CN105776154A - Preparation method of tungsten diselenide nanosheet - Google Patents
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- CN105776154A CN105776154A CN201610303570.7A CN201610303570A CN105776154A CN 105776154 A CN105776154 A CN 105776154A CN 201610303570 A CN201610303570 A CN 201610303570A CN 105776154 A CN105776154 A CN 105776154A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- C—CHEMISTRY; METALLURGY
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- 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
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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
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
The invention discloses a preparation method of a tungsten diselenide nanosheet, and belongs to the technical field of nanometer material preparation. The preparation method comprises the following steps of dissolving sodium borohydride into an organic solvent, and successively adding selenium powder and sodium tungstate to prepare a mixed solution; transferring the mixed solution to a reaction kettle, and performing reaction for 6 to 48 hours at 200 DEG C to 240 DEG C; after the temperature of the reaction kettle is naturally cooled to the room temperature, collecting black products through suction filtration; washing the product by deionized water and ethyl alcohol; freezing and drying the washed product to obtain the tungsten diselenide nanosheet. The invention provides the method for synthesizing the tungsten diselenide nanosheet in one step by a solvothermal method for the first time. The preparation method has the advantages that the raw materials are green and environment-friendly; the cost is low; the yield is high; the reaction condition is mild; the scale production can be realized. The high-crystallization tungsten diselenide nanosheet prepared by the method has the advantages that the size is great; the layer number is small; the distribution is uniform; the specific surface area is high; high application prospects are realized in the fields of catalysis, energy storage and the like.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to a kind of two tungsten selenide (WSe2) preparation method of nanometer sheet.
Background technology
In recent years, people are in the majority to the research of transient metal sulfide, and achieve very big achievement, main reason is that from current open source literature, and sulfur source is wide and most of toxicity is relatively low, and soluble selenide is all poisonous, therefore to transient metal sulfide MS2The preparation method of (M=Mo, W, Nb, Ta, Zr, Hf, Re, Pt) and the report of performance study thereof are also more, and relate to transition metal selenides MSe2The correlational study of (M=Mo, W, Nb, Ta, Zr, Hf, Re, Pt) is less, especially its morphology control and applied research aspect.Therefore, sight line has been turned to transition metal selenides by a lot of scholars.
Two tungsten selenide (WSe2) as main transition metal selenides, it is a kind of engineering material with multiple property and functional material.Structures shape character, character reflection structure is the basic law of chemistry or even nature.Therefore, the basic research thinking of nano material is also the size by regulating nanostructured.Component and pattern realize the control to performance, finally realize design and the synthesis of functional nano device.WSe2Crystal has similar MoS2Six side's sandwich, each WSe2Molecular layer is one layer of W atomic layer of folder between two-layer Se atomic layer, is connected with covalent bond between W atomic layer with Se atomic layer, and contiguous WSe2Layer all separates with Se layer, and farther out, active force is weak Van der Waals force to spacing.WSe2As main transition metal selenides, high temperature resistant, decomposition temperature reaches 850 DEG C；Acid and alkali-resistance and other media, good stability；Having good greasy property, shear strength is low；Additionally there are other prominent performances: WSe2It is diamagnetism p-type semiconductor material, conduction band low (1.16eV)；WSe2Being the material that thermal conductivity is minimum in the world at present, the heat in expression system is not easily scattered and disappeared, in other words, it is simply that the energy conversion efficiency of system can be higher, therefore this new diseases, will likely the service efficiency increasing substantially the energy.
Two tungsten selenide (WSe2) be with a wide range of applications in high-temperature solid lubrication, high performance solar batteries, novel energy-storing material, High Performance Adiabatic ceramic material and high-performance transistor of future generation etc..Such as: with WSe2Nano wire, as novel magnesium ion cell negative electrode material (B.Liuetal., ACSNano., 2013,7 (9), 8051-8058.), has shown WSe2Good embedding magnesium and de-magging ability；JHuang etc. successfully prepare WSe by CVD2Monocrystalline (JHuangetal., ACSNano, 2014,8 (1), 923-930), has the electric property of excellence.The research worker of Austria Vienna University of Science and Technology develops the diode that two tungsten selenide make first, and according to experiment display, this material is used as ultra-thin soft solaode.The solaode major part of standard is manufactured by silicon wafer, very heavy, and organic material is very fast for the degree of degeneration of photovoltaic applications, and therefore the two-dimensional structure of monoatomic layer has huge crystallization advantage, and its crystal structure more increases stability.
In sum, high-quality WSe is prepared2And composite is significant.But, WSe2Preparation difficulty, preparation technology is loaded down with trivial details, and cost is high, and therefore, its application has been also affected by considerable restraint.
Patent preliminary search shows two applications relating to two tungsten selenide preparation method of nano material: one to be application number be 201010572015.7 Chinese patent disclose a kind of method using solid phase method to prepare two tungsten selenide nanometer sheet; the method is with after the tungsten powder of certain mol proportion and selenium powder mix homogeneously; under argon shield; through pyroreaction, cooling to two tungsten selenide nanometer sheet.The method needs under argon shield, carries out, apparatus expensive, and reaction temperature is high, be 600 DEG C～700 DEG C in tube furnace.Another is application number be 201210374547.9 the Chinese patent preparation method that discloses a kind of high orientation two tungsten selenide nano wire, the method adopts two-step reaction method, first with Na2WO4·2H2O and CH3CSNH2For reactive solute, with CTAB for chelating agent, prepare WO by hydro-thermal method2Nano wire, then again by WO2Nano wire purity be 99.9% selenium powder at high temperature carry out selenizing, it is thus achieved that orientation two tungsten selenide nano wire.The method adopts two-step method, and preparation process is loaded down with trivial details, at WO2Selenidation process is also required to carry out under high-purity argon is protected, and reaction temperature is high, is 600 DEG C～900 DEG C.
Because with graphite, MOS2There is natural minerals difference, WSe2Prepared by the method only by synthetic, solubility selenium salt owing to synthesizing used by two tungsten selenide is poisonous, green synthesis method is single, it is confined to the solid phase synthesis of W-Se, existing technique is generally required for carrying out in CVD tube furnace, apparatus expensive, and preparation temperature is high, reaction atmosphere is required height, is unfavorable for large-scale industrial production.Therefore, WSe2Application be also affected by considerable restraint.
Summary of the invention
The defect that the present invention exists to overcome existing preparation technology, it is provided that a kind of using cheap selenium powder as selenium source, sodium tungstate is as tungsten source, and sodium borohydride is as reducing agent, and organic solvent is reaction dissolvent, by solvent-thermal method one-step synthesis two tungsten selenide (WSe2) nanometer sheet.Preparation method in the present invention is a kind of new highly crystalline two tungsten selenide (WSe2) scale synthesis process of nanometer sheet, there is the advantages such as technique is simple, raw material is easy to get, cost is low, reaction condition is gentle.The two tungsten selenide nanometer sheet that the present invention prepares have crystalline quality height, and yardstick is big, the number of plies is few, specific surface area advantages of higher.
To achieve these goals, technical scheme is as follows:
The preparation method of two tungsten selenide nanometer sheet, it is characterised in that comprise the following steps:
Step 1: be dissolved in organic solvent by sodium borohydride mix homogeneously, adds selenium powder and stirs to being completely dissolved, and adds sodium tungstate and prepares mixed solution；
Step 2: transfer in reactor by the mixed solution of step 1 gained, reacts 6 hours～48 hours when temperature range is 200 DEG C～240 DEG C；
Step 3: after the temperature of reactor naturally cools to room temperature in step 2, by collected by suction black product, and washs product with deionized water and ethanol respectively, and lyophilization obtains two tungsten selenide nanometer sheet after 24 hours.
Preferably, in described step 1, in mixed solution, the concentration of sodium tungstate is 0.0400mol/L～0.0667mol/L.
Preferably, in described step 1, the mol ratio of selenium powder and sodium tungstate is 2～2.3: 1.
Preferably, in described step 1, the mol ratio of sodium borohydride and sodium tungstate is 3: 4～2: 1.
Preferably, in described step 1 organic solvent be DMF, ethanol and dimethylbenzene any one.
In sum, the method have the advantages that
Compared with existing preparation method, the present invention adopts one-step synthesis, the present invention to use cheap selenium powder as selenium source, and sodium tungstate is as tungsten source, and borohydride sodium is as reduction auxiliary agent, by solvent-thermal method one-step synthesis two tungsten selenide (WSe2) nanometer sheet.The method technique is simple, raw material environmental protection, cost is low, reaction condition is gentle.Gained two tungsten selenide (WSe of the present invention2) nanometer sheet has significantly high crystalline quality, its uniform in size distribution and have high specific surface area, the thickness of nanometer sheet is at below 10nm, and can look forward to it has extraordinary application prospect in fields such as catalysis, energy storage and tribology.
Accompanying drawing explanation
Fig. 1 is the Raman spectrogram of embodiment 1 product；
Fig. 2 is X-ray diffraction (XRD) figure of embodiment 2 product；
Fig. 3 is scanning electron microscope (SEM) figure of embodiment 2 product；
Fig. 4 is transmission electron microscope (TEM) figure of embodiment 3 product；
Fig. 5 is high resolution transmission electron microscopy (HR-TEM) figure of embodiment 4 product.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in detail:
Embodiment 1:
Step 1: the sodium borohydride of 0.1513g is dissolved in 50mlN, mix homogeneously in dinethylformamide, the selenium powder adding 0.3632g stirs to being completely dissolved, and adds 0.6597g sodium tungstate and prepares mixed solution；
Step 2: transferred to by the mixed solution of step 1 gained in politef reactor, reacts 48 hours when temperature is 200 DEG C；
Step 3: after the temperature of reactor naturally cools to room temperature in step 2, by collected by suction black product, and washs product with deionized water and ethanol respectively, and lyophilization obtains two tungsten selenide nanometer sheet after 24 hours.
Fig. 1 is the Raman spectrogram that embodiment 1 reactant reacts 48 hours afterproducts when 200 DEG C, as seen from the figure, at 249cm-1Place occurs in that WSe2Obvious raman characteristic peak E1 2g。
Embodiment 2:
Step 1: the sodium borohydride of 0.1135g is dissolved in 50mlN, mix homogeneously in dinethylformamide, the selenium powder adding 0.3395g stirs to being completely dissolved, and adds 0.6597g sodium tungstate and prepares mixed solution；
Step 2: transferred to by the mixed solution of step 1 gained in politef reactor, reacts 36 hours when temperature is 220 DEG C；
Step 3: after the temperature of reactor naturally cools to room temperature in step 2, by collected by suction black product, and washs product with deionized water and ethanol respectively, and lyophilization obtains two tungsten selenide nanometer sheet after 24 hours.
Fig. 2 implements 2 reactants to react X-ray diffraction (XRD) figure of 36 hours afterproducts when 220 DEG C, and product is the good two tungsten selenide nanometer sheet (WSe of crystallization as seen from the figure2), and it is absent from any dephasign.
Fig. 3 is scanning electron microscope (SEM) figure that embodiment 2 reactant reacts 36 hours afterproducts when 220 DEG C, and wherein, product is more than 500nm, the WSe of very thin thickness by yardstick2Nanometer sheet forms.
Embodiment 3:
Step 1: the sodium borohydride of 0.1135g is dissolved in 80mlN, mix homogeneously in dinethylformamide, the selenium powder adding 0.6317g stirs to being completely dissolved, and adds 1.3194g sodium tungstate and prepares mixed solution；
Step 2: transferred to by the mixed solution of step 1 gained in politef reactor, reacts 24 hours when temperature is 240 DEG C；
Step 3: after the temperature of reactor naturally cools to room temperature in step 2, by collected by suction black product, and washs product with deionized water and ethanol respectively, and lyophilization obtains two tungsten selenide nanometer sheet after 24 hours.
Fig. 4 is transmission electron microscope (TEM) figure that embodiment 3 reactant reacts 24 hours afterproducts when 240 DEG C, and as seen from the figure, product is the WSe being similar to Graphene2Nano flake.
Embodiment 4:
Step 1: the sodium borohydride of 0.2270g is dissolved in 60mlN, mix homogeneously in dinethylformamide, the selenium powder adding 0.6475g stirs to being completely dissolved, and adds 1.3194g sodium tungstate and prepares mixed solution；
Step 2: transferred to by the mixed solution of step 1 gained in the reactor of politef, reacts 6 hours when temperature is 240 DEG C；
Step 3: after the temperature of reactor naturally cools to room temperature in step 2, by collected by suction black product, and washs product with deionized water and ethanol respectively, and lyophilization obtains two tungsten selenide nanometer sheet after 24 hours.
Fig. 5 is high resolution scanning electron microscope (HR-TEM) figure that the reactant of embodiment 4 reacts 6 hours afterproducts when 240 DEG C, figure can be clearly seen that WSe2The interlamellar spacing wide for 0.68nm of nanometer sheet, and can be seen that WSe in figure2Nanometer sheet is about 5 layers.
Embodiment 5:
Step 1: the sodium borohydride of 0.1513g is dissolved in mix homogeneously in 50ml ethanol, the selenium powder adding 0.3632g stirs to being completely dissolved, and adds 0.6597g sodium tungstate and prepares mixed solution；
Step 2: transferred to by the mixed solution of step 1 gained in the reactor of politef, reacts 24 hours when temperature is 240 DEG C；
Step 3: after the temperature of reactor naturally cools to room temperature in step 2, by collected by suction black product, and washs product with deionized water and ethanol respectively, and lyophilization obtains two tungsten selenide nanometer sheet after 24 hours.
Embodiment 6:
Step 1: the sodium borohydride of 0.1513g is dissolved in mix homogeneously in 50ml dimethylbenzene, the selenium powder adding 0.3632g stirs to being completely dissolved, and adds 0.6597g sodium tungstate and prepares mixed solution；
Step 2: transferred to by the mixed solution of step 1 gained in the reactor of politef, reacts 48 hours when temperature is 240 DEG C；
Step 3: after the temperature of reactor naturally cools to room temperature in step 2, by collected by suction black product, and washs product with deionized water and ethanol respectively, and lyophilization obtains two tungsten selenide nanometer sheet after 24 hours.
Above-described embodiment is illustrative principles of the invention and effect thereof only, not for the restriction present invention.Above-described embodiment all under the spirit and category of the present invention, can be modified or change by any those skilled in the art.Therefore, art has usually intellectual such as modifying without departing from all equivalences completed under disclosed spirit and technological thought or change, must be contained by the claim of the present invention.
Claims (5)
1. the preparation method of two tungsten selenide nanometer sheet, it is characterised in that comprise the following steps:
Step 1: be dissolved in organic solvent by sodium borohydride mix homogeneously, adds selenium powder and stirs to being completely dissolved, and adds sodium tungstate and prepares mixed solution；
Step 2: transfer in reactor by the mixed solution of step 1 gained, reacts 6～48 hours when temperature range is 200 DEG C～240 DEG C；
Step 3: after the temperature of reactor naturally cools to room temperature in step 2, by collected by suction black product, and washs product with deionized water and ethanol respectively, and lyophilization obtains two tungsten selenide nanometer sheet after 24 hours.
2. the preparation method of two tungsten selenide nanometer sheet according to claim 1, it is characterised in that in described step 1 organic solvent be DMF, ethanol and dimethylbenzene any one.
3. the preparation method of two tungsten selenide nanometer sheet according to claim 1, it is characterised in that in described step 1, in mixed solution, the concentration of sodium tungstate is 0.0400mol/L～0.0667mol/L.
4. the preparation method of two tungsten selenide nanometer sheet according to claim 2, it is characterised in that in described step 1, the mol ratio of selenium powder and sodium tungstate is 2～2.3: 1.
5. the preparation method of two tungsten selenide nanometer sheet according to claim 2, it is characterised in that in described step 1, the mol ratio of sodium borohydride and sodium tungstate is 3: 4～2: 1.
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Cited By (18)
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| CN106379871A (en) * | 2016-10-11 | 2017-02-08 | 电子科技大学 | Method for preparing rhenium diselenide nano-sheet |
| CN106824070A (en) * | 2017-01-22 | 2017-06-13 | 青岛科技大学 | A kind of two tungsten selenide nitrogen-doped graphene photocatalysis sorbing materials and preparation method thereof |
| CN106904580A (en) * | 2017-03-09 | 2017-06-30 | 哈尔滨工业大学 | Using the method for the two-dimensional nano piece of hydro-thermal method synthesis 1T phase degree of disorder coordinated regulations |
| CN107190361A (en) * | 2017-04-19 | 2017-09-22 | 江苏大学 | A kind of tungsten selenide/graphene/carbon nano-fiber composite material and preparation method thereof |
| CN107475694A (en) * | 2017-06-20 | 2017-12-15 | 广东工业大学 | A kind of method and its application that two tungsten selenide semiconductive thin films are prepared on FTO substrates |
| CN107475744A (en) * | 2017-08-10 | 2017-12-15 | 中国石油大学(华东) | A kind of two ferrous selenide nano composite materials and its synthetic method and application |
| CN107601443A (en) * | 2017-11-09 | 2018-01-19 | 安徽大学 | A kind of preparation method of ultra-thin tungsten selenide nanometer sheet |
| CN107999094A (en) * | 2017-12-29 | 2018-05-08 | 郑州大学 | A kind of metal phase tungsten selenide nanometer sheet/carbon nano-tube hybridization structure elctro-catalyst and preparation method thereof |
| CN107999093A (en) * | 2017-12-29 | 2018-05-08 | 郑州大学 | A kind of cobalt doped two dimension tungsten selenide elctro-catalyst and preparation method thereof |
| CN108906084A (en) * | 2018-06-21 | 2018-11-30 | 肇庆市华师大光电产业研究院 | A kind of preparation method and application of two selenizings cobalt nanorod |
| CN109052340A (en) * | 2018-10-10 | 2018-12-21 | 陕西科技大学 | A kind of preparation method of selenium/selenizing vanadium compound phase material |
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| CN111359638A (en) * | 2020-03-31 | 2020-07-03 | 中北大学 | Photocatalytic carbon dioxide reduction catalyst and preparation method and application thereof |
| CN111686779A (en) * | 2020-05-12 | 2020-09-22 | 广东工业大学 | Tungsten selenide/carbon nitride composite nanosheet and preparation method and application thereof |
| CN112573491A (en) * | 2020-12-18 | 2021-03-30 | 电子科技大学 | Coral-like Pd4Method for producing Se compound |
| CN112808228A (en) * | 2020-12-30 | 2021-05-18 | 华北电力大学（保定） | WSe2/halloysite nanotube demercuration adsorbent and preparation method and application thereof |
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| CN106379871A (en) * | 2016-10-11 | 2017-02-08 | 电子科技大学 | Method for preparing rhenium diselenide nano-sheet |
| CN106379871B (en) * | 2016-10-11 | 2018-05-15 | 电子科技大学 | A kind of method for preparing two selenizing rhenium nanometer sheets |
| CN106824070B (en) * | 2017-01-22 | 2019-06-28 | 青岛科技大学 | One kind two tungsten selenides-nitrogen-doped graphene photocatalysis adsorbent material and preparation method thereof |
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| CN106904580B (en) * | 2017-03-09 | 2019-11-15 | 哈尔滨工业大学 | Utilize the method for hydro-thermal method synthesis 1T phase-degree of disorder coordinated regulation two-dimensional nano piece |
| CN107190361A (en) * | 2017-04-19 | 2017-09-22 | 江苏大学 | A kind of tungsten selenide/graphene/carbon nano-fiber composite material and preparation method thereof |
| CN107475694A (en) * | 2017-06-20 | 2017-12-15 | 广东工业大学 | A kind of method and its application that two tungsten selenide semiconductive thin films are prepared on FTO substrates |
| CN107475694B (en) * | 2017-06-20 | 2019-10-18 | 广东工业大学 | A kind of method and its application preparing two tungsten selenide semiconductive thin films on FTO substrate |
| CN107475744A (en) * | 2017-08-10 | 2017-12-15 | 中国石油大学(华东) | A kind of two ferrous selenide nano composite materials and its synthetic method and application |
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