CN105600824A - High-performance micro-nano multilevel-structure MoS2 material and preparation method and application thereof - Google Patents
High-performance micro-nano multilevel-structure MoS2 material and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 40
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 20
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title abstract description 8
- 239000002077 nanosphere Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 57
- 239000000243 solution Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 9
- 239000011733 molybdenum Substances 0.000 claims description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 229910001416 lithium ion Inorganic materials 0.000 claims description 8
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000000314 lubricant Substances 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000005864 Sulphur Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000000975 dye Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 238000001338 self-assembly Methods 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 2
- -1 polyethylene Polymers 0.000 claims 2
- 229920000573 polyethylene Polymers 0.000 claims 2
- 239000013049 sediment Substances 0.000 claims 2
- 238000005259 measurement Methods 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000004094 surface-active agent Substances 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000004005 microsphere Substances 0.000 abstract 4
- 230000007613 environmental effect Effects 0.000 abstract 2
- 239000002135 nanosheet Substances 0.000 abstract 2
- 230000000694 effects Effects 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000002736 nonionic surfactant Substances 0.000 abstract 1
- 229920000151 polyglycol Polymers 0.000 abstract 1
- 239000010695 polyglycol Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 14
- 239000000047 product Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 230000004087 circulation Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 5
- 229920006324 polyoxymethylene Polymers 0.000 description 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 239000000088 plastic resin Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 3
- 235000018660 ammonium molybdate Nutrition 0.000 description 3
- 239000011609 ammonium molybdate Substances 0.000 description 3
- 229940010552 ammonium molybdate Drugs 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000018199 S phase Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 235000015393 sodium molybdate Nutrition 0.000 description 2
- 239000011684 sodium molybdate Substances 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/22—Compounds containing sulfur, selenium or tellurium
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
-
- 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
-
- 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
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- 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
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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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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
- C10M2201/066—Molybdenum sulfide
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/1003—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds used as base material
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- 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
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- 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
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Abstract
The invention relates to the technical field of nano material preparation and energy environmental protection, in particular to high-performance micro-nano multilevel-structure MoS2 material and a preparation method thereof. The preparation method is characterized in that nonionic surfactant polyglycol is introduced to allow MoS2 super-thin nano sheets generated by reaction to self-assemble into nano-sphere units, the nano-sphere units further assemble to form microspheres with a micro-nano multilevel structure, the microspheres are 2-10 micrometers in diameter, the nano-spheres are 50-200 nanometers in diameter, the nano sheets are 100-300 nanometers in length, 100-300 nanometers in width and 2-50 nanometers in thickness, the nano-sphere units interweave to form the microspheres, and the specific surface area of the microspheres is 10-100m<2>/g. The MoS2 material can bring the advantages of high activity and high efficiency of nano units into play. The preparation method completed in one step under a hydrothermal condition is simple in process, low in energy consumption and cost, short in preparation cycle, environmental friendly, beneficial to engineering large-scale preparation and application, and the like.
Description
Technical field
The invention belongs to nano material preparation technique and application field, relate in particular to a kind of high-performance micro-nano multilevel hierarchy MoS2The preparation method of powder.
Background technology
Two dimension transient metal sulfide there is class graphene-structured, its unique electronics, optical characteristics make its lithium ion battery,Hydrogen is produced in ultracapacitor, optical, electrical catalysis, and the fields such as catalytic hydrogenation have great application prospect, and is the focus of studying at present.Therefore, preparation research preparation has high performance MoS2Powder has important research justice.
Micro-nano multilevel hierarchy is by the higher-dimension complexity that has particular geometric pattern assembling by low-dimensional nano unit body materialStructure, this class formation had both retained the high-performance of nano particle, had again the advantages such as the easily separated processing of large scale particle, andThere is higher specific area, abundant pore passage structure, the coupling effect that it has and cooperative effect contribute to guest molecule (gasBody/dyestuff/organic molecule) in the absorption of material surface and the transmission of material internal, be people's design construction sensitive material, urgeWhen formed material, absorbing and storing material, energy conversion material, consider more structural model.
The molybdenum bisuphide material of report mostly is ultrathin nanometer sheet at present, or assembles taking ultrathin nanometer sheet as basic structural unitMoS2Nanosphere. And about MoS2Microballoon, the preparation research especially with multilevel hierarchical structure microballoon there is not yetReport. And develop a kind of simple and easy effective, with low cost, environmentally friendly and can synthesize on a large scale application synthetic method not onlyCan effectively expand MoS2Material is in the application of every field, also for other high performance dimensions of Design and manufacture are received multilevel hierarchyMaterial provides important evidence and technical support.
Summary of the invention
The object of the present invention is to provide a kind of high-performance micro-nano multilevel hierarchy MoS2The preparation method of powder, and by its applicationOn absorption, air-sensitive, catalysis, the field such as lubricated. The method preparation process is simple, and cost is low, and productive rate is high, without rear placeReason, environmentally safe, is easy to industrialization.
Micro-nano multilevel hierarchy MoS of the present invention2Powder is made up of the microballoon that is of a size of 2～10 μ m, microballoon by 50～The nanosphere unit of the 200nm formation that interweaves, and the ultrathin nanometer self assembly that nanosphere is 2～50nm by thickness forms. ItsIn, micro-nano multilevel hierarchy MoS2Microballoon, the nanosphere of composition microballoon is all that even dispersion distributes.
The invention still further relates to a kind of micro-nano multilevel hierarchy MoS2The preparation method of powder, employing be the hot method of hydrothermal/solvent, bagContain following steps:
1) at ambient temperature, a certain amount of molybdenum salt is slowly joined in solvent, be stirred to dissolving, then add certainThe sulphur source of amount stirs and obtains mixed solution A;
2) continuing to add a certain amount of polyethylene glycol in the A system stirring, after stirring and dissolving, obtain mixed solution B;
3) mixed solution B is positioned in Vltrasonic device and carries out ultrasonic processing, ultrasonic end is transferred in reactor and is carried out insteadShould;
4) reaction finishes rear centrifugation and collects step 3) in black precipitate, with the alternately washing of deionized water and ethanolRear being dried, obtains the MoS of micro-nano multilevel hierarchy2Powder;
The mol ratio in described Yu Liu source, molybdenum source is 1:7～1:50, wherein, the molar concentration of described molybdenum source solution is 0.01～0.5mol/L; The molar concentration in described sulphur source is 0.07mol/L～25mol/L.
Described solvent is deionized water, ethylene glycol, the mixed solvent of DMF or three's composition.
The molecular weight of described polyethylene glycol is 400～6000, and the mol ratio in polyethylene glycol and molybdenum source is 0.05～2.
Described mixed solution carried out ultrasonic dispersion treatment before adding reactor, and ultrasonic frequency is 60W～500W, superThe sound time is 5min～60min.
Another object of the present invention is by micro-nano multilevel hierarchy MoS2Powder application is in Dye Adsorption field.
Another object of the present invention is by micro-nano multilevel hierarchy MoS2Powder application is in lithium ion battery negative material and electro-catalysisDecompose aquatic products hydrogen field.
A further object of the present invention is by micro-nano multilevel hierarchy MoS2Powder application is in field of lubricant.
Micro-nano multilevel hierarchy MoS prepared by the present invention2Powder, with existing MoS2Scalping structure is compared beneficial effectBe:
Micro-nano multilevel hierarchy MoS prepared by the present invention2Powder dispersity is good, microspherulite diameter is even, and circularity is good, Gao BibiaoThe feature of area, good dispersion and easily separated recovery. Microballoon has secondary grading structure, gives the duct knot that it enriches moreStructure and microscopic appearance, can expose more surface-active site, can significantly improve the suction to dyestuff for adsorbing domainAttached efficiency, shortens adsorption time, has a good application prospect.
Brief description of the drawings
Fig. 1 is embodiment 1 micro-nano multilevel hierarchy MoS2The X ray diffracting spectrum of powder.
Fig. 2 is embodiment 1 micro-nano multilevel hierarchy MoS2The stereoscan photograph of powder.
Fig. 3 is embodiment 2 micro-nano multilevel hierarchy MoS2The X ray diffracting spectrum of powder.
Fig. 4 is embodiment 3 micro-nano multilevel hierarchy MoS2The BET test result of powder.
Detailed description of the invention
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment and only be not used in for the present invention is describedLimit the scope of the invention, after having read the present invention, those skilled in the art repair the various equivalent form of values of the present inventionChange and all fall within the application's claims limited range.
Embodiment 1
1) deionized water for stirring that the ammonium molybdate of 1.236g is dissolved in to 35ml, to dissolving, obtains clear solution;
2) thiocarbamide of 2.284g is added and in above-mentioned solution, stir 10min and obtain mixed solution to dissolving, then add 3g'sPEG6000 stirs 1h;
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasonic 30min under 100w power;
4) by 3) in the solution that obtains transfer in the hydrothermal reaction kettle of 50ml, at 180 DEG C, heat 24h, cooling after reaction,Gained black precipitate is carried out to centrifugation, respectively washed three times respectively products therefrom process with distilled water and absolute ethyl alcohol50 DEG C dry, obtains micro-nano multilevel hierarchy MoS2Powder.
The micro-nano multilevel hierarchy MoS of above-mentioned preparation2The X ray diffracting spectrum of powder as shown in Figure 1, its diffraction maximum and sixThe standard diagram of side's phase molybdenum bisuphide is consistent, illustrates that products therefrom is pure MoS2. The MoS of above-mentioned preparation2Sweeping of powderRetouch electromicroscopic photograph (seeing Fig. 2), as can be seen from the figure MoS2Powder is the microballoon of size uniform, the average grain diameter of microballoonBe about 5 μ m, dispersiveness, the uniformity of particle are better. Microballoon is interweaved and is formed by nanosphere, and nanosphere is by ultrathin nanometerSheet self assembly forms, and nanosphere surface has abundant pleated structure. MoS2The specific area of microballoon is 35m2/g。
The micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder carries out absorption property test: by the MoS of 5mg2Powder joins20ml concentration is in the methylene blue solution of 20mg/L, and in 1min, the degradation rate of methylene blue reaches 99%.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application, on lithium ion battery negative, shows charge and discharge firstCapacity is 960 and 581mAhg-1, after 50 circulations, charge and discharge capacity is respectively 520 and 318mAhg-1。
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application produces hydrogen field, the initial overpotential of evolving hydrogen reaction in electro-catalysisFor 160mV, in the time that overpotential is 280mv, cathode-current density is 45mA/cm2, Tafel slope is 87mV/dec.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application is in field of lubricant, by the MoS of 5wt%2Join heatIn plastic resin polyformaldehyde, the coefficient of friction of material is 0.13.
Embodiment 2
1) ammonium molybdate of 2.56g is dissolved in the ethylene glycol of 35ml and is stirred to dissolving, obtain clear solution;
2) thiocarbamide of 1.84g is added and in above-mentioned solution, stir 10min and obtain mixed solution to dissolving, then add 1.2g'sPEG6000 stirs 1h;
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasonic 1h under 60w power;
4) by 3) in the solution that obtains transfer in the hydrothermal reaction kettle of 50ml, at 160 DEG C, heat 24h, cooling after reaction,Gained black precipitate is carried out to centrifugation, respectively washed three times respectively products therefrom process with distilled water and absolute ethyl alcohol70 DEG C dry, obtains micro-nano multilevel hierarchy MoS2Powder.
The micro-nano multilevel hierarchy MoS of above-mentioned preparation2The X ray diffracting spectrum of powder as shown in Figure 3, its diffraction maximum and sixThe standard diagram of side's phase molybdenum bisuphide is consistent, illustrates that products therefrom is pure MoS2. The MoS of above-mentioned preparation2Powder microballoonAverage grain diameter be about 7 μ m, the specific area of microballoon is 24m2/g。
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder carries out absorption property test: by the MoS of 20mg2Powder addsIn the methylene blue solution that to enter to 100ml concentration be 50mg/L, in 1min, the degradation rate of methylene blue reaches 94%.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application, on lithium ion battery negative, shows charge and discharge firstCapacity is 870 and 549mAhg-1, after 50 circulations, charge and discharge capacity is respectively 509 and 302mAhg-1。
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application produces hydrogen in electro-catalysis, and the initial overpotential of evolving hydrogen reaction is143mV, in the time that overpotential is 280mv, cathode-current density is 43mA/cm2, Tafel slope is 75mV/dec.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application is in field of lubricant, by the MoS of 2wt%2Join heatIn plastic resin polyformaldehyde, the coefficient of friction of material is 0.15.
Embodiment 3
1) sodium molybdate of 2.5g is dissolved in the DMF of 35ml and is stirred to dissolving, obtain clear solution;
2) thiocarbamide of 5g is added and in above-mentioned solution, stir 10min and obtain mixed solution to dissolving, then add 1.2g'sPEG1500 stirs 1h;
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasonic 15min under 80w power;
4) by 3) in the solution that obtains transfer in the hydrothermal reaction kettle of 50ml, at 200 DEG C, heat 18h, cooling after reaction,Gained black precipitate is carried out to centrifugation, respectively washed three times respectively products therefrom process with distilled water and absolute ethyl alcohol50 DEG C dry, obtains micro-nano multilevel hierarchy MoS2Powder.
The micro-nano multilevel hierarchy MoS of above-mentioned preparation2The average grain diameter of powder microballoon is about 3.5 μ m, MoS2Powder BETTest result as shown in Figure 4, MoS2The specific area of microballoon is 46m2/ g. As can be seen from Figure 4, MoS2 micro-nano is manyThe adsorption-desorption thermoisopleth of level structure is obvious IV type thermoisopleth, and presents H3 type adsorption hysteresis ring, shows preparationThe MoS2 micro-nano multilevel hierarchy obtaining has abundant micropore and the macroporous structure drawn together.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder carries out absorption property test: by the MoS of 10mg2Powder addsIn the rhodamine B solution that to enter to 20ml concentration be 20mg/L, in 3min, the degradation rate of rhodamine reaches 92%.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application, on lithium ion battery negative, shows charge and discharge firstCapacity is 790 and 450mAhg-1, after 50 circulations, charge and discharge capacity is respectively 480 and 287mAhg-1。
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application produces hydrogen in electro-catalysis, and the initial overpotential of evolving hydrogen reaction is178mV, in the time that overpotential is 280mv, cathode-current density is 56mA/cm2, Tafel slope is 68mV/dec.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application is in field of lubricant, by the MoS of 10wt%2JoinIn thermoplastic resin polyformaldehyde, the coefficient of friction of material is 0.10.
Embodiment 4
1) ammonium molybdate of 1g is dissolved in to the water of 35ml and the mixed solvent (V of ethanol compositionWater:VAlcohol=1:1) in be stirred to dissolving,Obtain clear solution;
2) thioacetamide of 3g is added and in above-mentioned solution, stir 30min and obtain mixed solution to dissolving, then add 2g'sPEG1500 stirs 1h;
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasonic 20min under 100w power;
4) by 3) in the solution that obtains transfer in the hydrothermal reaction kettle of 50ml, at 170 DEG C, heat 18h, cooling after reaction,Gained black precipitate is carried out to centrifugation, respectively washed three times respectively products therefrom process with distilled water and absolute ethyl alcohol50 DEG C dry, obtains micro-nano multilevel hierarchy MoS2Powder.
The micro-nano multilevel hierarchy MoS of above-mentioned preparation2The average grain diameter of powder microballoon is about 4 μ m, and BET test result showsMoS2The specific area of microballoon is 57m2/g。
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder carries out absorption property test: by the MoS of 5mg2Powder addsIn the rhodamine B solution that is 20mg/L to 20ml concentration, in 10min, the degradation rate of rhodamine B reaches 97%.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application, on lithium ion battery negative, shows charge and discharge firstCapacity is 890 and 633mAhg-1, after 50 circulations, charge and discharge capacity is respectively 580 and 356mAhg-1。
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application produces hydrogen in electro-catalysis, and the initial overpotential of evolving hydrogen reaction is156mV, in the time that overpotential is 280mv, cathode-current density is 67mA/cm2, Tafel slope is 57mV/dec.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application is in field of lubricant, by the MoS of 8wt%2Join heatIn plastic resin polyformaldehyde, the coefficient of friction of material is 0.09.
Embodiment 5
1) sodium molybdate of 3.05g is dissolved in the DMF of 35ml and is stirred to dissolving, obtain clear solution;
2) thiocarbamide of 5.78g is added and in above-mentioned solution, stir 30min and obtain mixed solution to dissolving, then add 0.5g'sPEG6000 stirs 1h;
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasonic 30min under 80w power;
4) by 3) in the solution that obtains transfer in the hydrothermal reaction kettle of 50ml, at 150 DEG C, heat 20h, cooling after reaction,Gained black precipitate is carried out to centrifugation, respectively washed three times respectively products therefrom process with distilled water and absolute ethyl alcohol80 DEG C dry, obtains micro-nano multilevel hierarchy MoS2Powder.
The micro-nano multilevel hierarchy MoS of above-mentioned preparation2The average grain diameter of powder is about 4 μ m, and BET test result shows MoS2The specific area of microballoon is 35m2/g。
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder carries out absorption property test: by the MoS of 10mg2Powder addsIn the rhodamine B solution that to enter to 50ml concentration be 10mg/L, in 5min, the degradation rate of rhodamine B reaches 92%.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application, on lithium ion battery negative, shows charge and discharge firstCapacity is 920mAhg-1And 643mAhg-1, after 50 circulations, charge and discharge capacity is respectively 640 and 567mAh g-1。
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application produces hydrogen in electro-catalysis, and the initial overpotential of evolving hydrogen reaction is180mV, in the time that overpotential is 280mv, cathode-current density is 57mA/cm2, Tafel slope is 69mV/dec.
By the micro-nano multilevel hierarchy MoS of above-mentioned preparation2Powder application is in field of lubricant, by the MoS of 5wt%2Join heatIn plastic resin polyformaldehyde, the coefficient of friction of material is 0.11.
Claims (10)
1. a high-performance micro-nano multilevel hierarchy MoS2Material, is characterized in that: MoS2There is the microspheroidal that diameter is 2～10 μ mLooks, this microballoon is to be interweaved and to be formed by the nanosphere unit of the homogeneous of taking measurements greatly, microballoon specific area is 10～100m2/ g, groupBecoming the diameter of nanosphere unit of microballoon is 50～200nm, the ultrathin nanometer self assembly that nanosphere is is 2～50nm by thickness andBecome.
2. a high-performance micro-nano multilevel hierarchy MoS as claimed in claim 12The preparation method of material, is characterized in that: by MoSource and S source are dissolved in deionized water, ethylene glycol, and DMF or three are combined in the mixed solvent forming, then molten to thisIn liquid, add a certain amount of surfactant polyethylene, be stirred to after dissolving completely, mixed solution is shifted in hydrothermal device,Carry out hydro-thermal reaction and obtain the sediment of black, will after the centrifugation of sediment 1000r/min～10000r/min rotating speed, adopt successivelyDistilled water and absolute ethyl alcohol hocket washing, vacuum drying 3h～30h at 30 DEG C～100 DEG C again, obtain MoS2Micro-Receive material.
3. high-performance micro-nano multilevel hierarchy MoS according to claim 22Preparation method, it is characterized in that: described molybdenum source withThe mol ratio in sulphur source is 1:7～1:50, and wherein, the molar concentration of described molybdenum source solution is 0.01～0.5mol/L; Described sulphur source is moltenThe molar concentration of liquid is 0.07mol/L～25mol/L.
4. according to high-performance micro-nano multilevel hierarchy MoS claimed in claim 22Preparation method, it is characterized in that: described polyethylene glycolMolecular weight be 400～6000, the mol ratio in described polyethylene glycol and molybdenum source is 0.05～2.
5. high-performance micro-nano multilevel hierarchy MoS according to claim 22Preparation method, it is characterized in that described mixed solutionBefore adding reactor, carry out ultrasonic dispersion treatment, ultrasonic frequency is 60W～500W, and ultrasonic time is 5min～60min.
6. high-performance micro-nano multilevel hierarchy MoS according to claim 22Preparation method, it is characterized in that filling out of hydro-thermal reactionDegree of filling is 25%～45%; Described hydrothermal temperature is 100 DEG C～240 DEG C, the described hydro-thermal reaction time be 1h～60h。
7. a high-performance micro-nano multilevel hierarchy MoS2The application of powder on absorption organic dyestuff.
8. a high-performance micro-nano multilevel hierarchy MoS2The application of powder on lithium ion battery.
9. a high-performance micro-nano multilevel hierarchy MoS2Powder produces the application on hydrogen in optical, electrical catalysis.
10. a high-performance micro-nano multilevel hierarchy MoS2The application of powder on lubricant.
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