Lai Z C,Tan C L,et al.Solution-Processed Two-Dimensional Mo S2Nanosheets:Preparation,Hybridization,and Applications[J].AngewandteChemie,2016,55(31):8816-8838.
[20]Guo D S,Guo H Z.Study on the Preparation of Molybdenum Silicides by the Silicothermic Reduction of Mo S2[J].Journal of Alloys and Compounds,2017,728:295-306.
[21]Wang T Z,Liu C C,Xu J K,et al.Thermoelectric Performance of Restacked Mo S2Nanosheets Thin-film[J].Nanotechnology,2016,27:285703.
[22]Feng J D,Graf Michael,Liu Ke,et al.Single-layer Mo S2Nanopores as Nanopower Generators[J].Nature,2016,536:197-200.