CN106830083B - 金属相二硫化钼的制备方法 - Google Patents

金属相二硫化钼的制备方法 Download PDF

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CN106830083B
CN106830083B CN201710050764.5A CN201710050764A CN106830083B CN 106830083 B CN106830083 B CN 106830083B CN 201710050764 A CN201710050764 A CN 201710050764A CN 106830083 B CN106830083 B CN 106830083B
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molybdenum disulfide
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CN106830083A (zh
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崔小强
魏淑婷
祁琨
徐延超
张海燕
张雷
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Jilin University
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Abstract

本发明公开了一种金属相二硫化钼的制备方法，属于纳米材料领域。主要解决的问题是，采用了一种离子超声辅助的方法制备了金属相的二硫化钼。其步骤是通过水热法合成半导体相的二硫化钼，然后在铜盐溶液中进行超声处理，使半导体相的二硫化钼原子发生重排，原子面滑移，从而产生了金属相的二硫化钼。本发明的优点：该制备方法具有简单，安全，经济，高效，可大批量合成等优点。

Description

金属相二硫化钼的制备方法
技术领域
本发明涉及一种制备金属相二硫化钼方法，所制备的材料可用于电化学析氢领域，锂离子电池等领域。
背景技术
二维层状的二硫化钼是一种典型的过渡金属硫化物，因其具有特殊的类石墨烯结构以及独特的物理化学性质引起了研究者的广泛关注。目前研究的二硫化钼主要有半导体相、金属相和半金属相，半金属相的二硫化钼仅存在于块体二硫化钼中，半导体相二硫化钼是热力学稳定相，然而金属相是亚稳相，本质上不能稳定存在，但是，金属相的二硫化钼具有很多的活性位点以及良好的导电性，因此，在电催化制氢和超级电容器等领域，金属相的二硫化钼是一种非常有前景的材料。在过去的几十年中，利用Li离子插层的方法可以得到金属相和半导体相共存的二硫化钼，但是这种方法很危险并且耗时。因此，发明一种简单安全的方法得到金属相的二硫化钼对于催化领域是极其重要的。
发明内容
本发明的目的在于针对现有技术的不足，提供一种金属相二硫化钼的制备方法。
本发明的目的是通过以下技术方案实现的：一种金属相二硫化钼的制备方法，步骤如下：
(1)将钼酸铵和硫脲按照摩尔比1：14进行混合，然后置于去离子水中，搅拌均匀，形成均相溶液。其中，钼酸铵的浓度为1mmol/L；
(2)将溶液转移至不锈钢反应釜中，220℃反应18h，之后自然冷却到室温。
(3)将反应液离心分离，将沉淀清洗后，真空干燥，得到MoS2粉末。
(4)将真空干燥后的MoS2粉末分散到饱和的铜盐溶液中，MoS2的浓度为1.14mmol/L；超声处理24h；
(5)将上述溶液离心分离，将沉淀清洗后，真空干燥，得到金属相二硫化钼粉末。
本发明利用离子超声办法合成了金属相的二硫化钼。该方法具有简单，安全，经济，高效，可大批量合成等优点。
附图说明
图1为实施例1制备的金属相二硫化钼的扫面电子显微镜图(SEM)。
图2为实施例1制备的金属相二硫化钼的高分辨透射电子显微镜图(HRTEM)。
图3为实施例1制备的金属相二硫化钼的X射线光电子衍射(XPS)。
图4为实施例1制备的金属相二硫化钼的拉曼图。
图5为实施例1制备的样品在46天之后测试的拉曼图
图6为实施例2制备的金属相二硫化钼的拉曼图。
图7为实施例3制备的样品的拉曼图。
具体实施方式
实施例1
一种金属相二硫化钼的制备方法，步骤如下：
(1)将钼酸铵和硫脲按照摩尔比1：14进行混合，然后去离子水中，搅拌均匀，形成均相溶液。其中，钼酸铵的浓度为1mmol/L；
(2)将溶液转移至不锈钢反应釜中，220℃反应18h，之后自然冷却到室温。
(3)将反应液离心分离，将沉淀清洗后，真空干燥，得到MoS2粉末。
(4)将真空干燥后的MoS2粉末分散到饱和的铜盐溶液中，MoS2的浓度为1.14mmol/L；超声处理24h；
(5)将上述溶液离心分离，将沉淀清洗后，真空干燥，得到金属相二硫化钼粉末。
图1为制备的金属相二硫化钼的扫面电子显微镜图(SEM)，从图中可以看出合成的产物为二维片状结构，横向尺寸为100-250nm。图2为制备的金属相二硫化钼的高分辨透射电子显微镜图(HRTEM)，从图中可以看出所合成的二硫化钼纳米片由少层组成，其层间距为0.65nm，并且呈现了金属相二硫化钼的晶格。图3为本发明制备的金属相二硫化钼的X射线光电子衍射(XPS)，a)和b)分别为S 2p和Mo 3d谱，从图a)中S 2p3/2和S 2p1/2的峰对应的结合能分别是161.55eV和162.75eV；Mo 3d5/2和Mo 3d3/2的峰对应的结合能分别为228.75eV和232eV，这是归于金属相二硫化钼。
图4为合成的金属相二硫化钼的拉曼图，从图中可以看出这是典型的金属相的二硫化钼的振动模式所产生的拉曼图。144cm-1归于金属相中二硫化钼的Mo-Mo之间的弹性振动模式，194,279and 335cm-1是声子振动模式，375cm-1归于二硫化钼的面内振动模式。
图5为这个样品在46天之后测试的拉曼图，与图4相比，基本没有变化。
实施例2
本实施例同实施例1，步骤4中的MoS2浓度为0.11mmol/L，产物的Raman如图6所示。从图中可以看出此浓度下制备的样品已经发生相变，形成金属相的二硫化钼。
实施例3
本实施例同实施例1，步骤4中的MoS2浓度为2.84mmol/L，产物的Raman如图7所示。从图中可以看出此浓度下制备的样品仍为半导体相。
通过以上实施例可以看出，当MoS2的浓度为2.84mmol/L，不能生成金属相的二硫化钼，原因为浓度太大，导致纳米颗粒之间分散不均匀，铜离子与MoS2接触受阻，由铜离子产生的应力作用变小，MoS2中S层滑移受阻，所以导致其没有产生相变；当MoS2浓度为0.11mmol/L,可以生成金属相的二硫化钼，因此当浓度低1.14mmol/L，均可导致金属相二硫化钼的产生。

Claims (1)

1.一种金属相二硫化钼的制备方法，其特征在于，步骤如下：
（1）将钼酸铵和硫脲按照摩尔比1：14进行混合，然后置于去离子水中，搅拌均匀，形成均相溶液；其中，钼酸铵的浓度为1mmol/L；
（2）将溶液转移至不锈钢反应釜中，220℃反应18h，之后自然冷却到室温；
（3）将反应液离心分离，将沉淀清洗后，真空干燥，得到MoS2粉末；
（4）将真空干燥后的MoS2粉末分散到饱和的铜盐溶液中，MoS2的浓度为1.14mmol/L；超声处理24h；
（5）将上述溶液离心分离，将沉淀清洗后，真空干燥，得到金属相二硫化钼粉末。
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CN108557888B (zh) * 2018-03-28 2021-02-26 陕西师范大学 一种金属相二硫化钼纳米结构及其制备方法
CN109742362B (zh) * 2019-01-08 2021-09-28 福建师范大学 一种锡掺杂诱导合成1t-2h混相少层二硫化钼-小球藻衍生碳复合材料的制备和应用
CN111468143A (zh) * 2020-04-24 2020-07-31 吉林大学 一种氧化亚铜/二硫化钼复合材料及其制备方法与应用
CN114392756B (zh) * 2022-01-26 2024-01-19 华中师范大学 一种压电催化材料的制备方法、产品及其应用

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