CN105417582A - Method for preparing graphite-like tungsten disulfide nano-sheet - Google Patents
Method for preparing graphite-like tungsten disulfide nano-sheet Download PDFInfo
- Publication number
- CN105417582A CN105417582A CN201510975198.XA CN201510975198A CN105417582A CN 105417582 A CN105417582 A CN 105417582A CN 201510975198 A CN201510975198 A CN 201510975198A CN 105417582 A CN105417582 A CN 105417582A
- Authority
- CN
- China
- Prior art keywords
- graphite
- tungsten disulfide
- disulfide nano
- preparation
- nano slices
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
The invention provides a method for preparing a graphite-like tungsten disulfide nano-sheet. The method comprises the following steps of dissolving a surfactant in water, adding Na2S, NH2OH.HCl and Na2WO4 into the solution, conducting stirring, and regulating the pH value of the solution to be 6-8; then, removing the prepared solution into a reaction kettle, sealing the reaction kettle, reacting at a constant temperature, cooling the solution to room temperature to obtain a reaction product; and finally, separating, washing and drying the prepared reaction product to obtain the graphite-like tungsten disulfide nano-sheet. The preparation method is low in cost, has a simple and easily controlled production process and high product yield, and is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method of graphite-like tungsten disulfide nano slices.
Background technology
Transient metal sulfide, is widely used in the fields such as lubrication, lithium electricity, ultracapacitor and absorption due to the structure of its uniqueness and the performance of excellence.Molybdenumdisulphide and tungsten disulfide, as Typical Representative, receive and pay close attention to widely.They have the laminate structure of similar graphite flake layer, are very strong covalent linkage in layer, and interlayer is then very weak Van der Waals Er Sili, and layer and layer are easy to peel off, and has good anisotropy and lower frictional coefficient.
The method of synthesis of carbon/molybdenum disulfide is a lot, and particularly the emphasis studied especially of the Hydrothermal Synthesis of low temperature, effectively can control the pattern of product.Now for the preparation of nanometer WS
2method mainly contain high-temperature hot reaction, as gas-solid reaction, solid state sintering etc.Prior art adopts high-temperature hot reaction method to prepare WS
2nanotube, nanometer sheet, nano flower etc., Chinese patent discloses one and utilizes solvent-induced effect to prepare WS
2the method of nanometer rod, the method adopts planetary high-energy ball mill, by the WS of common micro level laminate structure
2powder and micron order S powder mixing and ball milling, obtain nanoscale twins form presoma, then in a kettle., adds dispersion agent polyoxyethylene glycol, and control temperature is cooled to room temperature 200 DEG C ~ 260 DEG C insulations after 10 ~ 30 hours, has synthesized WS
2nanometer rod.Patent CN102701283A discloses a kind of preparation method of Wolfram disulfide nano bar, adopts hydrothermal synthesis method to achieve WS
2effective control of pattern.On this basis, the present invention adopts mixed surfactant assisted hydrothermal synthesis method, simplifies processing step, makes WS
2the particle diameter of nano-powder and pattern can control, and have high specific surface area and frictional behaviour.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art and the preparation method providing a kind of graphite-like tungsten disulfide nano slices, the method is with low cost, technique is simple, productive rate is high.
The preparation method of graphite-like tungsten disulfide nano slices, comprises the following steps:
Step 1, tensio-active agent is soluble in water, then add Na
2s, NH
2oHHCl and Na
2wO
4, stir, regulator solution pH value to 6 ~ 8;
Step 2, moves into reactor by step 1 gained solution, and sealing, after isothermal reaction, is cooled to room temperature, obtains reaction product;
Step 3, is separated step 2 gained reaction product, and washing, drying, obtain graphite-like tungsten disulfide nano slices.
Further, Na in step 1
2s, NH
2oHHCl and Na
2wO
4mol ratio be 0.5 ~ 1.5:2.5 ~ 3.5:1.5 ~ 2.5, preferably 1.0 ~ 1.5:3.0 ~ 3.5:1.0 ~ 2.5, further preferably 1:3:2.
Further, tensio-active agent and Na in step 1
2wO
4mol ratio be 1:4 ~ 8, preferred 1:5 ~ 8, further preferably 1:5.
Further, tensio-active agent described in step 1 is the mixture of in cetyl trimethylammonium bromide, Pulan Buddhist nun gram F-127, Sodium dodecylbenzene sulfonate or polyoxyethylene glycol two kinds.Wherein the mol ratio of two kinds of components is 1:1 ~ 6, preferred 1:2.
Further, in step 2, constant temperature is 160 DEG C ~ 280 DEG C.
Further, in step 2, the isothermal reaction time is 24 ~ 96h, preferred 48h.
Preparation method of the present invention adopts surfactant-assisted hydrothermal synthesis graphite-like tungsten disulfide nano slices, achieves the reduction of tungsten disulfide in aqueous.Adding of mixed surfactant, be conducive to the control of product morphology.
Preparation method's cost of the present invention is inexpensive, and production technique is simple and easy to control, and efficiency of pcr product is high, is applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the graphite-like tungsten disulfide nano slices of embodiment 1;
Fig. 2 is the SEM figure of the graphite-like tungsten disulfide nano slices of embodiment 1.
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment 1
By molten for 0.18gCTAB and the 0.10gF-127 distilled water with 70mL, then add 1.20gNa
2s, 0.725gNH
2oHHCl and 1.56gNa
2wO
4, after dissolving completely, then about the HCl adjust ph to 6 using 2mol/L.After stirring 40min, mixed solution is transferred in the stainless steel cauldron of 100mL, is placed in vacuum drying oven in 180 DEG C of insulation 48h, is cooled to room temperature.Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and the powder product that finally 60 DEG C of dry 10h obtain grey black is under vacuum graphite-like tungsten disulfide nano slices.
The XRD figure spectrum of Fig. 1 illustrates that XRD peak position is consistent with standard diffraction figure (JCPDS84-1398), and product is pure WS
2hexagonal, Fig. 2 (a, b) is the SEM photo of product, obviously can sees product to be homogeneous thickness be the WS of about 20nm
2nanometer sheet, soilless sticking phenomenon.
Embodiment 2
0.18gCTAB and 0.30gF-127 is dissolved in the distilled water of 70mL, then adds 1.20gNa
2s, 0.725gNH
2oHHCl and 1.56gNa
2wO
4, after dissolving completely, then about the HCl adjust ph to 7 using 2mol/L.After stirring 40min, mixed solution is transferred in the stainless steel cauldron of 100mL, is placed in vacuum drying oven in 200 DEG C of insulation 72h, is cooled to room temperature.Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and the powder product that finally 60 DEG C of dry 10h obtain grey black is under vacuum graphite-like tungsten disulfide nano slices.
The WS of products therefrom to be homogeneous thickness be about 20nm
2nanometer sheet, and soilless sticking phenomenon.
Embodiment 3
0.18gCTAB and 0.17gSDBS is dissolved in the distilled water of 70mL, then adds 1.20gNa
2s, 0.725gNH
2oHHCl and 1.56gNa
2wO
4.After dissolving completely, then about regulating pH value to 6 with the HCl of 2mol/L.After stirring 40min, mixed solution is transferred in the stainless steel cauldron of 100mL, is placed in vacuum drying oven in 240 DEG C of insulation 72h, is cooled to room temperature.Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and the powder product that finally 80 DEG C of dry 12h obtain grey black is under vacuum graphite-like tungsten disulfide nano slices.
The WS of products therefrom to be homogeneous thickness be about 20nm
2nanometer sheet, and soilless sticking phenomenon.
Productive rate and the tribological property parametric results of embodiment 1 to 3 gained graphite-like tungsten disulfide nano slices are as follows:
Claims (6)
1. the preparation method of graphite-like tungsten disulfide nano slices, is characterized in that: comprise the following steps:
Step 1, tensio-active agent is soluble in water, then add Na
2s, NH
2oHHCl and Na
2wO
4, stir, regulator solution pH value to 6 ~ 8;
Step 2, moves into reactor by step 1 gained solution, and sealing, after isothermal reaction, is cooled to room temperature, obtains reaction product;
Step 3, is separated step 2 gained reaction product, and washing, drying, obtain graphite-like tungsten disulfide nano slices.
2. the preparation method of graphite-like tungsten disulfide nano slices according to claim 1, is characterized in that: Na in step 1
2s, NH
2oHHCl and Na
2wO
4mol ratio be 0.5 ~ 1.5:2.5 ~ 3.5:1.5 ~ 2.5.
3. the preparation method of graphite-like tungsten disulfide nano slices according to claim 1, is characterized in that: tensio-active agent and Na in step 1
2wO
4mol ratio be 1:4 ~ 8.
4. the preparation method of graphite-like tungsten disulfide nano slices according to claim 1, is characterized in that: tensio-active agent described in step 1 is the mixture of in cetyl trimethylammonium bromide, Pulan Buddhist nun gram F-127, Sodium dodecylbenzene sulfonate or polyoxyethylene glycol two kinds.
5. the preparation method of graphite-like tungsten disulfide nano slices according to claim 1, is characterized in that: in step 2, constant temperature is 160 DEG C ~ 280 DEG C.
6. the preparation method of graphite-like tungsten disulfide nano slices according to claim 1, is characterized in that: in step 2, the isothermal reaction time is 24 ~ 96h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510975198.XA CN105417582A (en) | 2015-12-22 | 2015-12-22 | Method for preparing graphite-like tungsten disulfide nano-sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510975198.XA CN105417582A (en) | 2015-12-22 | 2015-12-22 | Method for preparing graphite-like tungsten disulfide nano-sheet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105417582A true CN105417582A (en) | 2016-03-23 |
Family
ID=55496204
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510975198.XA Pending CN105417582A (en) | 2015-12-22 | 2015-12-22 | Method for preparing graphite-like tungsten disulfide nano-sheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105417582A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107090158A (en) * | 2017-05-09 | 2017-08-25 | 常州德毅新材料科技有限公司 | A kind of wear-resisting polyetheretherketonematerials materials and preparation method thereof |
| CN113023780A (en) * | 2021-03-17 | 2021-06-25 | 李伟强 | Nanoscale tungsten disulfide material, preparation method and preparation device thereof |
| CN113385195A (en) * | 2021-07-23 | 2021-09-14 | 兰州大学 | Preparation and application of tungsten disulfide/indium sulfide heterojunction photocatalytic material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818963A (en) * | 2014-02-21 | 2014-05-28 | 福州大学 | One-step hydrothermal method for synthesizing nanoflake tungsten sulfide |
| CN105140517A (en) * | 2015-09-14 | 2015-12-09 | 天津大学 | Preparation method of non-water-soluble transition metal disulphide nanosheets |
-
2015
- 2015-12-22 CN CN201510975198.XA patent/CN105417582A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818963A (en) * | 2014-02-21 | 2014-05-28 | 福州大学 | One-step hydrothermal method for synthesizing nanoflake tungsten sulfide |
| CN105140517A (en) * | 2015-09-14 | 2015-12-09 | 天津大学 | Preparation method of non-water-soluble transition metal disulphide nanosheets |
Non-Patent Citations (2)
| Title |
|---|
| M. THRIPURANTHAKA等: "Temperature dependent Raman spectroscopy of chemically derived few layer MoS2 and WS2 nanosheets", 《APPLIED PHYSICS LETTERS》 * |
| SHIXIU CAO等: "Hydrothermal synthesis of variety low dimensional WS2 nanostructures", 《MATERIALS LETTERS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107090158A (en) * | 2017-05-09 | 2017-08-25 | 常州德毅新材料科技有限公司 | A kind of wear-resisting polyetheretherketonematerials materials and preparation method thereof |
| CN113023780A (en) * | 2021-03-17 | 2021-06-25 | 李伟强 | Nanoscale tungsten disulfide material, preparation method and preparation device thereof |
| CN113385195A (en) * | 2021-07-23 | 2021-09-14 | 兰州大学 | Preparation and application of tungsten disulfide/indium sulfide heterojunction photocatalytic material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102701281B (en) | A kind of preparation method of flower-shaped molybdenumdisulphide tiny balloon | |
| CN104401948A (en) | Preparation method for single-layer graphite-type carbon nitride nanosheet solution | |
| CN105692573B (en) | A kind of preparation method of nanostructure nitridation carbon | |
| CN105366727B (en) | Preparation method of flower-shaped molybdenum disulfide nano-rods | |
| CN105776154A (en) | Preparation method of tungsten diselenide nanosheet | |
| CN102965105B (en) | Graphene-CuInS2 quantum dot compound and preparation method thereof | |
| CN103641169B (en) | A kind of Bi 2s 3-MoS 2the synthetic method of nano-heterogeneous structure | |
| CN103602362B (en) | Preparation method of ferrous disulfide-graphene composite nano lubricant | |
| CN107954483B (en) | Alpha-phase nickel hydroxide ultrathin nanosheet and preparation method thereof | |
| CN107221448B (en) | A kind of high-performance super capacitor electrode material PANI/CeO2/Ni(OH)2Multistage microballoon and preparation method thereof | |
| CN101927979A (en) | Stannic oxide/ graphene nano composite as well as preparation method and application thereof | |
| CN103086436A (en) | Preparation method of nano-molybdenum disulfide | |
| CN102701283A (en) | Preparation method of tungsten disulfide nanorods | |
| CN103626231B (en) | The preparation method of the carbosphere that a kind of molybdenumdisulphide is coated | |
| CN105417582A (en) | Method for preparing graphite-like tungsten disulfide nano-sheet | |
| CN105502502A (en) | Preparation method of tungsten disulfide nanorod | |
| CN104891485A (en) | Method for preparing nano graphite sheet | |
| CN105314686A (en) | FeS nanosheet preparing method | |
| CN105502370B (en) | A kind of solid-phase reduction process of graphene oxide | |
| CN107814408B (en) | SnS rich in S vacancy2Preparation method of ultrathin nanosheet | |
| CN104291386A (en) | Preparation method of two-dimensional nickel hydroxide ultrathin nano-film | |
| CN106542569A (en) | A kind of preparation method of flower ball-shaped tin ash | |
| CN103408063B (en) | Take Sulfite lignin as the method for tensio-active agent hydro-thermal legal system for nano zine oxide | |
| CN105097300A (en) | Preparation method of NiMoO4/MoS2/NiS nanocomposite | |
| CN102897722A (en) | Alpha-In2Se3 nano-grade flower-ball solvothermal synthesizing method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160323 |