CN106629845A - Macro preparation method for ultrathin single-layer metallic vanadium diselenide nanosheet with good electrocatalytic hydrogen-producing performance - Google Patents
Macro preparation method for ultrathin single-layer metallic vanadium diselenide nanosheet with good electrocatalytic hydrogen-producing performance Download PDFInfo
- Publication number
- CN106629845A CN106629845A CN201610813270.3A CN201610813270A CN106629845A CN 106629845 A CN106629845 A CN 106629845A CN 201610813270 A CN201610813270 A CN 201610813270A CN 106629845 A CN106629845 A CN 106629845A
- Authority
- CN
- China
- Prior art keywords
- reaction
- individual layer
- nanometer sheet
- ultra
- thin
- 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
- C01G31/00—Compounds of vanadium
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a macro preparation method for a metallic ultrathin single-layer vanadium diselenide nanosheet by utilizing a solvothermal method. According to the invention, by controlling a reaction temperature, a reaction solvent and a reaction selenium source, a vanadium diselenide nanocrystal without a impurity peak in corresponding XRD is obtained; and by controlling the reaction time to control the morphology of a vanadium selenide nanosheet, a homogeneous single-layer nanosheet is obtained, and two layers and three layers grow from an ultrathin singly layer. The preparation method provided by the invention has the advantages of simple process, easiness in operation, no need of special equipment in the whole process of a reaction, and facilitation synthetic production of the vanadium selenide nanosheet through a one-step process. The ultrathin single-layer metallic vanadium diselenide nanosheet with good electrocatalytic hydrogen-producing performance finally obtained by using the method provided by the invention has the following advantages: the electric resistance reaches 2 omega; and the hydrogen evolution potential can reach 204 mV when the electric current density is 10 mA/cm2. The material prepared by using the method provided by the invention is an electrocatalytic hydrogen-producing material with extensive commercial application prospects.
Description
Technical field
The present invention relates to a kind of individual layer, it is ultra-thin, with metallic nano material, specifically two selenizing vanadium ultrathin nanometer piece
Magnanimity preparation method.
Background technology
In recent years, Graphene is used as a kind of most strong Performances of Novel Nano-Porous of the most thin, maximum intensity, electrical and thermal conductivity performance having now been found that
Rice material, causes the fanaticism of the two-dimension nano materials such as material bound pair Graphene, class Graphene research.Graphene its excellent lead
The electron mobility of its superelevation is electrically come from, its excellent mechanical property comes from what carbon atom regularly arranged in its lattice was formed
SP2Hydridization.Two dimensional crystal generally shows electricity, optics and the magnetic property of uniqueness, and itself has unique structural advantage,
This has guided direction to explore novel electro-catalytic agent and energy storage material.Due to two-dimentional Transition-metal dichalcogenide uniqueness
Physics, chemical property, explore the more excellent ultrathin nanometer material such as MoS of new performance2, MoSe2, WS2, VS2Deng and
Become the focus of investigation of materials.VSe2It is typical transition metal sulfur family material, the VSe of individual layer2It is former by metal vanadium atom and selenium
Son interacts according to Van der Waals force according to the Se V Se figure layers that sandwich structure is formed and constitutes.Selenizing vanadium bulk material has
Excellent mechanics, magnetics and electric property, can be used as magnetoelectronic devices, super capacitor material etc..And this patent is visited first
Rope its electro-catalysis H2-producing capacity, the selenizing vanadium individual layer nanometer sheet prepared by the present invention has relatively low hydrogen-evolution overpotential, higher
Current density, relatively low resistance, resistance reaches 2 Ω, is 10mA/cm in current density2When hydrogen-evolution overpotential can reach 204mV.Its
Excellent electrocatalysis characteristic is expected to substitute the metal platinum of costliness and carries out electro-catalysis product hydrogen.
The content of the invention
It is an object of the invention to provide the magnanimity preparation method of a kind of individual layer, ultrathin nanometer piece.The method explores difference
Impact of the condition to nanocrystal XRD and pattern, such as change reaction temperature, reaction dissolvent, reaction raw materials and reaction time.
Go out by controlling the reaction time to control the growth of nanometer sheet, made lamellar structure from individual layer, small size to multilayer, large-sized
Growth.The method determines the reaction condition of the homogeneous selenizing vanadium nanometer chip architecture of good crystallinity, individual layer, pattern, and product
The excellent electro-catalysis H2-producing capacity having.
The magnanimity preparation method of individual layer, ultra-thin selenizing vanadium nanometer sheet, it is characterised in that by vanadyl acetylacetonate, selenium powder and oil
Amine aqueous solution mixes, and is warmed up to uniform temperature again after uniform temperature is vacuumized after mixing and reacts certain hour.Control differential responses
Time, single-layer sheet can be obtained to multilayer tablet.It is an advantage of the current invention that reaction is carried out in there-necked flask, one-step method adds institute
There is raw material to be reacted.The change of reaction condition is easily operated, and it is easy to control to react safety.
Specific embodiment
Weigh a certain amount of vanadyl acetylacetonate during operation first, then weigh a certain amount of selenium powder, and it is molten to be added to oleyl amine
Stir in agent.Vacuumize at a certain temperature, logical nitrogen it is repeated multiple times, to exclude solution in moisture, oxygen and its
His volatile impurity.Again the solution being well mixed is warming up into 230-330oC reacts, and intensification and course of reaction will lead to nitrogen
Gas.Reaction temperature is 330oBefore C, reactant does not all react complete, and the content of impurity is gradually decreased with the rising of temperature,
Until 330oReact completely during C and generate two pure selenizing vanadium nanocrystals.330oDuring C, regulate and control reaction time 0min-1.5h,
In reaction time 1.5h, good crystallinity, ultra-thin, individual layer VSe are obtained2Nanometer sheet.Collect VSe2The method of nanometer sheet is：Will
Reacted mixed solution is transferred to centrifuge tube and adds ethanol centrifugation, and a certain proportion of hexamethylene is added in the precipitated product for obtaining
Alkane and ethanol continue to wash several times, finally 60 in vacuum drying chamberoIt is dried under C.
Description of the drawings：
Fig. 1:The VSe synthesized at a temperature of differential responses2The XRD of nanocrystal；
Fig. 2：The VSe synthesized at a temperature of differential responses2The XRD of nanocrystal；
Fig. 3：330oC reacts the VSe of 1.5h2The XRD of nanometer sheet（Figure a）、TEM（Figure b）, individual layer, ultra-thin small pieces；
Fig. 4：30oC reacts 1.5 hours VSe for preparing2The linear sweep voltammetry characteristic curve (figure a) of ultrathin nanometer piece, impedance spectrum
Figure (figure b), stable circulation linearity curve（Figure c）, resistance reaches 2 Ω, and when current density is 10mA/cm2, hydrogen-evolution overpotential can reach
204mV。
Embodiment 1
During operation, 9mmol vanadyl acetylacetonates are weighed, 18mnol selenium powders, 40ml oleyl amines solvent is added to together three mouthfuls of 100ml
It is stirred in flask.Then heat to 140oC, vacuumizes 10min, logical nitrogen 5min repeatedly for three times.330 are warming up to againoC, instead
Answer and stop after 1.5h reaction to be cooled to room temperature.Product is transferred in four 50ml centrifuge tubes, 25ml ethanol is separately added into,
5min is centrifuged under 5000rpm, precipitated product uses 1:2（V：V）Hexamethylene：Ethanol is washed twice, then 60 in vacuum drying chamberoC
Lower drying, finally obtains good crystallinity, individual layer, ultra-thin selenizing vanadium nanometer sheet（Such as Fig. 3）.
Claims (7)
1. individual layer, the magnanimity preparation method of ultra-thin selenizing vanadium nanometer sheet, it is characterised in that by vanadyl acetylacetonate, selenium powder and oleyl amine
Solution mixes, and is warmed up to uniform temperature again after uniform temperature is vacuumized after mixing and reacts certain hour；During control differential responses
Between, single-layer sheet can be obtained to multilayer tablet；It is an advantage of the current invention that reaction is carried out in there-necked flask, one-step method adds all
Raw material is reacted；The change of reaction condition is easily operated, and it is easy to control to react safety；It is an object of the invention to provide a kind of
The magnanimity preparation method of individual layer, ultrathin nanometer piece；The method explores impact of the different condition to nanocrystal XRD and pattern,
Such as change reaction temperature, reaction dissolvent, reaction raw materials and reaction time；Draw by controlling the reaction time to control nanometer
The growth of piece, makes lamellar structure be urged to multilayer, large-sized growth, and the good electric that product has from individual layer, small size
Change H2-producing capacity.
2. individual layer according to claim 1, the magnanimity preparation method of ultra-thin selenizing vanadium nanometer sheet, it is characterised in that reaction temperature
Degree needs to reach 330oC, reaction raw materials could react complete.
3. individual layer according to claim 1, the magnanimity preparation method of ultra-thin selenizing vanadium nanometer sheet, it is characterised in that during reaction
Between react after 1h and carry out completely, and individual layer, ultra-thin, uniform nanometer sheet are obtained when 1.5h.
4. individual layer according to claim 1, the magnanimity preparation method of ultra-thin selenizing vanadium nanometer sheet, it is characterised in that reaction is molten
Agent（Including octadecylamine, tetradecy lamine, oleic acid, oleyl amine）Reaction is had a great impact；Due to the stronger reproducibility of oleyl amine, reaction is former
Material could react completely.
5. individual layer according to claim 1, the magnanimity preparation method of ultra-thin selenizing vanadium nanometer sheet, it is characterised in that with anti-
Increase between seasonable, nanometer sheet is grown into from individual layer to multilayer.
6. individual layer according to claim 1, the magnanimity preparation method of ultra-thin selenizing vanadium nanometer sheet, it is characterised in that carry first
Go out the scheme of nanometer sheet gram quantity level preparation.
7. individual layer according to claim 1, the magnanimity preparation method of ultra-thin selenizing vanadium nanometer sheet, it is characterised in that selenizing vanadium
Nanometer sheet need to be with ethanol and hexamethylene organic solvent washing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610813270.3A CN106629845A (en) | 2016-09-10 | 2016-09-10 | Macro preparation method for ultrathin single-layer metallic vanadium diselenide nanosheet with good electrocatalytic hydrogen-producing performance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610813270.3A CN106629845A (en) | 2016-09-10 | 2016-09-10 | Macro preparation method for ultrathin single-layer metallic vanadium diselenide nanosheet with good electrocatalytic hydrogen-producing performance |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106629845A true CN106629845A (en) | 2017-05-10 |
Family
ID=58852083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610813270.3A Pending CN106629845A (en) | 2016-09-10 | 2016-09-10 | Macro preparation method for ultrathin single-layer metallic vanadium diselenide nanosheet with good electrocatalytic hydrogen-producing performance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106629845A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279584A (en) * | 2018-10-10 | 2019-01-29 | 陕西科技大学 | A kind of self assembly VSe2The synthetic method of nanometer sheet |
| CN109295475A (en) * | 2018-10-10 | 2019-02-01 | 陕西科技大学 | A kind of preparation method of selenium doping selenizing vanadium composite material |
| CN111514909A (en) * | 2020-03-27 | 2020-08-11 | 电子科技大学 | Two-dimensional material VSe with different defect degrees2Preparation method of (1) |
| CN114314528A (en) * | 2021-12-20 | 2022-04-12 | 深圳大学 | Two-dimensional layered nanosheet and preparation method and application thereof |
| CN114890391A (en) * | 2022-03-25 | 2022-08-12 | 西北工业大学宁波研究院 | Two-dimensional ultrathin NiTe 2 Nanosheet and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103480856A (en) * | 2013-09-09 | 2014-01-01 | 南京邮电大学 | Method for preparing nanocomposite by using two-dimensional transition metal chalcogenide nanosheets and metal |
| CN103556198A (en) * | 2013-11-07 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Preparation method of vanadium dioxide nano rodlike thin film |
| CN104051733A (en) * | 2014-06-12 | 2014-09-17 | 江苏大学 | Vanadium selenide/carbon-based composite material, preparation method of material, and negative electrode of lithium ion battery |
-
2016
- 2016-09-10 CN CN201610813270.3A patent/CN106629845A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103480856A (en) * | 2013-09-09 | 2014-01-01 | 南京邮电大学 | Method for preparing nanocomposite by using two-dimensional transition metal chalcogenide nanosheets and metal |
| CN103556198A (en) * | 2013-11-07 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Preparation method of vanadium dioxide nano rodlike thin film |
| CN104051733A (en) * | 2014-06-12 | 2014-09-17 | 江苏大学 | Vanadium selenide/carbon-based composite material, preparation method of material, and negative electrode of lithium ion battery |
Non-Patent Citations (1)
| Title |
|---|
| WENWEN ZHAO ET AL.: "Colloidal synthesis of VSe2 single-layer nanosheets as novel electrocatalysts for the hydrogen evolution reaction", 《CHEM. COMMUN.》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279584A (en) * | 2018-10-10 | 2019-01-29 | 陕西科技大学 | A kind of self assembly VSe2The synthetic method of nanometer sheet |
| CN109295475A (en) * | 2018-10-10 | 2019-02-01 | 陕西科技大学 | A kind of preparation method of selenium doping selenizing vanadium composite material |
| CN109295475B (en) * | 2018-10-10 | 2020-01-21 | 陕西科技大学 | Preparation method of selenium-doped vanadium selenide composite material |
| CN111514909A (en) * | 2020-03-27 | 2020-08-11 | 电子科技大学 | Two-dimensional material VSe with different defect degrees2Preparation method of (1) |
| CN114314528A (en) * | 2021-12-20 | 2022-04-12 | 深圳大学 | Two-dimensional layered nanosheet and preparation method and application thereof |
| CN114890391A (en) * | 2022-03-25 | 2022-08-12 | 西北工业大学宁波研究院 | Two-dimensional ultrathin NiTe 2 Nanosheet and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106629845A (en) | Macro preparation method for ultrathin single-layer metallic vanadium diselenide nanosheet with good electrocatalytic hydrogen-producing performance | |
| Wang et al. | MoS2/graphene composites as promising materials for energy storage and conversion applications | |
| JP6550378B2 (en) | Method of manufacturing titanium oxide based supercapacitor electrode material | |
| CN107399729A (en) | A kind of bimetallic MOFs nitrogenous graphitized carbon material | |
| Zheng et al. | A new carbon allotrope: graphdiyne | |
| CN108264037B (en) | Three-dimensional porous nitrogen-doped graphene answers the preparation method of material and nitrogen-doped graphene | |
| Lei et al. | A facile solvothermal method to produce graphene-ZnS composites for superior photoelectric applications | |
| Huang et al. | Hollow nanospheres comprising amorphous NiMoS4 and crystalline NiS2 for all-solid-state supercapacitors | |
| CN104174422A (en) | High nitrogen doped graphene and fullerene-like molybdenum selenide hollow-ball nanocomposite and preparation method thereof | |
| Wang et al. | Carbon paper electrode modified by goethite nanowhiskers promotes bacterial extracellular electron transfer | |
| Yu et al. | Construction of SnS2@ MoS2@ rGO heterojunction anode and their half/full sodium ion storage performances | |
| CN105967155B (en) | The preparation method of two tungsten selenide nano flowers | |
| CN110336012A (en) | A kind of chalcogenide composite material and preparation method and application that carbon is compound | |
| CN106531986B (en) | A kind of titanium nitride/silicon nitride/carbonitride/graphene composite nano material and preparation method thereof | |
| Jin et al. | Synthesis of porous In2O3/carbon composites derived from metal-organic frameworks for high performance Li-ion batteries | |
| CN107359341A (en) | A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper | |
| Wang et al. | Fabrication of N-doped carbon coated spinel copper cobalt sulfide hollow spheres to realize the improvement of electrochemical performance for supercapacitors | |
| Albu-Yaron et al. | Nanotubes from two-dimensional materials in contemporary energy research: historical and perspective outlook | |
| Chang et al. | Three-dimensional FeSe 2 microflowers assembled by nanosheets: synthesis, optical properties, and catalytic activity for the hydrogen evolution reaction | |
| CN103632856A (en) | Production method and application of cobaltous oxide/carbon nanostructure array | |
| CN108963237B (en) | Preparation method of sodium ion battery negative electrode material | |
| CN110078130A (en) | A kind of preparation method of hollow structure Fe-base compound and its application as super capacitor anode material | |
| CN109473634A (en) | Solid phase heat together synthesizes two selenizing molybdenums/N doping carbon-point method | |
| Zhang et al. | FeS under wrinkled thin-layer carbon derived from ionic liquid as a high-performance sodium-ion battery anode material | |
| CN110357160B (en) | Network amorphous molybdenum oxide nano material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170510 |
|
| WD01 | Invention patent application deemed withdrawn after publication |