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CN105060348A - Method for preparing molybdenum disulfide nanosheet through solid-state chemical reaction - Google Patents

Method for preparing molybdenum disulfide nanosheet through solid-state chemical reaction Download PDF

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CN105060348A
CN105060348A CN201510497005.4A CN201510497005A CN105060348A CN 105060348 A CN105060348 A CN 105060348A CN 201510497005 A CN201510497005 A CN 201510497005A CN 105060348 A CN105060348 A CN 105060348A
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molybdenum disulfide
disulfide nanosheets
solid
nanosheets
chemical reaction
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陈凤娟
贾殿赠
金学坤
刘岸杰
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Xinjiang University
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Xinjiang University
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Abstract

本发明涉及一种固相化学反应制备二硫化钼纳米片的方法,属于纳米材料制备领域。该方法是将金属钼盐和硫代乙酰胺在室温条件下混合研磨,制得二维的二硫化钼纳米片,实现了二硫化钼纳米片的低热固相合成。不同于常规二硫化钼纳米片的合成方法,该方法只是通过钼酸盐的调节,利用低热固相化学法制得二硫化钼纳米片。本发明制备二硫化钼纳米片的低热固相化学法具有操作简单、不使用溶剂、高产率、成本低、合成工艺简单等特点;且本发明制备的二硫化钼纳米片具有大的比表面积和高的反应活性,将在光电器件、光催化等领域具有潜在的应用前景。The invention relates to a method for preparing molybdenum disulfide nanosheets by solid-phase chemical reaction, and belongs to the field of nanomaterial preparation. In the method, the metal molybdenum salt and thioacetamide are mixed and ground at room temperature to prepare two-dimensional molybdenum disulfide nanosheets, and the low-heat solid-phase synthesis of the molybdenum disulfide nanosheets is realized. Different from the synthesis method of conventional molybdenum disulfide nanosheets, this method only uses low-heat solid-phase chemical method to prepare molybdenum disulfide nanosheets through the adjustment of molybdate. The low-heat solid-phase chemical method for preparing molybdenum disulfide nanosheets of the present invention has the characteristics of simple operation, no solvent, high yield, low cost, and simple synthesis process; and the molybdenum disulfide nanosheets prepared by the present invention have large specific surface area and High reactivity will have potential application prospects in photoelectric devices, photocatalysis and other fields.

Description

一种固相化学反应制备二硫化钼纳米片的方法A method for preparing molybdenum disulfide nanosheets by solid phase chemical reaction

技术领域 technical field

本发明涉及一种固相化学反应制备二硫化钼纳米片的方法,属于纳米材料制备领域。 The invention relates to a method for preparing molybdenum disulfide nanosheets by solid-phase chemical reaction, and belongs to the field of nanomaterial preparation.

背景技术 Background technique

MoS2(二硫化钼)是一种抗磁性且具有半导体性质的层状二维材料,其晶体结构有1T、2H与3R三种,1T-MoS2与3R-MoS2构型是亚稳结构,通常2H-MoS2是稳定构型。2H-MoS2中每个钼原子被六个硫原子呈三角棱柱状围系,Mo-S棱面相当多,比表面积大,表面活性极高,摩擦系数低,是优良的催化剂与固体润滑剂,在催化材料与润滑材料中被广泛应用。近年来,研究人员发现二硫化钼纳米材料具有较强的润滑和催化效果。此外,由于纳米级材料的尺寸较小,其分界面处于既非长程有序、又非短程有序的高度无序状态,这就使其产生了块状材料所不具有的表面效应、小尺寸效应、量子效应和宏观量子隧道效应,表现在其具有和常规材料不同的光、热、电、磁等物理性质,因而引起了人们的极大关注。 MoS 2 (molybdenum disulfide) is a layered two-dimensional material with diamagnetic properties and semiconductor properties. Its crystal structure has three types: 1T, 2H and 3R. The configurations of 1T-MoS 2 and 3R-MoS 2 are metastable structures. , usually 2H-MoS 2 is a stable configuration. Each molybdenum atom in 2H-MoS 2 is surrounded by six sulfur atoms in a triangular prism shape. There are quite a lot of Mo-S facets, large specific surface area, high surface activity, and low friction coefficient. It is an excellent catalyst and solid lubricant. , are widely used in catalytic materials and lubricating materials. In recent years, researchers have discovered that molybdenum disulfide nanomaterials have strong lubricating and catalytic effects. In addition, due to the small size of nanoscale materials, their interface is in a highly disordered state with neither long-range order nor short-range order, which makes it produce surface effects and small size that bulk materials do not have. Effect, quantum effect, and macroscopic quantum tunneling effect, which are manifested in physical properties such as light, heat, electricity, and magnetism that are different from conventional materials, and thus have attracted great attention.

物质的性能和其形貌、结构有很大关系,通过研究性能和形貌的关系,我们可以进一步从去探讨各种反应机理,因此制备不同形貌的二硫化钼有着很重要的作用。其中,二维纳米材料因其各种特殊性质而受到越来越多人的关注。 The performance of a substance has a lot to do with its shape and structure. By studying the relationship between performance and shape, we can further explore various reaction mechanisms. Therefore, the preparation of molybdenum disulfide with different shapes plays a very important role. Among them, two-dimensional nanomaterials have attracted more and more attention due to their various special properties.

二硫化钼纳米片的制备和性能研究是当今纳米技术研究领域的一大焦点。目前,制备二硫化钼纳米片的方法主要包括水热或者溶剂热法、微乳液法、共沉淀法等技术。固相化学合成法不使用溶剂,具有高选择性、高产率、工艺过程简单等优点,已经成为合成纳米材料的一种重要方法。 The preparation and performance research of molybdenum disulfide nanosheets is a major focus in the field of nanotechnology research today. At present, the methods for preparing molybdenum disulfide nanosheets mainly include hydrothermal or solvothermal methods, microemulsion methods, co-precipitation methods and other technologies. The solid-phase chemical synthesis method does not use solvents, has the advantages of high selectivity, high yield, and simple process, and has become an important method for synthesizing nanomaterials.

发明内容 Contents of the invention

本发明的目的在于提供一种二硫化钼纳米片的制备方法,利用固相化学反应工艺通过调节金属钼盐来制备二硫化钼纳米片,为二硫化钼纳米片的合成提供了一种更简单的制备方法。 The purpose of the present invention is to provide a method for preparing molybdenum disulfide nanosheets, which uses a solid-phase chemical reaction process to prepare molybdenum disulfide nanosheets by adjusting metal molybdenum salts, which provides a simpler method for the synthesis of molybdenum disulfide nanosheets. method of preparation.

本发明公开了一种固相制备二硫化钼纳米片的方法。本发明是将金属钼盐和硫代乙酰胺作为反应物,在室温下通过研磨发生反应,进而制得二维的二硫化钼纳米片。 The invention discloses a method for preparing molybdenum disulfide nanosheets in solid state. The invention uses metal molybdenum salt and thioacetamide as reactants, reacts through grinding at room temperature, and then prepares two-dimensional molybdenum disulfide nanosheets.

本发明运用固相合成工艺实现了二硫化钼纳米片的合成,操作简单,成本低廉,环境友好,为二硫化钼纳米片的制备提供了一种新的思路。 The invention realizes the synthesis of molybdenum disulfide nanosheets by using a solid-phase synthesis process, has simple operation, low cost, and is environmentally friendly, and provides a new idea for the preparation of molybdenum disulfide nanosheets.

附图说明 Description of drawings

图1为所制备的二硫化钼纳米片的透射电镜图。 Figure 1 is a transmission electron microscope image of the prepared molybdenum disulfide nanosheets.

具体实施方式 Detailed ways

二硫化钼纳米片的固相化学合成,按以下步骤进行: The solid-phase chemical synthesis of molybdenum disulfide nanosheets is carried out in the following steps:

具体实施方式1:准确称取0.01摩尔的钼酸铵置于玛瑙研钵中,将其充分研细后加入0.02摩尔硫代乙酰胺,混合后快速研磨,继续研磨60分钟确保反应的充分进行。用去离子水和无水乙醇将其洗涤、抽滤,并于干燥箱中60度干燥2小时即得二硫化钼纳米材料。 Embodiment 1: Accurately weigh 0.01 mole of ammonium molybdate and place it in an agate mortar, grind it thoroughly and add 0.02 mole of thioacetamide, mix and grind quickly, and continue grinding for 60 minutes to ensure that the reaction is fully carried out. Wash it with deionized water and absolute ethanol, filter it with suction, and dry it in a drying oven at 60 degrees for 2 hours to obtain molybdenum disulfide nanomaterials.

具体实施方式2:准确称取0.01摩尔的钼酸钠置于玛瑙研钵中,将其充分研细后加入0.02摩尔硫代乙酰胺,混合后快速研磨,继续研磨60分钟确保反应的充分进行。用去离子水和无水乙醇将其洗涤、抽滤,并于干燥箱中60度干燥2小时即得二硫化钼纳米材料。 Specific embodiment 2: Accurately weigh 0.01 mole of sodium molybdate and place it in an agate mortar, grind it thoroughly and add 0.02 mole of thioacetamide, mix and grind quickly, and continue grinding for 60 minutes to ensure that the reaction is fully carried out. Wash it with deionized water and absolute ethanol, filter it with suction, and dry it in a drying oven at 60 degrees for 2 hours to obtain molybdenum disulfide nanomaterials.

Claims (1)

1.一种固相化学反应制备二硫化钼纳米片的方法,其特征是将金属钼盐和硫代乙酰胺以1:2的摩尔比混合,充分反应后制得二维的二硫化钼纳米片。 1. A method for preparing molybdenum disulfide nanosheets by solid-phase chemical reaction is characterized in that metal molybdenum salt and thioacetamide are mixed with a mol ratio of 1:2, and two-dimensional molybdenum disulfide nanosheets are prepared after sufficient reaction piece.
CN201510497005.4A 2015-08-14 2015-08-14 Method for preparing molybdenum disulfide nanosheet through solid-state chemical reaction Pending CN105060348A (en)

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CN105523585A (en) * 2016-02-26 2016-04-27 吉林大学 A kind of preparation method of two-dimensional MoS2 nanosheet
CN105810446A (en) * 2016-03-16 2016-07-27 杭州禹净环境科技有限公司 Preparation method for molybdenum disulfide nanosheet loaded tellurium nanotube
CN106186071A (en) * 2016-07-22 2016-12-07 中国科学院大学 The preparation method of a kind of two-dimension nano materials and two-dimension nano materials
CN106865616A (en) * 2017-03-30 2017-06-20 华南师范大学 The method for preparing the porous two-dimentional molybdenum disulfide nano sheet of high density
CN110614104A (en) * 2019-07-29 2019-12-27 西安工程大学 Preparation method of photocatalyst for efficiently treating sewage
CN111569911A (en) * 2020-05-22 2020-08-25 重庆工商大学 A kind of preparation method of 3R type molybdenum disulfide catalyst

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105523585A (en) * 2016-02-26 2016-04-27 吉林大学 A kind of preparation method of two-dimensional MoS2 nanosheet
CN105523585B (en) * 2016-02-26 2017-01-25 吉林大学 A kind of preparation method of two-dimensional MoS2 nanosheet
CN105810446A (en) * 2016-03-16 2016-07-27 杭州禹净环境科技有限公司 Preparation method for molybdenum disulfide nanosheet loaded tellurium nanotube
CN106186071A (en) * 2016-07-22 2016-12-07 中国科学院大学 The preparation method of a kind of two-dimension nano materials and two-dimension nano materials
CN106186071B (en) * 2016-07-22 2017-12-01 中国科学院大学 The preparation method and two-dimension nano materials of a kind of two-dimension nano materials
CN106865616A (en) * 2017-03-30 2017-06-20 华南师范大学 The method for preparing the porous two-dimentional molybdenum disulfide nano sheet of high density
CN106865616B (en) * 2017-03-30 2018-03-27 华南师范大学 The method for preparing the porous two-dimentional molybdenum disulfide nano sheet of high density
CN110614104A (en) * 2019-07-29 2019-12-27 西安工程大学 Preparation method of photocatalyst for efficiently treating sewage
CN111569911A (en) * 2020-05-22 2020-08-25 重庆工商大学 A kind of preparation method of 3R type molybdenum disulfide catalyst
CN111569911B (en) * 2020-05-22 2022-04-22 重庆工商大学 Preparation method of 3R type molybdenum disulfide catalyst

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