CN104402055B - The preparation method of large scale lamellar orderly hexagonal tungsten disulfide - Google Patents
The preparation method of large scale lamellar orderly hexagonal tungsten disulfide Download PDFInfo
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- CN104402055B CN104402055B CN201410597619.5A CN201410597619A CN104402055B CN 104402055 B CN104402055 B CN 104402055B CN 201410597619 A CN201410597619 A CN 201410597619A CN 104402055 B CN104402055 B CN 104402055B
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- C01G41/00—Compounds of tungsten
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract
A kind of preparation method of large scale lamellar orderly hexagonal tungsten disulfide, it is characterized in that as follows: take tungsten disulfide amorphous powder and load ceramic boat, it is placed in tube furnace central authorities, after emptying air, atmosphere 1200 DEG C ~ 1300 DEG C reaction of the mixed gas that the hydrogen at nitrogen and sulfur steam atmosphere or the nitrogen of 92 ~ 97% with 3 ~ 8% is constituted 2 ~ 4 hours.Nanometer layer lamellar hexagonal tungsten disulfide of the present invention has good electric conductivity under visible light, photoelectricity and data storage device can be effectively applied to, invent described nanometer layer lamellar hexagonal tungsten disulfide simultaneously and there is good lubricity, machining industry can be efficiently applied to.
Description
Technical field
The invention belongs to field of material preparation, relate to the preparation method of a kind of Wolfram disulfide nano material.
Background technology
In recent years, two-dimensional nanostructure, owing to presenting brand-new specific performance, has caused substantial amounts of concern.Laminated structure nano material is respectively provided with considerable application prospect due to many characteristics such as its multifunctionality, low-surface-energy, geometry effect, memory effect, interfacial effects in each field.
Tungsten disulfide has many significantly physical characteristics, as high temperature resistant, coefficient of friction is relatively low, comprcssive strength is big, antioxidation, cracking performance high, be catalyzed activity stabilized reliably, length in service life etc..
In recent years, due to the discovery of Graphene peculiar property, metal-thiolate clusters compound two-dimension nano materials causes each field keen interest.Transition metal two chalcogenide has sandwich structure, and the two-layer up and down having S atom to constitute is middle containing the intermediate layer being made up of with hexagon metallic atom.Two dimension tungsten disulfide stratified nano materials has similar performance in some aspects to Graphene, has the performance of self uniqueness simultaneously.But, the most common tungsten disulfide scantling is less, shape is the most regular, is generally unsuitable for making electricity device.
Summary of the invention
The present invention mainly provides the preparation method of a kind of large scale lamellar orderly hexagonal tungsten disulfide material preparing simple, controlled shape.
The present invention is achieved by the following technical solutions.
The preparation process that the present invention is concrete is as follows:
Take tungsten disulfide amorphous powder and load ceramic boat, be placed in tube furnace central authorities.After emptying air, atmosphere 1200 DEG C ~ 1300 DEG C reaction of the mixed gas that the hydrogen at nitrogen and sulfur steam atmosphere or the nitrogen of 92 ~ 97% with 3 ~ 8% is constituted 2 ~ 4 hours.
Nanometer layer lamellar hexagonal tungsten disulfide of the present invention has good electric conductivity under visible light, can be effectively applied to photoelectricity and data storage device.Invent described nanometer layer lamellar hexagonal tungsten disulfide simultaneously and there is good lubricity, machining industry can be efficiently applied to.
Accompanying drawing explanation
Fig. 1 is the XRD test analysis figure of large scale lamellar of the present invention orderly hexagonal tungsten disulfide.
Fig. 2 is the environmental scanning electronic microscope map analysis of large scale lamellar of the present invention orderly hexagonal tungsten disulfide.
Fig. 3 is the environmental scanning electronic microscope map analysis of large scale lamellar of the present invention orderly hexagonal tungsten disulfide.
Fig. 4 is the XRD test analysis figure of large scale lamellar of the present invention orderly hexagonal tungsten disulfide.
Fig. 5 is the environmental scanning electronic microscope map analysis of large scale lamellar of the present invention orderly hexagonal tungsten disulfide.
Fig. 6 is the transmission electron microscope map analysis of large scale lamellar of the present invention orderly hexagonal tungsten disulfide.
Detailed description of the invention
The present invention will be described further by following example.
Embodiment 1.
Take tungsten disulfide amorphous powder and load ceramic boat, be placed in tube furnace central authorities.After emptying air, nitrogen 92% and 8% the mixed gas atmosphere that constitutes of hydrogen under 1300 DEG C react 2 hours.Obtain tungsten disulfide class Graphene laminated structure nano material.Final prepared such as large scale lamellar orderly hexagonal tungsten disulfide in Fig. 1.
Embodiment 2.
Take tungsten disulfide amorphous powder and load ceramic boat, be placed in tube furnace central authorities, take appropriate Sublimed Sulfur and fill ceramic boat and be placed in inlet end.After emptying air, 1200 DEG C are reacted 2 hours under nitrogen atmosphere.Obtain tungsten disulfide class Graphene laminated structure nano material.Final prepared such as large scale lamellar orderly hexagonal tungsten disulfide in Fig. 3.
Embodiment 3.
Take tungsten disulfide amorphous powder and load ceramic boat, be placed in tube furnace central authorities, take appropriate Sublimed Sulfur and fill ceramic boat and be placed in inlet end.After emptying air, 1250 DEG C are reacted 2 hours under nitrogen atmosphere.Obtain large scale lamellar orderly hexagonal tungsten disulfide.
Embodiment 4.
Take tungsten disulfide amorphous powder and load ceramic boat, be placed in tube furnace central authorities.After emptying air, nitrogen 97% and 3% the mixed gas atmosphere that constitutes of hydrogen under 1200 DEG C react 3 hours.Obtain large scale lamellar orderly hexagonal tungsten disulfide.
Embodiment 5.
Take tungsten disulfide amorphous powder and load ceramic boat, be placed in tube furnace central authorities.After emptying air, nitrogen 95% and 5% the mixed gas atmosphere that constitutes of hydrogen under 1300 DEG C react 4 hours.Obtain tungsten disulfide class Graphene laminated structure nano material.Final prepared such as large scale lamellar orderly hexagonal tungsten disulfide in Fig. 5.
Obviously, those skilled in the art can carry out various change and modification without departing from the spirit and scope of the present invention to large scale lamellar orderly hexagonal tungsten disulfide of the present invention and preparation method thereof.So, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these variation and modification.
Claims (1)
1. the preparation method of a large scale lamellar orderly hexagonal tungsten disulfide, it is characterized in that as follows: take tungsten disulfide amorphous powder and load ceramic boat, it is placed in tube furnace central authorities, after emptying air, atmosphere 1200 DEG C ~ 1300 DEG C reaction of the mixed gas that the hydrogen at nitrogen and sulfur steam atmosphere or the nitrogen of 92 ~ 97% with 3 ~ 8% is constituted 2 ~ 4 hours.
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| CN201410597619.5A CN104402055B (en) | 2014-10-31 | 2014-10-31 | The preparation method of large scale lamellar orderly hexagonal tungsten disulfide |
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| CN201410597619.5A CN104402055B (en) | 2014-10-31 | 2014-10-31 | The preparation method of large scale lamellar orderly hexagonal tungsten disulfide |
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| CN104402055A CN104402055A (en) | 2015-03-11 |
| CN104402055B true CN104402055B (en) | 2016-10-12 |
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| CN107119328B (en) * | 2017-04-07 | 2019-06-21 | 湖南大学 | A kind of stratiform WS with complicated helical structure2Two-dimension nano materials and preparation method thereof |
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| CN101857274B (en) * | 2010-06-13 | 2012-01-04 | 中南大学 | Method for preparing nano WS2/MoS2 granules |
| CN103771521B (en) * | 2014-02-26 | 2015-02-25 | 新疆大学 | Method for preparing tungsten disulfide nano sheet |
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