CN108862260A - 一种二硫化钼团簇层复合石墨烯材料的无毒制备方法 - Google Patents

一种二硫化钼团簇层复合石墨烯材料的无毒制备方法 Download PDF

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CN108862260A
CN108862260A CN201810798003.2A CN201810798003A CN108862260A CN 108862260 A CN108862260 A CN 108862260A CN 201810798003 A CN201810798003 A CN 201810798003A CN 108862260 A CN108862260 A CN 108862260A
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molybdenum disulfide
preparation
graphite alkene
layer composite
cluster layer
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张学谦
王依山
温广武
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Shandong University of Technology
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Abstract

本发明提供一种二硫化钼团簇层复合石墨烯材料的无毒制备方法，属于纳米材料制备领域，其特征在于采用以下步骤：（1）0.5~10 mg/mL氧化石墨搅拌1~4 h，然后超声0.5~2 h，得到氧化石墨烯溶液；（2）在搅拌条件下，向氧化石墨烯溶液中加入0.01~0.2 mol/L钼酸铵和0.02~1 mol/L硫脲，混合液搅拌0.5~4 h；（3）采用水热法，将混合液放入水热反应釜中，180~200℃水热反应20~30 h，即得二硫化钼团簇层复合石墨烯材料。二硫化钼附着在片层石墨烯上，二硫化钼为团簇层状，直径为400~600 nm，壁厚20 nm左右。本发明制备过程无毒，工艺简单，操作安全，温度低，二硫化钼团簇层分离度好，二硫化钼在石墨烯片层上分布均匀。

Description

一种二硫化钼团簇层复合石墨烯材料的无毒制备方法
技术领域
本发明提供一种二硫化钼团簇层复合石墨烯材料的无毒制备方法，属于纳米材料制备领域。
背景技术
二维纳米材料具有独特的电学、光学等物理化学特性，因此受到人们的广泛关注。在所有二维材料中，石墨烯是由sp2杂化的碳原子通过六边形连接得到的具有共轭结构的二维纳米材料，是碳纳米管、富勒烯和石墨的基本组成单元。石墨烯的独特二维结构赋予了其诸多的优异性能，包括2630 m2/g的大笔表面积，200000 cm2/vs的高载流子迁移率，1.0Tpa的高杨氏模量，5000 W/mK的高热导率，97.7%的高光透过率和其它优异的电学特性。使其在电子器件、光电器件、电化学储能、储氢、传感及热电灯诸多领域都有应用。作为一种与石墨烯类似的二维层状材料，二硫化钼每个片层之间由S-Mo-S三原子层组成，在催化、储能、润滑、光学、催化等领域具有广阔的应用前景。因此，将石墨烯和二硫化钼两种二维材料进行复合可以更大程度的发挥两种材料的优势，拓展应用领域，提高材料性能。目前关于二硫化钼和石墨烯进行复合的制备方法有以下技术报道：1、专利CN104658764A“石墨烯气凝胶三元复合超级电容器电极材料制备及应用”以钼酸钠和L-半胱氨酸为原料，采用水热法制备出花状二硫化钼粉体，然后在冰浴情况下酸性环境中诱发苯胺聚合得到二硫化钼-聚苯胺复合物，之后分散在经过预处理的氧化石墨烯-阳离子悬浮液中，再经过水热过程得到二硫化钼-聚苯胺-石墨烯水凝胶。缺点是方法复杂，周期长，不利于工业化生产；反应需在酸性环境下进行，操作危险，对环境造成污染。2、专利CN106340394A“一种二硫化钼掺杂线性聚合物修饰石墨烯复合材料及其制备方法”通过回流的方法得到聚合物修饰的氧化石墨烯，然后通过离子交换法将钼酸根阴离子交换到聚合物修饰的氧化石墨烯上，之后通过水热反应用硫代乙酰胺对钼酸根进行硫化，最后碳化处理得到二硫化钼掺杂线性聚合物修饰石墨烯复合材料。缺点是方法复杂，周期长，不利于大规模推广。3、论文“Three-dimensional MoS2/reduced graphene oxide aerogel as a macroscopic visible-light photocatalyst”采用水热法，以钼酸铵、硫脲、氧化石墨和氨水为原料，得到二硫化钼与石墨烯复合材料。缺点是在制备过程中需要加入氨水，氨水易挥发产生出有毒的氨气。
因此，研究一种操作简单并且无毒，具有工业化推广应用的二硫化钼与石墨烯复合材料具有重要的价值。
发明内容
本发明的技术目的是针对上述二硫化钼复合石墨烯材料制备技术的现状，提供一种效率高、操作简单安全、无毒的二硫化钼团簇层复合石墨烯材料的无毒制备方法，其技术方案为：
一种二硫化钼团簇层复合石墨烯材料的无毒制备方法，其特征在于采用以下步骤：（1）0.5~10 mg/mL氧化石墨搅拌1~4 h，然后超声0.5~2 h，得到氧化石墨烯溶液；（2）在搅拌条件下，向氧化石墨烯溶液中加入0.01~0.2 mol/L钼酸铵和0.02~1 mol/L硫脲，混合液搅拌0.5~4 h；（3）采用水热法，将混合液倒入水热反应釜中，180~200 ℃水热反应20~30 h，即得花状二硫化钼复合石墨烯材料。二硫化钼附着在片层石墨烯上，二硫化钼为团簇层状，直径为400~600 nm，壁厚20 nm左右。
所述的制备方法，步骤（1）中所用的氧化石墨为采用Hummers法制备的氧化石墨。
所述的制备方法，步骤（1）中钼酸铵与硫脲的摩尔比为1：2~5。
所述的制备方法，步骤（3）中混合液倒入量为水热反应釜容量的70~90%。
本发明具有如下优点：
1、本发明制备二硫化钼团簇层复合石墨烯材料采用的是无毒制备法，操作简单，安全可靠，效率高；
2、本发明制备的制备的二硫化钼均匀分布在片状石墨烯，二硫化钼为团簇层状，结构完整，层状厚度均匀，具有广泛的应用价值。
附图说明
图1是本发明实施后得到的二硫化钼团簇层复合石墨烯材料的XRD图谱。
图2是本发明实施后得到的二硫化钼团簇层复合石墨烯材料的SEM照片。

Claims (5)

1.一种二硫化钼团簇层复合石墨烯材料的无毒制备方法，其特征在于采用以下步骤：（1）0.5~10 mg/mL氧化石墨搅拌1~4 h，然后超声0.5~2 h，得到氧化石墨烯溶液；（2）在搅拌条件下，向氧化石墨烯溶液中加入0.01~0.2 mol/L钼酸铵和0.02~1 mol/L硫脲，混合液搅拌0.5~4 h；（3）采用水热法，将混合液倒入水热反应釜中，180~200 ℃水热反应20~30 h，即得二硫化钼团簇层复合石墨烯材料。
2.二硫化钼附着在片层石墨烯上，二硫化钼为团簇层状，直径为400~600 nm，壁厚20nm左右。
3.如权利要求1所述的制备方法，其特征在于：步骤（1）中所用的氧化石墨为采用Hummers法制备的氧化石墨。
4.如权利要求1所述的制备方法，其特征在于：步骤（1）中钼酸铵与硫脲的摩尔比为1：2~5。
5.如权利要求1所述的制备方法，其特征在于：步骤（3）中混合液倒入量为水热反应釜容量的70~90%。
CN201810798003.2A 2018-07-19 2018-07-19 一种二硫化钼团簇层复合石墨烯材料的无毒制备方法 Pending CN108862260A (zh)

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