CN101712492A - Method for preparing mono-disperse molybdenum disulfide nano sheet - Google Patents
Method for preparing mono-disperse molybdenum disulfide nano sheet Download PDFInfo
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- CN101712492A CN101712492A CN200910227198A CN200910227198A CN101712492A CN 101712492 A CN101712492 A CN 101712492A CN 200910227198 A CN200910227198 A CN 200910227198A CN 200910227198 A CN200910227198 A CN 200910227198A CN 101712492 A CN101712492 A CN 101712492A
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Abstract
The invention provides a method for preparing a mono-disperse molybdenum disulfide nano sheet, which is characterized in that a mixture of molybdenum oxide and sulfur is used as a raw material, and the mixture is activated through ball milling in protective atmosphere; and then the mixture is annealed at the constant temperature of between 400 and 700 DEG C to be fully vulcanized so as to obtain mono-disperse molybdenum disulfide nano sheet granules. A large amount of mono-disperse molybdenum disulfide nano material is prepared through the simple and effective chemical synthesis method; and the method is simple and quick, has low production cost, and provides possibility for the broad application of the material in the aspects of lubrication and catalysis.
Description
Technical field
The invention belongs to field of nano material preparation, relate to a kind of single preparation method who disperses molybdenum disulfide nano sheet.
Technical background
Nano molybdenum disulfide (MoS
2) because of having very high specific surface area and good light, electricity, lubricated, catalytic performance, be with a wide range of applications at aspects such as electronic probe, oil catalysis, hydrogen storage material, friction, lubrication and solar cells.At present, the method for preparing the molybdenum disulfide nano material mainly comprises high temperature gas-solid reaction method, thermal decomposition method, hydrothermal method, electrochemical process, chemical Vapor deposition process etc.The appearance structure of the molybdenum disulfide nano material of preparing also has nothing in common with each other, comprise nanotube, nano wire, nanometer rod, nanometer flower, hollow nano-sphere and inorganic fullerene structure, it is less that but two-dimensional nanostructure is but reported, mainly be because molybdenumdisulphide belongs to typical laminated structure, the layer with layer between all be to combine with more weak Van der Waals force, under ectocine, the dangling bonds at lamella two ends are unstability very easily, take place to curl, thereby form closed tubulose or fullerene structure.
And as petroleum catalyst, the main activity site of molybdenumdisulphide is exactly to be positioned at lamella periphery keys (rims and edges) all around, the basic catalytically inactive of basal plane, therefore prepare the two-dimensional sheet nanostructure, obtain more periphery keys, improve the catalytic activity of catalyzer, become an important techniques difficult problem.The Tye of UBC (UBC) etc. make the molybdenumdisulphide of individual layer by lift-off technology, and study its catalytic performance, the result shows, single layer structure can effectively improve catalytic activity, but lift-off technology only is at structure cleavage longitudinally, can't produce horizontal basal plane cut apart thinning effect, therefore, prepare nano level single sheet nanostructure of disperseing, become and limit the bottleneck that its catalytic performance further improves.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of mass production list and disperses MoS
2The preparation method of nanometer sheet, it is low that it has a production cost, is easy to produce in batches product epigranular, active high characteristics.
Technical solution of the present invention is as follows:
A kind of single preparation method who disperses molybdenum disulfide nano sheet, it is characterized in that, with the mol ratio is that the molybdenum oxide of 10-0.05 and the mixture of sulphur are raw material, make it ball milling activation back constant temperature under 400-700 ℃ of condition in the shielding gas atmosphere, annealing, in constant temperature and annealed preposition sulphur powder sulphur source as a supplement simultaneously, be cooled to again below 200 ℃, can make single molybdenum disulfide nano sheet that disperses; The sulphur powder in described sulphur as a supplement source and the mass ratio of reaction mixture are between 10-0.05.
Described ball milling reactivation process is: as ball-milling medium, ratio of grinding media to material is 10-80 with Stainless Steel Ball: 1, and with 100-600rmp ball milling 2-120h.
Constant temperature time is 30min-120min.
Insulation and annealed environment are tube furnace; the mixture of molybdenum oxide and sulphur is placed on respectively in 2 different porcelain boats with the sulphur powder in sulphur source as a supplement; when insulation and annealing, 2 porcelain boats all are in the described tube furnace, and the porcelain boat of dress sulphur powder is placed on the place, upper reaches of shielding gas.
Described shielding gas is argon gas or nitrogen.
Beneficial effect:
The present invention has prepared a large amount of single sheet molybdenum disulfide nano materials that disperses by simple and effective chemical synthesis process, the method simple and fast, and production cost is low, for it provides possibility in the widespread use aspect lubricated and the catalysis.
Products therefrom of the present invention is pure single molybdenum disulfide nano sheet that disperses, and granularity is between 50-200nm, as shown in Figure 1.
The present invention prepares single molybdenum disulfide nano sheet that disperses, and simple for process, cost is low, and it is little to make product granularity, and is active high, is expected to produce in enormous quantities.Traditional physical purification and mechanical crushing method prepare ultra-fine molybdenumdisulphide, minimum particle size has reached 550nm abroad, and domestic is 1500nm, yet because of cold welding in the shattering process and reunion regrowth effect, further refinement of granularity becomes the bottleneck in the ultra-fine molybdenumdisulphide technology of preparing.The present invention avoids traditional physics fragmentation, and activation of set Mechanical Crushing and high-temperature chemical reaction successfully stop particle to be grown up, make the following nanometer MOS 2 particle of 200nm, this grain graininess is littler, and activity is higher, have stronger adhesive power, can effectively improve lubricity and catalytic performance.
Description of drawings
Fig. 1 is single field emission scanning electron microscope (SEM) photo that disperses molybdenum disulfide nano sheet that the present invention makes;
Fig. 2 is single X-ray diffraction (XRD) collection of illustrative plates that disperses molybdenum disulfide nano sheet that the present invention makes.
Embodiment
Below with reference to figure and specific implementation process the present invention is described in further details:
Embodiment 1
5g molybdenum oxide and 10g sulphur are mixed in the adding stainless steel jar mill, feed argon gas as shielding gas, as ball-milling medium, ratio of grinding media to material is 60: 1 with Stainless Steel Ball, with 400rpm ball milling 24h.Take out 1g and put into porcelain boat from the ball milling activation products, other gets the porcelain boat 2g sulphur of packing into; Tube furnace feeds argon gas in advance and drains air, and is heated to 600 ℃, then above-mentioned two boats is placed the heating zone, and wherein, the porcelain boat of dress sulphur places the gas upper reaches to locate sulphur source as a supplement; Behind the constant temperature 2h, cool to 200 ℃ with the furnace under argon atmosphere, take out porcelain boat, collect black powder, can obtain single molybdenum disulfide nano sheet that disperses, granularity is between 50-200nm.
Embodiment 2
5g molybdenum oxide and 10g sulphur are mixed in the adding stainless steel jar mill, feed argon gas as shielding gas, as ball-milling medium, ratio of grinding media to material is 60: 1 with Stainless Steel Ball, with 400rmp ball milling 24h.Take out 1g and put into porcelain boat from the ball milling activation products, tube furnace feeds argon gas in advance and drains air, and is heated to 600 ℃, then porcelain boat is placed the heating zone, does not have the sulphur source of replenishing; Behind the constant temperature 2h, cool to 200 ℃ with the furnace under argon atmosphere, take out porcelain boat, collect black powder, adopt XRD to detect, the result shows that product comprises molybdenumdisulphide and partial oxidation molybdenum, illustrates that sulfuration is incomplete, therefore must preposition additional sulphur source.
Embodiment 3
5g molybdenum oxide and 10g sulphur are mixed in the adding stainless steel jar mill, feed argon gas as shielding gas, as ball-milling medium, ratio of grinding media to material is 60: 1 with Stainless Steel Ball, with 400rmp ball milling 24h.Take out 1g and put into porcelain boat from the ball milling activation products, other gets the porcelain boat 2g sulphur of packing into; Tube furnace feeds argon gas in advance and drains air, and is heated to 400 ℃, then above-mentioned two boats is placed the heating zone, and wherein, the porcelain boat of dress sulphur places the gas upper reaches to locate sulphur source as a supplement; Behind the constant temperature 2h, cool to 200 ℃ with the furnace under argon atmosphere, take out porcelain boat, collect black powder, can obtain single molybdenum disulfide nano sheet that disperses, pattern is identical with example 1 with structure, but degree of crystallinity is relatively poor relatively.
Embodiment 4
5g molybdenum oxide and 10g sulphur are mixed in the adding stainless steel jar mill, feed argon gas as shielding gas, as ball-milling medium, ratio of grinding media to material is 60: 1 with Stainless Steel Ball, with 400rmp ball milling 24h.Take out 1g and put into porcelain boat from the ball milling activation products, other gets the porcelain boat 2g sulphur of packing into; Tube furnace feeds argon gas in advance and drains air, and is heated to 700 ℃, then above-mentioned two boats is placed the heating zone, and wherein, the porcelain boat of dress sulphur places the gas upper reaches to locate sulphur source as a supplement; Behind the constant temperature 2h, cool to 200 ℃ with the furnace under argon atmosphere, take out porcelain boat, collect black powder, can obtain single molybdenum disulfide nano sheet that disperses, pattern is identical with example 1 with structure, and degree of crystallinity is better.
Comparative Examples
0.33g molybdenum oxide and 0.67g sulphur without ball milling, are directly mixed, put into porcelain boat, other gets the porcelain boat 2g sulphur of packing into; Tube furnace feeds argon gas in advance and drains air, and is heated to 600 ℃, then above-mentioned two boats is placed the heating zone, and wherein, the porcelain boat of dress sulphur places the gas upper reaches to locate sulphur source as a supplement; Behind the constant temperature 2h, cool to 200 ℃ with the furnace under argon atmosphere, take out porcelain boat, collect black powder, the result shows, can't obtain single molybdenum disulfide nano sheet that disperses under this condition, and the products therefrom granularity is big to several microns, and vulcanizes insufficiently, and the surface portion sulfuration is only arranged.
Claims (5)
1. single preparation method who disperses molybdenum disulfide nano sheet, it is characterized in that, with the mol ratio is that the molybdenum oxide of 10-0.05 and the mixture of sulphur are raw material, make it ball milling activation back constant temperature under 400-700 ℃ of condition in the shielding gas atmosphere, annealing, in constant temperature and annealed preposition sulphur powder sulphur source as a supplement simultaneously, be cooled to again below 200 ℃, can make single molybdenum disulfide nano sheet that disperses; The sulphur powder in described sulphur as a supplement source and the mass ratio of reaction mixture are between 10-0.05.
2. single preparation method who disperses molybdenum disulfide nano sheet according to claim 1, it is characterized in that described ball milling reactivation process is: as ball-milling medium, ratio of grinding media to material is 10-80 with Stainless Steel Ball: 1, with 100-600rmp ball milling 2-120h.
3. single preparation method who disperses molybdenum disulfide nano sheet according to claim 1 is characterized in that constant temperature time is 30min-120min.
4. single preparation method who disperses molybdenum disulfide nano sheet according to claim 1; it is characterized in that; insulation and annealed environment are tube furnace; the mixture of molybdenum oxide and sulphur is placed on respectively in 2 different porcelain boats with the sulphur powder in sulphur source as a supplement; when insulation and annealing; 2 porcelain boats all are in the described tube furnace, and the porcelain boat of dress sulphur powder is placed on the place, upper reaches of shielding gas.
5. single preparation method who disperses molybdenum disulfide nano sheet according to claim 1 is characterized in that described shielding gas is argon gas or nitrogen.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102398920A (en) * | 2011-11-07 | 2012-04-04 | 北京航空航天大学 | Method for preparing two-dimensional nano molybdenum disulfide by jet cavitation technology |
| CN102583547A (en) * | 2012-03-07 | 2012-07-18 | 长安大学 | Preparation method of monolayer MoS2 nano-sheet solution |
| CN103614777A (en) * | 2013-10-15 | 2014-03-05 | 中国科学院理化技术研究所 | Preparation method of large-area single-layer and multi-layer molybdenum diselenide single crystal wafer |
| CN103695873A (en) * | 2013-12-23 | 2014-04-02 | 向勇 | Preparation method of monomolecular layer/polymolecular layer molybdenum disulfide film |
| CN103964507A (en) * | 2014-05-08 | 2014-08-06 | 中国科学技术大学 | Single-layer transition metal sulfur compound thin film and preparation method thereof |
| CN104355363A (en) * | 2014-11-20 | 2015-02-18 | 中南大学 | Method for cleaning up oil dirt on water surface through MoS2 adsorbent and recycling method of adsorbent |
| CN104709892A (en) * | 2013-12-11 | 2015-06-17 | 中国科学院大连化学物理研究所 | Method for controllably preparing single layer and few layer molybdenum sulfide |
| 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 |
| CN107892330A (en) * | 2017-12-01 | 2018-04-10 | 东华大学 | A kind of preparation method of piece heap molybdenum disulfide nano tube |
| CN110357162A (en) * | 2019-07-22 | 2019-10-22 | 金堆城钼业股份有限公司 | A method of efficiently synthesizing high pure alcohol |
| CN110436525A (en) * | 2019-07-22 | 2019-11-12 | 金堆城钼业股份有限公司 | A kind of preparation method of micro-/ nano molybdenum disulfide |
| WO2021059325A1 (en) * | 2019-09-24 | 2021-04-01 | Dic株式会社 | Molybdenum sulfide powder and method for producing same |
| CN113788497A (en) * | 2021-08-12 | 2021-12-14 | 华南理工大学 | Multiphase molybdenum sulfide composite material and preparation method and application thereof |
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2009
- 2009-12-11 CN CN200910227198A patent/CN101712492A/en active Pending
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102398920B (en) * | 2011-11-07 | 2013-07-03 | 北京航空航天大学 | Method for preparing two-dimensional nano molybdenum disulfide by jet cavitation technology |
| CN102398920A (en) * | 2011-11-07 | 2012-04-04 | 北京航空航天大学 | Method for preparing two-dimensional nano molybdenum disulfide by jet cavitation technology |
| CN102583547A (en) * | 2012-03-07 | 2012-07-18 | 长安大学 | Preparation method of monolayer MoS2 nano-sheet solution |
| CN102583547B (en) * | 2012-03-07 | 2013-12-04 | 长安大学 | Preparation method of monolayer MoS2 nano-sheet solution |
| CN103614777A (en) * | 2013-10-15 | 2014-03-05 | 中国科学院理化技术研究所 | Preparation method of large-area single-layer and multi-layer molybdenum diselenide single crystal wafer |
| CN104709892A (en) * | 2013-12-11 | 2015-06-17 | 中国科学院大连化学物理研究所 | Method for controllably preparing single layer and few layer molybdenum sulfide |
| CN103695873B (en) * | 2013-12-23 | 2016-03-16 | 向勇 | A kind of preparation method of monomolecular layer/polymolecular layer molybdenum disulfide film |
| CN103695873A (en) * | 2013-12-23 | 2014-04-02 | 向勇 | Preparation method of monomolecular layer/polymolecular layer molybdenum disulfide film |
| CN103964507A (en) * | 2014-05-08 | 2014-08-06 | 中国科学技术大学 | Single-layer transition metal sulfur compound thin film and preparation method thereof |
| CN103964507B (en) * | 2014-05-08 | 2015-10-21 | 中国科学技术大学 | A kind of individual layer transition metal chalcogenide film and preparation method thereof |
| CN104355363A (en) * | 2014-11-20 | 2015-02-18 | 中南大学 | Method for cleaning up oil dirt on water surface through MoS2 adsorbent and recycling method of adsorbent |
| CN104355363B (en) * | 2014-11-20 | 2016-08-24 | 中南大学 | Utilize MoS2method and the recovery method of adsorbent of water oil stain removed by adsorbent |
| 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 |
| 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 |
| CN107892330A (en) * | 2017-12-01 | 2018-04-10 | 东华大学 | A kind of preparation method of piece heap molybdenum disulfide nano tube |
| CN107892330B (en) * | 2017-12-01 | 2019-06-25 | 东华大学 | A kind of preparation method of piece heap molybdenum disulfide nano tube |
| CN110357162A (en) * | 2019-07-22 | 2019-10-22 | 金堆城钼业股份有限公司 | A method of efficiently synthesizing high pure alcohol |
| CN110436525A (en) * | 2019-07-22 | 2019-11-12 | 金堆城钼业股份有限公司 | A kind of preparation method of micro-/ nano molybdenum disulfide |
| CN110436525B (en) * | 2019-07-22 | 2021-09-28 | 金堆城钼业股份有限公司 | Preparation method of micro/nano molybdenum disulfide |
| CN110357162B (en) * | 2019-07-22 | 2021-11-09 | 金堆城钼业股份有限公司 | Method for efficiently synthesizing high-purity molybdenum disulfide |
| WO2021059325A1 (en) * | 2019-09-24 | 2021-04-01 | Dic株式会社 | Molybdenum sulfide powder and method for producing same |
| CN113788497A (en) * | 2021-08-12 | 2021-12-14 | 华南理工大学 | Multiphase molybdenum sulfide composite material and preparation method and application thereof |
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Application publication date: 20100526 |