CN110339845B - 一种二硫化钼花状纳米球的制备方法及析氢应用 - Google Patents
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 27
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Abstract
本发明公开了一种二硫化钼花状纳米球的制备方法及析氢应用，该方法包括以下步骤：1）将一定量的硫脲（CS(NH2)2）、二水合钼酸钠(Na2MoO4·2H2O)、柠檬酸（C6H8O7）溶于去离子水和无水乙醇的混合溶剂中；2）搅拌至完全溶解后，倒入密闭的聚四氟乙烯反应釜中，反应一段时间后自然冷却得到黑色溶液；3）将溶液置入离心管离心操作；4）将离心产物置于真空干燥箱作干燥处理，得到二硫化钼；5）将样品进行析氢测试。本发明采用一步溶剂热法制备二硫化钼，原料价廉易得；过程工艺简单，条件温和；产物均匀，具有花状纳米球特殊形貌；且电化学性能优异：在N2饱和的1M KOH条件下，电流密度为10 mA/cm2时，该方法制备的二硫化钼的析氢过电势为3 mV，比玻碳电极（877 mV）降低了874 mV，且能与商用50%Pt/C（1.5 mV）媲美。
Description
技术领域
本发明属于一种二硫化钼纳米材料制备技术及应用领域，具体涉及一种二硫化钼花状纳米球的制备方法以及析氢催化应用。
背景技术
化石燃料的巨大消耗和二氧化碳的大量排放对环境的影响促使人们大力开发一种具有足够规模的新可再生能源，以取代化石燃料，改善环境并满足日益增长的全球能源需求。而氢能以其高能量密度，燃烧产物无污染，质量小等优异的性能，成为最具潜力的新型能源之一。其中，电解水是获得氢燃料的重要途径之一，也是清洁、可扩展的能源替代品的重要途径。电解水可以直接产生氢气，涉及到氢的析出反应（HER），需要催化剂来提高转化效率。贵金属及其氧化物电催化剂如IrO2、RuO2和Pt/C被认为是标准催化剂，在HER中具有优异的性能。然而，它们储量少和高成本极大地阻碍了它们的广泛应用。
二硫化钼（MoS2）因其在理论上接近最佳的氢吸附自由能、较高的耐化学腐蚀性、地球丰度和较低的成本而被广泛地研究为一种有前途的酸性HER的铂替代品，以降低Pt的用量。
发明内容
为了解决现有的技术问题，本发明的目的在于提供一种通过工艺简单，低成本合成二硫化钼的方法，本发明具有反应条件温和、成本低廉、操作简单等优点。产物具有特殊形貌且均匀、比表面积较大、催化活性位点较多、电化学析氢性能优异等特点，在一定程度上可减少Pt的用量。
为了实现上述目标，本发明采用如下的技术方案：
1) 将硫脲（CS(NH2)2）、二水合钼酸钠(Na2MoO4·2H2O)，溶于含有柠檬酸（C6H8O7）的混合溶液中，搅拌均匀后得到透明无色溶液；
2) 将上述混合溶液倒入50 mL密闭聚四氟乙烯高压反应釜中，加热反应一段时间；
3) 将混合溶液用去离子水、无水乙醇离心洗涤；
4) 将产物置于真空干燥箱中干燥处理，得到二硫化钼花状纳米球；
5) 将样品进行析氢测试。
进一步，所述步骤1）中，硫源为硫脲，钼源为二水合钼酸钠，柠檬酸作为表面活性剂，混合溶液为去离子水和无水乙醇其比例为2:1（mL/mL）。
进一步，所述步骤2）中，加热温度为220℃，加热时间为21小时。
进一步，所述步骤3）中，离心速度为12000 rpm，离心时间为3分钟。
进一步，所述步骤4）中，真空干燥温度为60℃，加热时间为24小时在制备催化剂中硫脲、二水合钼酸钠两种材料的比例为4:1 (mol/mol)。
进一步，所述步骤5）中，测试条件为在N2饱和1M KOH下，采用三电极体系对样品进行HER极化曲线研究，扫描速度为5 mV•s-1。
本发明的有益效果在于：
1.合成的二硫化钼具有特殊形貌：
过渡金属硫化物作为一种非贵金属材料已被广泛研究作为催化剂用于电解水中的析氢反应。特别是二维二硫化钼（MoS2）具有暴露的边缘，在近年来被证明是HER非常有前途的电化学催化剂；然而，MoS2的固有问题存在于电化学反应中，即两个相邻的范德华结合的S-Mo-S板之间的电导率极低。我们通过调控MoS2 的形貌，进一步改善这一问题：在传统水热法制备MoS2的溶剂中通常把去离子水作为单一的溶剂，我们则加入了一定量的无水乙醇形成混合溶液，调控反应温度、反应釜填充度、体系压强大小进而制备得到了花瓣状球体二硫化钼。进一步的，在球型拥有着大比表面积的基础上穿插着片状，这在增加比表面积的同时还充分暴露了活性位点，从而大幅度的改善了其析氢性能。
2.合成的二硫化钼在碱性条件下有理想的析氢性能：
对于酸性介质，氢中间体（H*）来自于氢离子；在碱性溶液中，H*是由水的离解形成的，这可能会引入一个额外的能量屏障，很有可能成为速率决定步骤。这导致在碱性介质中，其反应速率通常比酸性介质低2到3个数量级。然而该发明方法所制得的MoS2在N2饱和的1M KOH条件下，电流密度为10 mA/cm2时，其析氢过电势为3 mV，比玻碳电极（877 mV）降低了874 mV，且能与商用50% Pt/C（1.5 mV）媲美。
综上，我们制备的MoS2催化材料具有特殊的形貌且在碱性条件下具有理想的析氢性能。
附图说明
为了使本发明的目的、技术方案和优点更加清楚，下面将结合附图对本发明作进一步的详细描述，其中：
图1为实施例1（MoS2）的X射线粉末衍射图（XRD）；
图2为实施例1的热场发射扫描电子显微镜图（FESEM）；
图3为实施例1的X射线能谱分析图（EDS）；
图4为实施例1的析氢（HER）的线性扫描曲线图。
Claims (1)
1.一种二硫化钼花状纳米球的制备方法，包括以下步骤：
1) 将硫脲（CS(NH2)2）、二水合钼酸钠(Na2MoO4·2H2O)和柠檬酸（C6H8O7）,在磁力搅拌器的搅拌下加入到去离子水和无水乙醇的混合溶液中得到分散均匀的无色透明溶液；
2) 将上述混合溶液置于聚四氟乙烯高压反应釜进行反应；
3) 将反应后混合溶液置于离心管离心操作；
4) 将产物置于真空干燥箱中干燥处理，得到二硫化钼催化材料；
5) 将样品进行析氢测试；
所述步骤2）中，将混合溶液转移至50 mL密闭聚四氟乙烯高压反应釜中，加热温度为220 ℃，加热时间为21小时；
所述步骤3）中，用去离子水和无水乙醇分别离心洗涤3次，离心速度为12000 rpm，离心时间为3分钟；
所述步骤4）中，真空干燥温度为60℃，加热时间为24小时，且制备的二硫化钼为花瓣状的纳米球特殊形貌，在制备催化剂中硫脲、二水合钼酸钠两种材料的比例为4:1(mol/mol)；
所述步骤5）中，制备的二硫化钼电化学析氢性能优异：在N2饱和的1M KOH条件下，电流密度为10 mA/cm2时，该方法制备的二硫化钼的析氢过电势为3 mV，比玻碳电极（877 mV）降低了874 mV，且能与商用50% Pt/C（1.5 mV）媲美。
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| CN114380334B (zh) * | 2022-01-26 | 2023-09-19 | 江西师范大学 | 螺旋金字塔结构的二硫化钼的制备方法和应用 |
| CN114887631B (zh) * | 2022-05-05 | 2023-08-18 | 中国石油大学(华东) | 一种溶剂热法制备混合形貌1T-2H MoS2的制备方法及应用 |
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