CN107804874A - 一种气凝胶状二硫化钼纳米材料的制备方法 - Google Patents

一种气凝胶状二硫化钼纳米材料的制备方法 Download PDF

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CN107804874A
CN107804874A CN201711250354.1A CN201711250354A CN107804874A CN 107804874 A CN107804874 A CN 107804874A CN 201711250354 A CN201711250354 A CN 201711250354A CN 107804874 A CN107804874 A CN 107804874A
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molybdenum disulfide
disulfide nano
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airsetting glue
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郑学军
裴大钊
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Xiangtan University
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Abstract

本发明公开了一种气凝胶状二硫化钼纳米材料的制备方法，其制备方法是使用四水钼酸铵作为钼源，硫脲作为硫源，在反应温度220摄氏度，反应时间为24小时的水热条件下合成花状二硫化钼纳米球。水浴超声处理水热反应合成的花状纳米球1小时，接着在‑50摄氏度真空环境冷冻干燥超声处理后的二硫化钼36小时，获得气凝胶状二硫化钼纳米材料。所合成的材料因其具有介孔结构在锂离子电池和超级电容器等领域具有广阔的应用前景。

Description

一种气凝胶状二硫化钼纳米材料的制备方法
技术领域
本发明涉及一种气凝胶状二硫化钼纳米材料的制备方法，属于纳米材料制备领域。
背景技术
二硫化钼是一种典型的过渡金属硫化物，由六方晶系的单层或多层二硫化钼组成的具有“三明治夹心”结构的化合物。其中单层二硫化钼由三层原子层构成，上下两层均为硫原子层，中间一层为钼原子层，钼原子层被两层硫原子层所夹形成类“三明治”结构。这种结构使得层内存在较强的共价键，层间则存在较弱的范德华力，S原子暴露在MoS2晶体表面，对金属表面产生较强的吸附作用。多层二硫化钼由若干单层二硫化钼组成，层间距大约为0.65 纳米。作为一种重要的二维层状纳米材料，二硫化钼以其独特的“三明治夹心”结构在润滑剂、电催化、能源储备等众多领域得到了广泛的应用。
花状二硫化钼纳米球材料的制备方法多为水热法。Ke-Jing Huang等用Na2MoO4·2H2O作为钼源，L-半胱氨酸作为硫源，摩尔比为1：3混合搅拌成均匀溶液倒入聚四氟乙烯反应釜，在180摄氏度水热反应48小时得到花状二硫化钼。此方法得到二硫化钼样品的比表面积较低，抑制其作为储能电极材料时器件的电化学性能。
本发明专利基于水热法的基础上增加后续超声处理和冷冻干燥步骤，提供一种气凝胶状二硫化钼纳米材料的制备方法，这种气凝胶状二硫化钼纳米材料具有高的比表面积和介孔密度，提高二硫化钼在储能领域的应用性能。
发明内容
本发明的目的是提供一种高比表面积和介孔密度的气凝胶状二硫化钼纳米材料的制备方法。
本发明采用的技术方案步骤如下：
第一步：用去离子水溶解四水钼酸铵，得到溶液A；
第二步：将硫脲溶解到溶液A中，得到溶液B；
第三步：将溶液B磁力搅拌1小时得到均匀溶液C；
第四步：将溶液C转移至不锈钢高压反应釜的聚四氟乙烯内衬中，在220摄氏度反应24小时得到反应混合产物，待不锈钢高压反应釜自然冷却至室温后，先除去上层清液，随后将反应混合产物转移至烧杯中；
第五步：使用去离子水与乙醇分别清洗反应混合产物三次，静置沉淀除去上层清液后得到含乙醇的花状二硫化钼纳米球；
第六步：将含乙醇的花状二硫化钼纳米球放入真空干燥箱中，在50摄氏度下干燥8小时，得到干燥的花状二硫化钼纳米球；
第七步：将水热反应合成的花状二硫化钼粉末加入到去离子水中，超声波处理60分钟；
第八步：将超声波处理后的溶液放入冷冻干燥机，在-50摄氏度下冷冻12小时；
第九步：开启冷冻干燥机真空泵抽真空，待冰块完全升华后得到气凝胶状二硫化钼纳米材料。
上述四水钼酸铵与硫脲的摩尔比为1：15。
本发明的有益效果是：气凝胶状二硫化钼纳米材料具有高的比表面积和孔径密度，这种结构在储能领域具有广泛的应用。应用于超级电容器领域，作为电极材料高比表面积可提供更多的活性位点可增加超级电容器的比电容；应用于锂离子电池领域，作为锂离子电池负极材料利用多孔界面和表面的缺陷结构缓解嵌锂过程中的体积膨胀可提高锂离子电池的循环稳定性。
附图说明
图1是实施例1所得气凝胶状二硫化钼的XRD图谱。
图2是实施例1所得气凝胶状二硫化钼的Raman图谱。
图3是实施例1所得气凝胶状二硫化钼的低分辨率SEM照片。
图4是实施例1所得气凝胶状二硫化钼的高分辨率SEM照片。
图5是实施例1所得气凝胶状二硫化钼的氮吸附/脱附等温线图。
图6是实施例1所得气凝胶状二硫化钼的孔径分布图
具体实施方式
制备气凝胶状二硫化钼纳米材料，其主要步骤为：
实施例1：
(1) 分别称取1mmol 四水钼酸铵和15mmol 硫脲溶解在40ml 去离子水中，将溶液磁力搅拌1小时得到均匀溶液；
(2) 将溶液转移至不锈钢高压反应釜的聚四氟乙烯内衬中，在220摄氏度保温24小时得到反应混合产物，待不锈钢高压反应釜自然冷却至室温后，先除去上层清液，随后将反应混合产物转移至烧杯中；
(3) 使用去离子水与乙醇分别清洗反应混合产物三次，静置沉淀除去上层清液后得到含乙醇的花状二硫化钼纳米球；
(4) 将含乙醇的花状二硫化钼纳米球放入真空干燥箱中，在50摄氏度下干燥8小时，得到干燥的花状二硫化钼纳米球。将水热反应合成的花状二硫化钼粉末加入到去离子水中，超声波处理60分钟；
(5) 超声波处理后的溶液放入冷冻干燥机，在-50摄氏度下冷冻12小时；
(6) 开启冷冻干燥机真空泵抽真空，待冰块完全升华后得到气凝胶状二硫化钼纳米材料。

Claims (2)

1.一种气凝胶状二硫化钼纳米材料的制备方法，其特征在于：水热反应、超声处理和冷冻干燥。
2.根据权利要求1所述的一种气凝胶状二硫化钼纳米材料的制备方法，其特征在于：
第一步：用去离子水溶解四水钼酸铵，得到溶液A；
第二步：将硫脲溶解到溶液A中，得到溶液B；
第三步：将溶液B磁力搅拌1小时得到均匀溶液C；
第四步：将溶液C转移至不锈钢高压反应釜的聚四氟乙烯内衬中，在220摄氏度反应24小时得到反应混合产物，待不锈钢高压反应釜自然冷却至室温后，先除去上层清液，随后将反应混合产物转移至烧杯中；
第五步：使用去离子水与乙醇分别清洗反应混合产物三次，静置沉淀除去上层清液后得到含乙醇的花状二硫化钼纳米球；
第六步：将含乙醇的花状二硫化钼纳米球放入真空干燥箱中，在50摄氏度下干燥8小时，得到干燥的花状二硫化钼纳米球；
第七步：将水热反应合成的花状二硫化钼粉末加入到去离子水中，超声波处理60分钟；
第八步：将超声波处理后的溶液放入冷冻干燥机，在-50摄氏度下冷冻12小时；
第九步：开启冷冻干燥机真空泵抽真空，待冰块完全升华后得到气凝胶状二硫化钼纳米材料。
CN201711250354.1A 2017-12-01 2017-12-01 一种气凝胶状二硫化钼纳米材料的制备方法 Pending CN107804874A (zh)

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CN108786855A (zh) * 2017-05-04 2018-11-13 中国计量大学 一种介孔二硫化钼可见光催化剂材料的制备方法及其在降解抗生素废水领域中的应用
CN110853935A (zh) * 2019-11-21 2020-02-28 北京协同创新研究院 一种硫化钼超级电容器电极及其制备方法
CN111099658A (zh) * 2020-01-07 2020-05-05 南开大学 一种不同层间距二硫化钼纳米材料的制备方法
CN113522319A (zh) * 2021-07-05 2021-10-22 北京建筑大学 一种催化材料的制备方法及其应用

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CN106732668A (zh) * 2016-11-18 2017-05-31 中国计量大学 一种花状二硫化钼/氧化铜复合纳米材料的水热制备方法
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108786855A (zh) * 2017-05-04 2018-11-13 中国计量大学 一种介孔二硫化钼可见光催化剂材料的制备方法及其在降解抗生素废水领域中的应用
CN110853935A (zh) * 2019-11-21 2020-02-28 北京协同创新研究院 一种硫化钼超级电容器电极及其制备方法
CN111099658A (zh) * 2020-01-07 2020-05-05 南开大学 一种不同层间距二硫化钼纳米材料的制备方法
CN113522319A (zh) * 2021-07-05 2021-10-22 北京建筑大学 一种催化材料的制备方法及其应用

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