CN105688944A - Method for preparing layered MoS2-SnO2 nano composite material - Google Patents
Method for preparing layered MoS2-SnO2 nano composite material Download PDFInfo
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- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000000463 material Substances 0.000 title claims abstract description 49
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 52
- 238000003756 stirring Methods 0.000 claims abstract description 47
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 42
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011812 mixed powder Substances 0.000 claims abstract description 30
- 238000009830 intercalation Methods 0.000 claims abstract description 29
- 230000002687 intercalation Effects 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 22
- -1 aromatic thioether Chemical class 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 239000007800 oxidant agent Substances 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 33
- 238000002360 preparation method Methods 0.000 claims description 29
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 23
- 229910052750 molybdenum Inorganic materials 0.000 claims description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 239000011733 molybdenum Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000002360 explosive Substances 0.000 claims description 17
- 230000001476 alcoholic effect Effects 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 11
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical group OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims description 11
- 150000004984 aromatic diamines Chemical class 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
- 150000003568 thioethers Chemical class 0.000 claims description 8
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 5
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 2
- 238000005422 blasting Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 15
- 239000002356 single layer Substances 0.000 abstract description 11
- 239000002086 nanomaterial Substances 0.000 abstract description 8
- 239000000047 product Substances 0.000 abstract description 8
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 241000446313 Lamella Species 0.000 abstract description 3
- 239000011229 interlayer Substances 0.000 abstract description 3
- 238000009903 catalytic hydrogenation reaction Methods 0.000 abstract description 2
- 238000004880 explosion Methods 0.000 abstract 4
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000004299 exfoliation Methods 0.000 abstract 1
- 230000001050 lubricating effect Effects 0.000 abstract 1
- 239000011858 nanopowder Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 24
- 229910052961 molybdenite Inorganic materials 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 13
- 238000001816 cooling Methods 0.000 description 9
- 239000012065 filter cake Substances 0.000 description 9
- 238000011068 loading method Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 239000002057 nanoflower Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- 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
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/12—Oxidising
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- 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
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- 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
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- 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
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- 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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- 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
- 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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Abstract
The invention provides a method for preparing a layered MoS2-SnO2 nano composite material. Molybdenum disulfide powder is added into a layering solution for layering reaction to form a mixed solution; oxidant is added into the mixed solution for oxidation-intercalation reaction, then SnO2 nano powder is added under the stirring condition and continues to be stirred evenly, and intercalation MoS2-SnO2 mixed powder is obtained; the intercalation MoS2-SnO2 mixed powder and an explosion agent are mixed for explosion reaction, an explosion reaction product is taken out after being cooled to room temperature, and the layered MoS2-SnO2 nano composite material is obtained. The sulphophile characteristic of aromatic thioether is used, interlayer van der Waals' force of molybdenum disulfide raw material powder is reduced, and intercalation exfoliation is conducted on the molybdenum disulfide raw material powder in cooperation with explosion impact. The product prepared through the method is the layered molybdenum disulfide and SnO2 nano-particle composite nano material with high carrier mobility, SnO2 nano-particles are evenly attached to a single-layer molybdenum sulfide lamella, catalytic hydrogenation and lubricating performance of the single-layer molybdenum sulfide lamella are improved, and the application range of molybdenum sulfide is greatly enlarged.
Description
Technical field
The invention belongs to metal molybdenum technical field, relate to molybdenum bisuphide composite, be specifically related to a kind of stratiform MoS2-SnO2The preparation method of nano composite material。
Background technology
The class Graphene molybdenum bisuphide (Graphene-likeMoS being made up of monolayer or few layer molybdenum bisuphide2) it is a kind of New Two Dimensional (2D) lamellar compound with similar graphene-structured and performance, emerging study hotspot is become in recent years with the physics of its uniqueness, chemical property。The two dimensional crystal material with " sandwich " layer structure that class Graphene molybdenum bisuphide is made up of the single or multiple lift molybdenum bisuphide of hexagonal crystal system, monolayer molybdenum bisuphide is made up of three layers atomic layer, middle one layer is molybdenum atom layer, upper and lower two-layer is sulphur atom layer, molybdenum atom layer forms class " sandwich " structure folded by two-layer sulphur atom layer, and molybdenum atom is combined formation two-dimensional atomic crystal with sulphur atom with covalent bond；Multilamellar molybdenum bisuphide is made up of some monolayer molybdenum bisuphide, is usually no more than five layers, and interlayer exists weak Van der Waals force, and interlamellar spacing is about 0.65nm。
It is widely used in various fields such as lubricant, catalysis, energy storage, composites with " sandwich " layer structure of its uniqueness as the two-dimensional layer nano material that a class is important, monolayer or few layer molybdenum bisuphide。Compared to zero band gap of Graphene, there is regulatable band gap in class Graphene molybdenum bisuphide, has brighter prospect at field of photoelectric devices；Said three-dimensional body phase structure compared to silicon materials, class Graphene molybdenum bisuphide has the two-dimensional layered structure of nanoscale, can be used to manufacture quasiconductor or specification is less, efficiency is higher electronic chip, will be used widely in fields such as follow-on nano-electric devices。
Molybdenum bisuphide is due to its higher theoretical capacity, it is believed that is the succedaneum of lithium ion battery negative material of future generation, was studied by vast researcher in the last few years。But the structure of molybdenum sulfide nanometer anode material can be produced very big destruction by the volumetric stress owing to bringing in lithium ion charge and discharge process, thus bringing the rapid reduction of battery capacity。Therefore, the key solving the problems referred to above by preparing the nano material with certain structural stability to become。
SnO2As one extremely successfully n-type wide bandgap semiconductor (Eg=3.8eV), there is injection cost low, the features such as toxicity is low, and chemical stability is good, always at gas sensing, ion battery and having a wide range of applications on feds。So, if by layer structure MoS2And SnO2Carry out compound, form MoS2-SnO2Heterojunction nanometer material, then in this system, the MoS of layer structure2As P type low-gap semiconductor (Eg=1.8eV), MoS2And SnO2Forming p-n heterojunction at composite contact place, thus inhibiting electron-hole rate of load condensate, increasing specific surface area and increasing effective field launch point, this is to MoS2Performance in photocatalysis and Flied emission etc. has bigger lifting, thus becoming the heterojunction composite of a kind of great potential。
Publication No. is that the Chinese invention patent of CN201410086264A discloses the use of solvent thermal and combines the method for calcining and be prepared for the nano heterojunction of titanium dioxide or tin dioxide nanometer tube and the molybdenum disulfide nano sheet being used as lithium ion battery negative material。
The Chinese invention patent that publication No. is CN201410542132A discloses three-dimensional MoS2-SnO2Heterogeneous semiconductor nano material and preparation method thereof, synthesizes MoS first with hydrothermal synthesis method2Nano flower crystal, with this MoS2Nano flower is as base material, with hydrothermal synthesis method at MoS2Nano flake grows SnO equably2Nanometer rods, obtains three-dimensional MoS2-SnO2Heterogeneous semiconductor nano material。
Although adopting said method to prepare MoS2-SnO2Composite nano materials, but it adopts hydro-thermal method to prepare MoS2, flow process is complicated, and energy consumption is big, is not suitable for industrialized production, and for adopting MoS2Powder is prepared laminar composite as raw material and is not proposed effective workaround, and for the MoS of rich in mineral resources2Material, rationalizes it, higher value application is the trend of at present development。Therefore, explore one and adopt MoS2Powder prepares stratiform MoS as raw material2-SnO2The simple and easy method of nano composite material is very necessary。
Summary of the invention
Based on problems of the prior art, the present invention proposes a kind of stratiform MoS2-SnO2The preparation method of nano composite material, it is thus achieved that there is the stratiform MoS of nanoscale, superior performance2-SnO2Nano composite material, solves existing MoS2-SnO2Composite preparation flow is complicated, and energy consumption is big, is not suitable for industrialized production, and makes photocatalysis and the poor technical problem of greasy property for graininess。
It should be noted that the stratiform MoS in the application2-SnO2MoS in nano composite material2It is monolayer or few layer MoS2Nano material, described few layer refers to 2 layers to 5 layers。
In order to solve above-mentioned technical problem, the application adopts the following technical scheme that and is achieved:
A kind of stratiform MoS2-SnO2The preparation method of nano composite material, the method comprises the following steps:
Step one, adds molybdenum disulfide powder and carries out layering reaction in layering solution, form mixed liquor；
Step 2, adds oxidant in mixed solution and carries out oxidation intercalation, then add SnO under stirring2Nanometer powder, obtains intercalation MoS after continuing to stir2-SnO2Mixed-powder；
Step 3, by intercalation MoS2-SnO2Mixed-powder mixes with burster, carries out explosive reaction, takes out explosive reaction product, namely obtain stratiform MoS after being cooled to room temperature2-SnO2Nano composite material。
The present invention also has and distinguishes technical characteristic as follows:
Described layering solution is the alcoholic solution of aromatic thioether；Described oxidant is potassium permanganate；Described burster is picric acid。
Described aromatic thioether is polyphenylene sulfide or aromatic diamine monomer thioether, and the mass concentration of the alcoholic solution of aromatic thioether is 10%～60%。
In step one, the detailed process of described layering reaction is: molybdenum disulfide powder being ground to 200 orders and sieves, added by molybdenum disulfide powder in the alcoholic solution of aromatic thioether, heating is to 30～50 DEG C and stirs 5～12h, forms mixed liquor。
In step one, the mass ratio of described molybdenum disulfide powder and aromatic thioether is 1:(10～40)。
The detailed process of described step 2 is: add KMnO in mixed solution4Powder, heating in water bath is to 50～90 DEG C and stirs 2～5h, under agitation adds SnO2Nanometer powder, continues stirring 1～3h, filters and dry, obtain intercalation MoS2-SnO2Mixed-powder。
In step 2, the molybdenum bisuphide in described potassium permanganate and mixed liquor mass ratio be (0.5～3): 1。
In step 2, described SnO2Molybdenum bisuphide in nanometer powder and mixed liquor mass ratio be (0.3～2): 1。
In step 2, described SnO2The preparation process of nanometer powder adopts document Integratedprocessoflarge-scaleandsize-controlledSnO2The hydrothermal preparing process of nanoparticlesbyhydrothermalmethod (Trans.NonferrousMet.Soc.China, 23 (2013) 725-730): ammonia is instilled SnCl4·5H2O solution (SnCl4Concentration is 0.5～2mol/L) in, regulating Ph is 8～10, is placed in reactor by solution, heats 4～24h, cooled and filtered, cleaning, drying, namely obtain SnO at 160～240 DEG C2Nanometer powder。
In step 2, described SnO2The particle diameter of nanometer powder is at 10～20nm。
In step 3, the detailed process of described explosive reaction is: by intercalation MoS2-SnO2Mixed-powder is mixed homogeneously with burster, loads in autoclave, and by autoclave evacuation and pass into argon, heating, to 350～600 DEG C of reactions of blasting, cools to taking-up explosive reaction thing after room temperature with the furnace, namely obtains stratiform MoS2-SnO2Nano composite material。
In step 3, described intercalation MoS2-SnO2Mixed-powder and picric mass ratio 1:(0.5～3)。
Compared with prior art, useful has the technical effect that the present invention
(I) present invention utilizes the close sulphur property of aromatic thioether, reduces the interlayer Van der Waals force of molybdenum bisuphide material powder, in conjunction with blast impulse, it is carried out intercalation stripping。The method is adopted to prepare stratiform MoS2-SnO2Nano composite material, simple to operate, it is not necessary to complicated and loaded down with trivial details preparation facilities, not only preparation efficiency is high, and yield is big。
(II) product prepared by the present invention is platelike molybdenumdisulfide and the SnO with high carrier mobility2The nano material of nano-particles reinforcement, and SnO2Nano-particle is uniformly attached on monolayer molybdenum bisuphide lamella, improves its catalytic hydrogenation and greasy property, is greatly expanded the range of application of molybdenum bisuphide。
(III) present invention prepares stratiform MoS2-SnO2Nano composite material, simple to operate, it is not necessary to complicated and loaded down with trivial details preparation facilities, it is suitable for industrialized production。
Accompanying drawing explanation
Fig. 1 is the stratiform MoS in embodiment 12-SnO2The Raman collection of illustrative plates of nano composite material。
Fig. 2 be in embodiment 1 in stratiform MoS2-SnO2The TEM figure of nano composite material。
Fig. 3 is the MoS in comparative example 12-SnO2The Raman collection of illustrative plates of composite。
Fig. 4 is the MoS in comparative example 12-SnO2The TEM figure of composite。
Below in conjunction with drawings and Examples, the particular content of the present invention is described in more detail。
Detailed description of the invention
Defer to technique scheme, specific embodiments of the invention given below, it is necessary to explanation is to the invention is not limited in specific examples below, and all equivalents done on technical scheme basis each fall within protection scope of the present invention。Below in conjunction with embodiment, the present invention is described in further details。
Embodiment 1:
The present embodiment provides a kind of stratiform MoS2-SnO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 10%, in alcoholic solution containing 100g polyphenylene sulfide, heating in water bath is to 30 DEG C and stirs 12h, obtains mixed liquor。
Step 2, adds 5gKMnO in mixed liquor4Powder, heating in water bath is to 50 DEG C and stirs 5h, adds 3gSnO under fast stirring2Nanometer powder, continues stirring 1h, filters and is dried by filter cake, obtains 6.5g intercalation MoS2-SnO2Mixed-powder。
Step 3, takes 3g intercalation MoS2-SnO2Mixed-powder is with 1.5g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 500 DEG C, takes out explosive reaction thing, namely obtain stratiform MoS after cooling to room temperature with the furnace2-SnO2Nano composite material。
Stratiform MoS prepared by the present embodiment2-SnO2Nano composite material Raman collection of illustrative plates is as it is shown in figure 1, high-resolution TEM schemes as shown in Figure 2。
E in Raman collection of illustrative plates in Fig. 12g 1With Ag 1Value respectively 383.78 and 405.21, displacement difference is 21.43, belongs to few Rotating fields MoS2, it was shown that MoS in sample prepared by the present embodiment2For stratified material。
Fig. 2 middle high-resolution TEM figure demonstrates SnO2Granule and stratiform MoS2Nanometer sheet is complex as a whole。
Comprehensive accompanying drawing can show that the sample prepared by the present embodiment is stratiform MoS2-SnO2Nano composite material。
Embodiment 2:
The present embodiment provides a kind of stratiform MoS2-SnO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 20%, in alcoholic solution containing 200g polyphenylene sulfide, heating in water bath is to 40 DEG C and stirs 10h, obtains mixed liquor。
Step 2, adds 10gKMnO in mixed liquor4Powder, heating in water bath is to 60 DEG C and stirs 4.5h, adds 6gSnO under fast stirring2Nanometer powder, continues stirring 1.5h, filters and is dried by filter cake, obtains 8g intercalation MoS2-SnO2Mixed-powder。
Step 3, takes 3g intercalation MoS2-SnO2Mixed-powder is with 3g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 480 DEG C, takes out explosive reaction thing, namely obtain stratiform MoS after cooling to room temperature with the furnace2-SnO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-SnO2The character of nano composite material is substantially the same manner as Example 1。
Embodiment 3:
The present embodiment provides a kind of stratiform MoS2-SnO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 30%, in alcoholic solution containing 300g polyphenylene sulfide, heating in water bath is to 50 DEG C and stirs 8h, obtains mixed liquor。
Step 2, adds 15gKMnO in mixed liquor4Powder, heating in water bath is to 70 DEG C and stirs 4h, adds 9gSnO under fast stirring2Nanometer powder, continues stirring 2h, filters and is dried by filter cake, obtains 12g intercalation MoS2-SnO2Mixed-powder。
Step 3, takes 3g intercalation MoS2-SnO2Mixed-powder is with 4.5g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 450 DEG C, takes out explosive reaction thing, namely obtain stratiform MoS after cooling to room temperature with the furnace2-SnO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-SnO2The character of nano composite material is substantially the same manner as Example 1。
Embodiment 4:
The present embodiment provides a kind of stratiform MoS2-SnO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 40%, in alcoholic solution containing 400g aromatic diamine monomer thioether, heating in water bath is to 35 DEG C and stirs 7h, obtains mixed liquor。
Step 2, adds 25gKMnO in mixed liquor4Powder, heating in water bath is to 80 DEG C and stirs 3.5h, adds 12gSnO under fast stirring2Nanometer powder, continues stirring 2.5h, filters and is dried by filter cake, obtains 15g intercalation MoS2-SnO2Mixed-powder。
Step 3, takes 3g intercalation MoS2-SnO2Mixed-powder is with 6g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 550 DEG C, takes out explosive reaction thing, namely obtain stratiform MoS after cooling to room temperature with the furnace2-SnO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-SnO2The character of nano composite material is substantially the same manner as Example 1。
Embodiment 5:
The present embodiment provides a kind of stratiform MoS2-SnO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 60%, in alcoholic solution containing 300g aromatic diamine monomer thioether, heating in water bath is to 45 DEG C and stirs 5h, obtains mixed liquor。
Step 2, adds 20gKMnO in mixed liquor4Powder, heating in water bath is to 85 DEG C and stirs 2h, adds 16gSnO under fast stirring2Nanometer powder, continues stirring 3h, filters and is dried by filter cake, obtains 18g intercalation MoS2-SnO2Mixed-powder。
Step 3, takes 3g intercalation MoS2-SnO2Mixed-powder is with 7.5g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 510 DEG C, takes out explosive reaction thing, namely obtain stratiform MoS after cooling to room temperature with the furnace2-SnO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-SnO2The character of nano composite material is substantially the same manner as Example 1。
Embodiment 6:
The present embodiment provides a kind of stratiform MoS2-SnO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 50%, in alcoholic solution containing 200g aromatic diamine monomer thioether, heating in water bath is to 50 DEG C and stirs 3h, obtains mixed liquor。
Step 2, adds 10gKMnO in mixed liquor4Powder, heating in water bath is to 90 DEG C and stirs 3h, adds 20gSnO under fast stirring2Nanometer powder, continues stirring 3h, filters and is dried by filter cake, obtains 22.5g intercalation MoS2-SnO2Mixed-powder。
Step 3, takes 3g intercalation MoS2-SnO2Mixed-powder is with 9g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 500 DEG C, takes out explosive reaction thing, namely obtain stratiform MoS after cooling to room temperature with the furnace2-SnO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-SnO2The character of nano composite material is substantially the same manner as Example 1。
Comparative example 1:
This comparative example provides a kind of MoS2-SnO2The preparation method of composite, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 5%, in alcoholic solution containing 50g aromatic diamine monomer thioether, heating in water bath is to 25 DEG C and stirs 2h, obtains mixed liquor。
Step 2, adds 5gKMnO in mixed liquor4Powder, heating in water bath is to 45 DEG C and stirs 1h, adds 2gSnO under fast stirring2Nanometer powder, continues stirring 1h, filters and is dried by filter cake, obtains 5g pretreatment MoS2-SnO2Mixed-powder。
Step 3, takes 3g pretreatment MoS2-SnO2Mixed-powder is with 1g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 600 DEG C, takes out explosive reaction thing, obtain MoS after cooling to room temperature with the furnace2-SnO2Complex。
The MoS that this comparative example is prepared2-SnO2Complex carries out Raman spectrum analysis and tem analysis。
Raman spectrum is as it is shown on figure 3, its E2g 1With Ag 1Value respectively 383.94 and 409.51, displacement difference is 25.57, belongs to block structure MoS2.
TEM image as shown in Figure 4, illustrates this product MoS2Block is piled up, and presents multiple structure, and at MoS2Surface or surrounding do not find obvious SnO2Granule, is not belonging to monolayer or few layer MoS2Nano composite material。
Comparative example 2:
This comparative example provides a kind of MoS2-SnO2The preparation method of composite, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 70%, in alcoholic solution containing 500g aromatic diamine monomer thioether, heating in water bath is to 60 DEG C and stirs 4h, obtains mixed liquor。
Step 2, adds 2gKMnO in mixed liquor4Powder, heating in water bath is to 35 DEG C and stirs 2h, adds 1gSnO under fast stirring2Nanometer powder, continues stirring 0.5h, filters and is dried by filter cake, obtains 3.8g pretreatment MoS2-SnO2Mixed-powder。
Step 3, takes 3g pretreatment MoS2-SnO2Mixed-powder is with 1.5g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 650 DEG C, takes out explosive reaction thing, obtain MoS after cooling to room temperature with the furnace2-SnO2Complex。
The MoS that this comparative example prepares2-SnO2Composite block the same as comparative example 1 is piled up, and SnO2Granule occurs in MoS2Block surface and surrounding, be not belonging to monolayer or few layer molybdenum disulfide nano-composite material。
Comparative example 3:
This comparative example provides a kind of MoS2-SnO2The preparation method of composite, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 8%, in alcoholic solution containing 60g aromatic diamine monomer thioether, heating in water bath is to 70 DEG C and stirs 6h, obtains mixed liquor。
Step 2, adds 25gKMnO in mixed liquor4Powder, heating in water bath is to 20 DEG C and stirs 8h, adds 22gSnO under fast stirring2Nanometer powder, continues stirring 5h, filters and is dried by filter cake, obtains 25.5g pretreatment MoS2-SnO2Mixed-powder。
Step 3, takes 3g pretreatment MoS2-SnO2Mixed-powder is with 10g picric acid by mixing homogeneously in loading autoclave, and evacuation also passes into argon, reactor heating is blasted to 620 DEG C, takes out explosive reaction thing, obtain MoS after cooling to room temperature with the furnace2-SnO2Complex。
The MoS that this comparative example prepares2-SnO2Composite block the same as comparative example 1 is piled up, and SnO2Granule occurs in MoS2Block surface and surrounding, be not belonging to monolayer or few layer molybdenum disulfide nano-composite material。
Claims (10)
1. a stratiform MoS2-SnO2The preparation method of nano composite material, it is characterised in that: the method comprises the following steps:
Step one, adds molybdenum disulfide powder and carries out layering reaction in layering solution, form mixed liquor；
Step 2, adds oxidant in mixed solution and carries out oxidation intercalation, then add SnO under stirring2Nanometer powder, obtains intercalation MoS after continuing to stir2-SnO2Mixed-powder；
Step 3, by intercalation MoS2-SnO2Mixed-powder mixes with burster, carries out explosive reaction, takes out explosive reaction product, namely obtain stratiform MoS after being cooled to room temperature2-SnO2Nano composite material。
2. preparation method as claimed in claim 1, it is characterised in that: described layering solution is the alcoholic solution of aromatic thioether；Described oxidant is potassium permanganate；Described burster is picric acid。
3. preparation method as claimed in claim 2, it is characterised in that: described aromatic thioether is polyphenylene sulfide or aromatic diamine monomer thioether, and the mass concentration of the alcoholic solution of aromatic thioether is 10%～60%。
4. preparation method as claimed in claim 2, it is characterized in that: in step one, the detailed process of described layering reaction is: molybdenum disulfide powder is ground to 200 orders and sieves, molybdenum disulfide powder is added in the alcoholic solution of aromatic thioether, heating is to 30～50 DEG C and stirs 5～12h, forms mixed liquor。
5. preparation method as claimed in claim 2, it is characterised in that: in step one, the mass ratio of described molybdenum disulfide powder and aromatic thioether is 1:(10～40)。
6. preparation method as claimed in claim 2, it is characterised in that: the detailed process of described step 2 is: add KMnO in mixed solution4Powder, heating in water bath is to 50～90 DEG C and stirs 2～5h, under agitation adds SnO2Nanometer powder, continues stirring 1～3h, filters and dry, obtain intercalation MoS2-SnO2Mixed-powder。
7. preparation method as claimed in claim 2, it is characterised in that: in step 2, described potassium permanganate and the molybdenum bisuphide in mixed liquor mass ratio be (0.5～3): 1。
8. preparation method as claimed in claim 2, it is characterised in that: in step 2, described SnO2Molybdenum bisuphide in nanometer powder and mixed liquor mass ratio be (0.3～2): 1。
9. preparation method as claimed in claim 2, it is characterised in that: in step 3, the detailed process of described explosive reaction is: by intercalation MoS2-SnO2Mixed-powder is mixed homogeneously with burster, loads in autoclave, and by autoclave evacuation and pass into argon, heating, to 350～600 DEG C of reactions of blasting, cools to taking-up explosive reaction thing after room temperature with the furnace, namely obtains stratiform MoS2-SnO2Nano composite material。
10. preparation method as claimed in claim 2, it is characterised in that: in step 3, described intercalation MoS2-SnO2Mixed-powder and picric mass ratio 1:(0.5～3)。
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