CN106099053A - A kind of molybdenum sulfide/selenizing molybdenum composite material and preparation thereof and application - Google Patents
A kind of molybdenum sulfide/selenizing molybdenum composite material and preparation thereof and application Download PDFInfo
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- CN106099053A CN106099053A CN201610392008.6A CN201610392008A CN106099053A CN 106099053 A CN106099053 A CN 106099053A CN 201610392008 A CN201610392008 A CN 201610392008A CN 106099053 A CN106099053 A CN 106099053A
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- Prior art keywords
- molybdenum
- selenizing
- composite material
- molybdenum sulfide
- sulfide
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- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 122
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 239000011733 molybdenum Substances 0.000 title claims abstract description 121
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 32
- 239000006185 dispersion Substances 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 11
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 7
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052961 molybdenite Inorganic materials 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- VBNIGYNNILMQRE-UHFFFAOYSA-N O.NN.[Se] Chemical compound O.NN.[Se] VBNIGYNNILMQRE-UHFFFAOYSA-N 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052711 selenium Inorganic materials 0.000 claims description 3
- 239000011669 selenium Substances 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims description 2
- 230000001186 cumulative effect Effects 0.000 claims description 2
- 229940113088 dimethylacetamide Drugs 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 41
- 239000002356 single layer Substances 0.000 abstract description 28
- 238000000034 method Methods 0.000 abstract description 9
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 241000446313 Lamella Species 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 7
- 229910052723 transition metal Inorganic materials 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 6
- 235000015393 sodium molybdate Nutrition 0.000 description 6
- 239000011684 sodium molybdate Substances 0.000 description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 6
- 150000003624 transition metals Chemical class 0.000 description 6
- 230000001629 suppression Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 101000911390 Homo sapiens Coagulation factor VIII Proteins 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 102000057593 human F8 Human genes 0.000 description 2
- -1 molybdenum sulfide Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229940047431 recombinate Drugs 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical compound CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001786 chalcogen compounds Chemical class 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- MODMKKOKHKJFHJ-UHFFFAOYSA-N magnesium;dioxido(dioxo)molybdenum Chemical compound [Mg+2].[O-][Mo]([O-])(=O)=O MODMKKOKHKJFHJ-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical class O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- B01J35/33—
-
- B01J35/396—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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
- Y02E60/10—Energy storage using batteries
-
- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention relates to a kind of molybdenum sulfide/selenizing molybdenum composite material and preparation thereof and application, molybdenum sulfide/selenizing molybdenum composite material is that molybdenum sulfide nanometer sheet surface in situ grows selenizing molybdenum nanometer sheet；Wherein selenizing molybdenum nanometer sheet with curling sheet form vertical-growth on molybdenum sulfide nanoscale twins.Preparation: prepare monolayer or few layer molybdenum sulfide nanometer sheet by ultrasonic wave added stripping method, then by solvent-thermal method few layer selenizing molybdenum nanometer sheet of growth in situ on monolayer or few layer molybdenum sulfide nanometer sheet.Application: be widely used in liberation of hydrogen catalyst, lithium ion battery and ultracapacitor equal energy source field.The present invention is designed by simple preparation technology, the few layer selenizing molybdenum nanoscale twins of growth on the monolayer or few layer molybdenum sulfide nanoscale twins of ultrasonic stripping, it is thus achieved that have the heterojunction structure of multi-stage porous, improve the performances such as its conduction, catalysis.
Description
Technical field
The invention belongs to composite and preparation thereof and application, particularly to a kind of molybdenum sulfide/selenizing molybdenum composite wood
Expect and prepare and application.
Background technology
Recently as the dilute development waiting two-dimension nano materials of graphite and application, there is the transition metal of typical layered structure
Chalcogen compound (such as molybdenum sulfide, selenizing molybdenum etc.), due to its uniqueness the be stripped into two dimension dilute structure of class graphite characteristic with
And they are in catalyst, energy storage and the outstanding representation of field of electronic devices, cause the extensive concern of people.Stratiform transition
Metal sulfide can use molecular formula MX2Representing, M represents transition metal (typically Mo, W etc.), and X represents the unit of VI race
Element (S, Se, Te etc.), the typical lamellar compound being made up of the M-X-M of sandwich structure, between layers with Van der Waals force
Combining, therefore block materials is easy to be stripped into monolayer or the ultrathin nanometer sheet of few layer.Although stratiform transition metal two sulfur
Compound structurally has similarity, but they show different electronic properties, and stratiform transition metal two sulfur of body phase
Nature difference between compound and the transition metal dichalcogenide of monolayer is the biggest, such as molybdenum sulfide nanometer sheet and molybdenum sulfide block phase
Ratio, is changed into direct band-gap semicondictor by indirect band-gap semiconductor, and it is special that this change makes it that electricity, magnetic, light etc. can produce some
Different reaction.
In the research process to new material, people regulate the character of existing material the most as required, expand
Corresponding range of application and the performance of optimization material.
Summary of the invention
The technical problem to be solved is to provide a kind of molybdenum sulfide/selenizing molybdenum composite material and preparation thereof and answers
Prepare monolayer or few layer molybdenum sulfide nanometer sheet by, the present invention by ultrasonic wave added stripping method, then by solvent-thermal method at monolayer or
The few layer selenizing molybdenum nanometer sheet of growth in situ in few layer molybdenum sulfide nanometer sheet.The present invention makes full use of material molybdenum sulfide interlayer Van der Waals
Power is more weak, is easily peeled into monolayer or the feature of few layer nanometer sheet, successfully prepares stable chemical nature, monolayer that specific surface area is big
Or lack layer molybdenum sulfide nanometer sheet；Molybdenum sulfide prepared by the present invention-selenizing molybdenum composite material has the feature of morphology controllable, with stripping
Monolayer or the few layer molybdenum sulfide nanometer sheet prepared from method are substrate, in the few layer selenizing molybdenum nanometer sheet of its superficial growth, effectively suppress
The reunion of selenizing molybdenum nanometer sheet self and stacking, and the electronics regulating composite by constructing semiconductor heterostructure ties
Structure and then improve its electric conductivity, catalytic performance etc.；Molybdenum sulfide prepared by the present invention-selenizing molybdenum composite material is expected to as one
Plant promising high performance electrode material, have extensively in liberation of hydrogen catalyst, lithium ion battery and ultracapacitor equal energy source field
Application.
A kind of molybdenum sulfide/selenizing the molybdenum composite material of the present invention, described molybdenum sulfide/selenizing molybdenum composite material is that molybdenum sulfide is received
Rice sheet surface in situ growth selenizing molybdenum nanometer sheet；Wherein selenizing molybdenum nanometer sheet with curling sheet form vertical-growth at molybdenum sulfide
On nanoscale twins.
A kind of preparation method of the molybdenum sulfide/selenizing molybdenum composite material of the present invention, including:
(1) molybdenite is disperseed in organic solvent, ultrasonic, obtain blackish green dispersion liquid, centrifugal going is precipitated, then by upper
Layer clear liquid is diluted, and obtains the dispersion liquid of molybdenum sulfide nanometer sheet；
(2) selenium powder is added in hydrazine hydrate, stirring, obtain selenium-hydrazine hydrate dispersion liquid；Molybdate is dissolved in minor amount of water, super
Sound fully dissolves, and obtains molybdate dispersion liquid；
(3) by the dispersion liquid of above-mentioned molybdenum sulfide nanometer sheet, selenium-hydrazine hydrate dispersion liquid, the mixing of molybdate dispersion liquid, carry out molten
Agent thermal response, reaction temperature is 160-220 DEG C, and the response time is 10-24h, the black precipitate sucking filtration obtained, washing, is dried,
To molybdenum sulfide/selenizing molybdenum composite material.
In described step (1), organic solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or N-methylpyrrole
Alkanone；Preferably N,N-dimethylformamide.
Molybdenite dispersion concentration in organic solvent is 1-50mg/mL, preferably 5-20mg/mL.
In described step (1), ultrasonic time is 2-48h, preferably 6-24h.
In described step (1) centrifugal go in precipitation being centrifuged and be: centrifugal speed is 1000-3000rpm, preferably 1500-
2000rpm；Centrifugation time is 2-20min, preferably 5-10min.
Described step (1) is diluted to organic solvent and is diluted, and the volume of taken supernatant is 1-6mL, preferably 1-5mL；
Extension rate is 0-10 times, preferably 2-6 times；The cumulative volume of dilution after cure molybdenum dispersion liquid is 10mL.
Dilution organic solvent is DMF, N,N-dimethylacetamide or N-Methyl pyrrolidone, excellent
Select N,N-dimethylformamide.
In described step (2), the concentration of selenium-hydrazine hydrate dispersion liquid is 0.5-6mg/mL, preferably 1-4mg/mL, hydrazine hydrate
Volume is 10-30mL.
In step (2), sodium molybdate only need to be completely dissolved by the consumption of aqueous solvent.
In described step (2), molybdate is ammonium molybdate, sodium molybdate, magnesium molybdate and zinc molybdate etc..
Sodium molybdate is 1:2 with the mol ratio of selenium powder.
In described step (3), solvent thermal reaction is: carry out in a kettle., preferably: reaction temperature is 180-200 DEG C, instead
It is 12-18h between Ying Shi.
In step (3), washing is for using organic solvent, ethanol and the repeated multiple times washing of deionized water.
Described step (3) is dried and is: lyophilization 12-48h, preferably 24-30h or 60 DEG C of vacuum drying 2-12h, preferably
4-8h。
The application of a kind of molybdenum sulfide/selenizing molybdenum composite material of the present invention, molybdenum sulfide/selenizing molybdenum composite material is urged at liberation of hydrogen
Application in agent, lithium ion battery and ultracapacitor.
The present invention peels off molybdenum sulfide Ore by ultrasonic wave added and obtains monolayer or few layer molybdenum sulfide lamella；By selenium powder and molybdic acid
Salt is prepared by a step solvent-thermal method few layer selenizing molybdenum nanometer sheet of growth in situ on monolayer or few layer molybdenum sulfide lamella.
The present invention is designed by simple preparation technology, raw on the monolayer or few layer molybdenum sulfide nanoscale twins of ultrasonic stripping
Long few layer selenizing molybdenum nanoscale twins, it is thus achieved that there is the heterojunction structure of multi-stage porous, improve the performances such as its conduction, catalysis.This molybdenum sulfide-
Selenizing molybdenum composite material has the advantage that (1) has the monolayer of unique two-dimensional layered structure or layer molybdenum sulfide nanometer sheet can less
Think that selenizing molybdenum provides more growth site, the reunion of suppression selenizing molybdenum nanometer sheet and stacking, enable selenizing molybdenum nanometer sheet
Expose more activity site, edge；Lack layer selenizing molybdenum nanometer sheet vertical-growth can also be effective on molybdenum sulfide lamella simultaneously
Again the stacking of suppression molybdenum sulfide nanoscale twins；(2) in molybdenum sulfide-selenizing molybdenum composite material, by two kinds of level-density parameter of coupling
Semi-conducting material, molybdenum sulfide and selenizing molybdenum intersection can form semiconductor heterostructure, it is possible to effectively realize separation of charge
Suppress electron-hole to recombinate, thus improve its electric conductivity and catalytic performance.(3) molybdenum sulfide-selenizing molybdenum composite material can carry
For bigger specific surface area, the beneficially entrance of electrolyte, the transmission energy of electrode material surface proton and electronics can be obviously improved
Power, embodies more excellent chemical property.Therefore, molybdenum sulfide is effectively combined with selenizing molybdenum, can realize the best
Synergism, prepare the molybdenum sulfide-selenizing molybdenum composite material of electrochemical performance.
Preparation work electrode tests molybdenum sulfide-selenizing molybdenum composite material polarization in acid condition prepared by the present invention
Curve, concrete preparation method is as follows:
Molybdenum sulfide-selenizing molybdenum composite material prepared by this experiment of 3.0mg is dispersed in 175 μ L dehydrated alcohol and 47 μ L
In Nafion solution, ultrasonic obtaining uniform dispersion liquid, (glass-carbon electrode is successively in glassy carbon electrode surface to take 2.2 μ L dispersant liquid drops
Polished, cleaning obtains clean glass-carbon electrode), obtain molybdenum sulfide-selenizing molybdenum composite material electrode after natural drying.
Using molybdenum sulfide-selenizing molybdenum composite material electrode as working electrode, saturated calomel electrode is as reference electrode, graphite
Rod, as to electrode, chooses the 0.5mol/L H that nitrogen is saturated2SO4Solution is electrolyte, with the scanning speed p-wire of 2mV/s
Property voltammetric scan curve, result is as shown in Figure 1.
Transmission electron microscope (TEM), X-ray diffraction (XRD) and electrochemical workstation is used to characterize the present invention made
The structure and morphology of the molybdenum sulfide-selenizing molybdenum composite material obtained and electrochemistry, its result is as follows:
(1) TEM test result shows: prepared molybdenum sulfide-selenizing molybdenum composite material has the multilevel hierarchy of uniqueness,
Edge it can be seen that few layer or the molybdenum sulfide nanoscale twins of monolayer, selenizing molybdenum nanometer sheet with the sheet form vertical-growth of curling at list
On layer or few layer molybdenum sulfide nanoscale twins.In molybdenum sulfide-selenizing molybdenum composite material, there is the monolayer of unique layer structure or few
Layer molybdenum sulfide lamella is that selenizing molybdenum provides and more grows site, makes selenizing molybdenum nanometer sheet be uniformly coated on monolayer or few layer
On molybdenum sulfide lamella, the reunion of suppression selenizing molybdenum self, so that the selenizing molybdenum nanometer sheet edge with catalysis activity is filled
The exposure divided.
(2) XRD test result shows, the molybdenum sulfide of stripping in 2 θ=14.4,32.7,39.5,49.8,58.3 and 60.2o
Diffraction maximum correspond respectively to (002) of hexagonal crystal system molybdenum sulfide, (100), (103), (105), (110) and (008) crystal face, by force
Diffraction maximum show that the crystallinity of monolayer or few layer molybdenum sulfide is fine.Selenizing molybdenum in 2 θ=13.4, the diffraction at 32.9 and 56.7 °
Peak corresponds respectively to (002) of hexagonal structure 2H phase selenizing molybdenum, (100) and (110) crystal face.Prepared molybdenum sulfide-selenizing molybdenum
Composite shows molybdenum sulfide and the characteristic peak of selenizing molybdenum, illustrates that selenizing molybdenum nanometer sheet is the most successfully carried on molybdenum sulfide lamella
On；But (002) crystal face of molybdenum sulfide nanometer sheet substantially weakens, show that selenizing molybdenum nanometer sheet inhibits the heap again of molybdenum sulfide lamella
Folded.
(3) Electrochemical results shows, the molybdenum sulfide of stripping electric current density under η=355mV just can reach 10mA/
cm2, this is likely due to the monolayer peeled off or the catalysis activity that layer molybdenum sulfide lamella self is poor less.Selenizing molybdenum need to η=
Under 261mV, electric current density can reach 10mA/cm2, this is likely due to selenizing molybdenum nanometer sheet and is self-assembled into nano flower-like structure, cruelly
Reveal less hydrogen evolution activity site.Molybdenum sulfide-selenizing molybdenum composite material shows substantially excellent catalytic activity for hydrogen evolution, η=
Under 201mV, electric current density can reach 10mA/cm2, it is evenly coated at monolayer or few layer sulfuration molybdenum sheet owing to selenizing molybdenum nanometer sheet
On layer, the reunion of suppression selenizing molybdenum self, thus expose more activity site, edge.In addition the molybdenum sulfide that the present invention constructs-
Selenizing molybdenum composite material can regulate the electronic structure of both quasiconductors, thus improves its electric conductivity and catalysis activity.
Beneficial effect
(1) preparation process of the present invention is simple, it is easy to operation, is a kind of preparation method the most efficiently；
(2) experimental design is ingenious.
First, this experiment prepares monolayer or few layer molybdenum sulfide nanometer sheet by the method that ultrasonic wave added is peeled off, as life
Long substrate, the growth that class Graphene layer structure is selenizing molybdenum nanometer sheet of its uniqueness provides and more grows site, makes selenium
Change molybdenum nanometer sheet to be uniformly coated in monolayer or few layer molybdenum sulfide nanometer sheet, the reunion of suppression selenizing molybdenum self, so that tool
The edge having the selenizing molybdenum nanometer sheet of catalysis activity is sufficiently exposed, and can significantly improve the electro-chemical activity of material.
Second, achieved the hydridization of two kinds of Transition-metal dichalcogenides by simple solvent thermal process, the sulfur of structure
Change molybdenum-selenizing molybdenum composite material, it is provided that the entrance of bigger specific surface area, beneficially electrolyte, hence it is evident that improve electrode material
Material surface plasmon and the transmittability of electronics, show more excellent chemical property.
3rd, in molybdenum sulfide-selenizing molybdenum composite material, by coupling the semi-conducting material of two kinds of level-density parameter, at sulfur
Change molybdenum and selenizing molybdenum intersection and construct semiconductor heterostructure, it is possible to effectively realize separation of charge to suppress electron-hole to recombinate,
Thus improve its electric conductivity and catalytic performance.
Therefore, selenizing molybdenum is effectively combined with molybdenum sulfide, the best synergism can be realized so that both
Advantage fully combined and played, thus prepare the molybdenum sulfide-selenizing molybdenum composite material of electrochemical performance.
(3) molybdenum sulfide prepared by the present invention-selenizing molybdenum composite material is expected to as a kind of promising high-performance electrode
Material, is widely used in liberation of hydrogen catalyst, lithium ion battery, ultracapacitor equal energy source field.
Accompanying drawing explanation
Fig. 1 is the SEM figure of molybdenum sulfide in embodiment 1-selenizing molybdenum composite material；
Fig. 2 is the TEM figure of molybdenum sulfide in embodiment 1-selenizing molybdenum composite material；Wherein a is low amplification；B is that height is put
Big multiple；
Fig. 3 is the XRD figure of molybdenum sulfide in the present invention-selenizing molybdenum composite material；
Fig. 4 is the linear voltammetric scan curve of molybdenum sulfide in embodiment 1-selenizing molybdenum composite material；
Fig. 5 is the linear voltammetric scan curve of the molybdenum sulfide-selenizing molybdenum composite material of different compositions in the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
(1) 1g molybdenite is joined in 100mL DMF, lower continuous ultrasound in supersonic cleaning machine
12h, obtains cyan dispersion liquid；
(2) taking the monolayer obtained in (1) or few layer molybdenum sulfide nanometer sheet dispersion liquid is centrifuged, centrifugal speed is
1500rpm, centrifugation time is 8min, removes precipitate；
(3) take 2.5mL monolayer or few layer molybdenum sulfide nanometer sheet dispersion liquid 7.5mL N,N-dimethylformamide carries out dilute
Release, standby；
(4) 25mg selenium powder is dissolved in 10mL hydrazine hydrate, stirring at normal temperature 2h, is allowed to dispersed；
(5) being dissolved in minor amount of water by 38.3mg sodium molybdate, ultrasonic being allowed to fully is dissolved；
(6) being transferred in hydrothermal synthesis reaction still by the dispersion liquid of preparation in (3) (4) (5), at 180 DEG C, solvent thermal is anti-
Answer 12h；
(7) the black precipitate sucking filtration that will prepare, and the most with DMF, ethanol and deionized water
Secondary cleaning, is then dried in freeze dryer, i.e. can get molybdenum sulfide-selenizing molybdenum composite material, and named molybdenum sulfide-selenizing molybdenum-
2.Embodiment 2
(1) 1g molybdenite is joined in 100mL DMF, lower continuous ultrasound in supersonic cleaning machine
12h, obtains cyan dispersion liquid；
(2) taking the monolayer obtained in (1) or few layer molybdenum sulfide nanometer sheet dispersion liquid is centrifuged, centrifugal speed is
1500rpm, centrifugation time is 8min, removes precipitate；
(3) take 1.25mL monolayer or few layer molybdenum sulfide nanometer sheet dispersion liquid 8.75mL N,N-dimethylformamide is carried out
Dilution, standby；
(4) 25mg selenium powder is dissolved in 10mL hydrazine hydrate, stirring at normal temperature 2h, is allowed to dispersed；
(5) being dissolved in minor amount of water by 38.3mg sodium molybdate, ultrasonic being allowed to fully is dissolved；
(6) being transferred in hydrothermal synthesis reaction still by the dispersion liquid of preparation in (3) (4) (5), at 180 DEG C, solvent thermal is anti-
Answer 12h；
(7) the black precipitate sucking filtration that will prepare, and the most with DMF, ethanol and deionized water
Secondary cleaning, is then dried in freeze dryer, i.e. can get molybdenum sulfide-selenizing molybdenum composite material, and named molybdenum sulfide-selenizing molybdenum-
1。
Embodiment 3
(1) 1g molybdenite is joined in 100mL DMF, lower continuous ultrasound in supersonic cleaning machine
12h, obtains cyan dispersion liquid；
(2) taking the monolayer obtained in (1) or few layer molybdenum sulfide nanometer sheet dispersion liquid is centrifuged, centrifugal speed is
1500rpm, centrifugation time is 8min, removes precipitate；
(3) take 5mL monolayer or few layer molybdenum sulfide nanometer sheet dispersion liquid 5mL DMF is diluted, standby
With；
(4) 25mg selenium powder is dissolved in 10mL hydrazine hydrate, stirring at normal temperature 2h, is allowed to dispersed；
(5) being dissolved in minor amount of water by 38.3mg sodium molybdate, ultrasonic being allowed to fully is dissolved；
(6) being transferred in hydrothermal synthesis reaction still by the dispersion liquid of preparation in (3) (4) (5), at 180 DEG C, solvent thermal is anti-
Answer 12h；
(7) the black precipitate sucking filtration that will prepare, and the most with DMF, ethanol and deionized water
Secondary cleaning, is then dried in freeze dryer, i.e. can get molybdenum sulfide-selenizing molybdenum composite material, and named molybdenum sulfide-selenizing molybdenum-
3。
Claims (10)
1. molybdenum sulfide/selenizing molybdenum composite material, it is characterised in that: described molybdenum sulfide/selenizing molybdenum composite material is molybdenum sulfide
Nanometer sheet surface in situ growth selenizing molybdenum nanometer sheet；Wherein selenizing molybdenum nanometer sheet is vulcanizing with the sheet form vertical-growth of curling
On molybdenum nanoscale twins.
2. a preparation method for molybdenum sulfide as claimed in claim 1/selenizing molybdenum composite material, including:
(1) being disperseed in organic solvent by molybdenite, ultrasonic, centrifugal going is precipitated, and then the supernatant is diluted, obtains sulfur
Change the dispersion liquid of molybdenum nanometer sheet；
(2) selenium powder is added in hydrazine hydrate, stirring, obtain selenium-hydrazine hydrate dispersion liquid；Molybdate is soluble in water, ultrasonic, obtains molybdenum
Hydrochlorate dispersion liquid；
(3) by the dispersion liquid of above-mentioned molybdenum sulfide nanometer sheet, selenium-hydrazine hydrate dispersion liquid, the mixing of molybdate dispersion liquid, solvent thermal is carried out
Reaction, reaction temperature is 160-220 DEG C, and the response time is 10-24h, then sucking filtration, washing, is dried, obtains molybdenum sulfide/selenizing
Molybdenum composite material.
The preparation method of a kind of molybdenum sulfide/selenizing molybdenum composite material the most according to claim 2, it is characterised in that: described
In step (1), organic solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or N-Methyl pyrrolidone；Molybdenite divides
Dissipating concentration in organic solvent is 1-50mg/mL.
The preparation method of a kind of molybdenum sulfide/selenizing molybdenum composite material the most according to claim 2, it is characterised in that: described
In step (1), ultrasonic time is 2-48h.
The preparation method of a kind of molybdenum sulfide/selenizing molybdenum composite material the most according to claim 2, it is characterised in that: step
(1) supernatant is diluted being diluted for organic solvent, and the volume of taken supernatant is 1-6mL, and extension rate is 0-10
Times, the cumulative volume of dilution after cure molybdenum dispersion liquid is 10mL.
The preparation method of a kind of molybdenum sulfide/selenizing molybdenum composite material the most according to claim 2, it is characterised in that: described
In step (2), the concentration of selenium-hydrazine hydrate dispersion liquid is 0.5-6mg/mL, and the volume of hydrazine hydrate is 10-30mL.
The preparation method of a kind of molybdenum sulfide/selenizing molybdenum composite material the most according to claim 2, it is characterised in that: described
In step (2), molybdate is 1:2 with the mol ratio of selenium powder.
The preparation method of a kind of molybdenum sulfide/selenizing molybdenum composite material the most according to claim 2, it is characterised in that: described
In step (3), solvent thermal reaction is: carry out in a kettle., and reaction temperature is 180-200 DEG C, and the response time is 12-18h.
The preparation method of a kind of molybdenum sulfide/selenizing molybdenum composite material the most according to claim 2, it is characterised in that: described
Step (3) is dried and is: lyophilization 12-48h or 60 DEG C of vacuum drying 2-12h.
10. the application of molybdenum sulfide as claimed in claim 1/selenizing molybdenum composite material, it is characterised in that: molybdenum sulfide/selenium
Change molybdenum composite material application in liberation of hydrogen catalyst, lithium ion battery and ultracapacitor.
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