CN107601567B - A kind of method of liquid phase method synthesis triangle molybdenum disulfide nano sheet - Google Patents
A kind of method of liquid phase method synthesis triangle molybdenum disulfide nano sheet Download PDFInfo
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- CN107601567B CN107601567B CN201710783603.7A CN201710783603A CN107601567B CN 107601567 B CN107601567 B CN 107601567B CN 201710783603 A CN201710783603 A CN 201710783603A CN 107601567 B CN107601567 B CN 107601567B
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- molybdenum disulfide
- disulfide nano
- nano sheet
- triangle molybdenum
- liquid phase
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Abstract
A kind of method of liquid phase method synthesis triangle molybdenum disulfide nano sheet of the invention, belongs to technical field of nanometer material preparation, using six Ammonium paramolybdate tetrahydrates of mass ratio 1:1.87 and thiocarbamide as raw material, deionized water is solvent；Triangle molybdenum disulfide nano sheet is synthesized using liquid phase method.Sample size uniformity prepared by the present invention, Xiang Chundu is very high, sample crystallization is good, and this preparation method has many advantages, such as that process is simple, repeatability is high.
Description
Technical field
The invention belongs to the technical field of nano material preparation, in particular to a kind of methods for preparing two-dimensional nano piece.
Background technique
In recent years, with the development and application of two-dimensional layer material (for example, graphene), with molybdenum disulfide for typical two
Transient metal sulfide is tieed up due to the outstanding representation in fields such as catalysis, electronics transport, optics and mechanics, causes scientist pole
Big research interest.Compared with the full carbon of graphene composition and without the Electronic Structure Characteristics of band gap, transient metal sulfide
Component is abundant, and with the adjusting of element and size, shows the electronic structure of many novelties.For example, in electronic component
It is reported on material magazine (electronic component and material .1001-2028 (2015) 09-0007-06.): between block molybdenum disulfide is
Tape splicing gap semiconductor material (1.2eV), and the molybdenum disulfide of single layer shows the direct band gap characteristic that forbidden bandwidth is 1.9eV,
These features will expand its application field, optimize the physical and chemical properties of material.But up to the present, about preparing triangle
Molybdenum disulfide nano sheet does not have been reported, and therefore, it is necessary to explore and develop simple method to prepare triangle molybdenum disulfide nano
Piece, the physics and chemical property of extension and optimization material.
Summary of the invention
The technical problem to be solved by the present invention is overcoming the problems, such as that background technique exists and defect, provide a kind of simple
Prepare the synthetic method of triangle molybdenum disulfide nano sheet.
For the present invention using six Ammonium paramolybdate tetrahydrates and thiocarbamide as raw material, water is solvent, synthesizes triangle molybdenum disulfide nano sheet.Tool
The technical solution of body is as follows:
A kind of method of liquid phase method synthesis triangle molybdenum disulfide nano sheet, firstly, six water for being 1:1.87 by mass ratio
Close ammonium molybdate and thiocarbamide to be fitted into beaker, add deionized water and stir evenly, every gram of six Ammonium paramolybdate tetrahydrates using 100mL go from
Sub- water；The autoclave that obtained liquid is poured into polytetrafluoroethyllining lining reacts 12 hours at 180 DEG C in insulating box,
By obtained product with volume ratio be 1:3 water and ethyl alcohol washing lotion eccentric cleaning three times, obtain black sample；Black sample is put
Enter to make in the hydrochloric acid solution of pH=1 hydrochloric acid to submerge black sample, room temperature preservation 6 hours, centrifugation obtained triangle molybdenum disulfide and receives
Rice piece.
The utility model has the advantages that
The present invention prepares the advantages of triangle molybdenum disulfide nano sheet method and is: the sample morphology of preparation is regular, size
It is uniform, Xiang Chundu is very high, sample crystallization is good and this preparation method has many advantages, such as that process is simple, repeatability is high.Have
The potentiality of triangle molybdenum disulfide nano sheet are mass produced.
Detailed description of the invention
Fig. 1 is a triangle molybdenum disulfide nano sheet transmission electron microscope picture of embodiment more than 1.
Fig. 2 is the single triangle molybdenum disulfide nano sheet transmission electron microscope picture of embodiment 1.
Fig. 3 is triangle molybdenum disulfide nano sheet high resolution electron microscopy figure prepared by embodiment 1.
Fig. 4 is triangle molybdenum disulfide nano sheet energy spectrum diagram prepared by embodiment 1.
Fig. 5 is triangle molybdenum disulfide nano sheet light field scanning transmission electron microscope figure prepared by embodiment 1.
Fig. 6 is triangle molybdenum disulfide nano sheet sulphur (S) distribution diagram of element prepared by embodiment 1.
Fig. 7 is triangle molybdenum disulfide nano sheet molybdenum (Mo) distribution diagram of element prepared by embodiment 1.
Specific embodiment
The present invention is more specifically described now in conjunction with the following example, unless otherwise specified, agents useful for same be it is commercially available can
The product of acquisition is purified not plus further and is used.
Embodiment 1
Firstly, weighing 0.1 gram of six Ammonium paramolybdate tetrahydrate and 0.187 gram of thiocarbamide respectively, be fitted into beaker, then measure 10mL go from
Beaker is added in sub- water, stirs evenly, obtained liquid is poured into the autoclave of polytetrafluoroethyllining lining, is placed on insulating box
In, it is reacted 12 hours at 180 DEG C, obtains black product；The washing lotion for the water and ethyl alcohol that black product is 1:3 with volume ratio is centrifuged
Cleaning three times, obtains black sample；Black sample is put into the hydrochloric acid solution of 3mL pH=1, room temperature preservation 6 hours, is centrifuged
Obtain triangle molybdenum disulfide nano sheet.
The transmission electron microscope picture of triangle molybdenum disulfide nano sheet manufactured in the present embodiment is as illustrated in fig. 1 and 2, two sulphur of triangle
The size for changing molybdenum nanometer sheet is approximately 254nm.Fig. 3 is the high resolution electron microscopy picture of triangle molybdenum disulfide nano sheet, shows that this is received
Rice piece is monocrystalline.Fig. 4 is the energy spectrum diagram of triangle molybdenum disulfide nano sheet, shows that sample contains S and Mo element.Fig. 5~Fig. 7 is
The distribution diagram of element of triangle molybdenum disulfide nano sheet, display S and Mo element are uniformly distributed, and constitute triangle molybdenum disulfide nano
Piece.
Claims (1)
1. a kind of method of liquid phase method synthesis triangle molybdenum disulfide nano sheet, firstly, six hydrations for being 1:1.87 by mass ratio
Ammonium molybdate and thiocarbamide are fitted into beaker, are added deionized water and are stirred evenly, and every gram of six Ammonium paramolybdate tetrahydrates use 100mL deionization
Water；The autoclave that obtained liquid is poured into polytetrafluoroethyllining lining reacts 12 hours at 180 DEG C in insulating box, will
Obtained product with volume ratio be 1:3 water and ethyl alcohol washing lotion eccentric cleaning three times, obtain black sample；Black sample is put into
Hydrochloric acid is set to submerge black sample in the hydrochloric acid solution of pH=1, room temperature preservation 6 hours, centrifugation obtained triangle molybdenum disulfide nano
Piece.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710783603.7A CN107601567B (en) | 2017-09-04 | 2017-09-04 | A kind of method of liquid phase method synthesis triangle molybdenum disulfide nano sheet |
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| CN201710783603.7A CN107601567B (en) | 2017-09-04 | 2017-09-04 | A kind of method of liquid phase method synthesis triangle molybdenum disulfide nano sheet |
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| CN107601567A CN107601567A (en) | 2018-01-19 |
| CN107601567B true CN107601567B (en) | 2019-05-07 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058458A (en) * | 2014-07-07 | 2014-09-24 | 中国科学技术大学 | Method for preparing high-quality single/double-layer controllable molybdenum disulfide |
| CN104108755A (en) * | 2014-07-25 | 2014-10-22 | 深圳新宙邦科技股份有限公司 | Curved-surface molybdenum disulfide nanosheet and preparation method thereof |
| CN105140517A (en) * | 2015-09-14 | 2015-12-09 | 天津大学 | Preparation method of non-water-soluble transition metal disulphide nanosheets |
| CN106929827A (en) * | 2017-04-27 | 2017-07-07 | 郑州大学 | A kind of few layer MoS2The preparation method of film |
-
2017
- 2017-09-04 CN CN201710783603.7A patent/CN107601567B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058458A (en) * | 2014-07-07 | 2014-09-24 | 中国科学技术大学 | Method for preparing high-quality single/double-layer controllable molybdenum disulfide |
| CN104108755A (en) * | 2014-07-25 | 2014-10-22 | 深圳新宙邦科技股份有限公司 | Curved-surface molybdenum disulfide nanosheet and preparation method thereof |
| CN105140517A (en) * | 2015-09-14 | 2015-12-09 | 天津大学 | Preparation method of non-water-soluble transition metal disulphide nanosheets |
| CN106929827A (en) * | 2017-04-27 | 2017-07-07 | 郑州大学 | A kind of few layer MoS2The preparation method of film |
Non-Patent Citations (3)
| Title |
|---|
| Controllable Growth and Transfer of Monolayer MoS2 on Au Foils and Its Potential Application in Hydrogen Evolution Reaction;Jianping Shi et al.;《ACS NANO》;20140911;第8卷(第10期);第10196-10204页 |
| Synthesis of Atomically Thin MoS2 Triangles and Hexagrams and Their Electrical Transport Properties;Robert Ionescu et al.;《IEEE TRANSACTIONS ON NANOTECHNOLOGY》;20140731;第13卷(第4期);第749-754页 |
| 超薄MS2(M=Mo,W)纳米片的制备与性能研究;张向华;《中国博士学位论文全文数据库 工程科技I辑》;20150515(第05期);第50-60页 |
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