CN106145192B - A kind of preparation method of two dimensional nano electrodes material - Google Patents
A kind of preparation method of two dimensional nano electrodes material Download PDFInfo
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- CN106145192B CN106145192B CN201610521339.5A CN201610521339A CN106145192B CN 106145192 B CN106145192 B CN 106145192B CN 201610521339 A CN201610521339 A CN 201610521339A CN 106145192 B CN106145192 B CN 106145192B
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- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 50
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 25
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010949 copper Substances 0.000 claims abstract description 14
- 238000009830 intercalation Methods 0.000 claims abstract description 13
- 230000002687 intercalation Effects 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052802 copper Inorganic materials 0.000 claims abstract description 12
- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- 239000002114 nanocomposite Substances 0.000 claims abstract description 3
- 239000002086 nanomaterial Substances 0.000 claims description 27
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 21
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims description 20
- 238000012545 processing Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- CMXPERZAMAQXSF-UHFFFAOYSA-M sodium;1,4-bis(2-ethylhexoxy)-1,4-dioxobutane-2-sulfonate;1,8-dihydroxyanthracene-9,10-dione Chemical compound [Na+].O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=CC=C2O.CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC CMXPERZAMAQXSF-UHFFFAOYSA-M 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- DLEDOFVPSDKWEF-UHFFFAOYSA-N lithium butane Chemical compound [Li+].CCC[CH2-] DLEDOFVPSDKWEF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- 230000005518 electrochemistry Effects 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 230000003287 optical effect Effects 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 6
- 239000002055 nanoplate Substances 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005253 cladding Methods 0.000 abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000010970 precious metal Substances 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 239000000356 contaminant Substances 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract description 2
- 239000002135 nanosheet Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 6
- 229910001431 copper ion Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000011787 zinc oxide Substances 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/40—Electric properties
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- 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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention discloses a kind of doping of non precious metal, the preparation method for the two dimensional nano electrodes material that cost is low, to prepare simple, photoelectric activity high.The titanium dioxide nanoplate material of this method In-situ reaction Copper-cladding Aluminum Bar on the molybdenum disulfide nano sheet of copper intercalation, one kettle way is prepared for the two-dimensional nano composite Cu TiO of copper-doped titanium dioxide nano square In-situ reaction molybdenum disulfide2/MoS2.Prepared Cu TiO2/MoS2It can be applied to that prepared by solar-energy photo-voltaic cell, optical electro-chemistry sensor is built and the field such as photocatalytic water splitting hydrogen manufacturing, photocatalysis degradation organic contaminant.The invention belongs to Nano-function thin films and green energy resource technical field.
Description
Technical field
The present invention relates to a kind of preparation method of two-dimension nano materials, prepared two-dimension nano materials have optical electro-chemistry
Activity, can be applied to solar-energy photo-voltaic cell preparation, optical electro-chemistry sensor and builds and photocatalytic water splitting hydrogen manufacturing, photocatalysis
The fields such as degradable organic pollutant.The invention belongs to Nano-function thin films and green energy resource technical field.
Background technology
Solar cell is also known as " solar chip " or " photocell ", is a kind of photoelectricity of the utilization sunshine direct generation of electricity
Wafer.As long as the illumination that it is satisfied certain illumination conditions is arrived, moment output voltage and can have the situation in loop
Lower generation electric current.Physically it is being referred to as photovoltaic, abbreviation photovoltaic.Solar cell is by photoelectric effect or photochemical
Learn the device that effect directly changes into luminous energy electric energy.The electrode material commonly used in photovoltaic cell mainly includes silica, dioxy
Change a variety of semiconductors, wherein titanium dioxide such as titanium, zinc oxide（TiO2）Because its oxidability is strong, chemical property stablizes nontoxic, and
And can be by as photochemical catalyst, for photocatalytic water splitting hydrogen manufacturing and photocatalysis degradation organic contaminant.However, fully to send out
The actual application level of titanium dioxide is waved, it is necessary on the one hand be carried by regulating and controlling its material morphology to expose more high activity crystal faces
Bloom electro-chemical activity, on the other hand regulates and controls photosensitive wavelength by adulterate different metal or metal oxide and expands to visible-range
Open up to improve the utilization rate of sunshine.Due to two-dimentional titanium dioxide nano material, such as titanium dioxide nanoplate, nano titania
Square etc., can expose more high activity crystal faces, and with higher optical electro-chemistry activity, titanium dioxide nanoplate has than receiving
Rice corpuscles preferably application prospect, the research for titanium dioxide nanoplate also receives much concern.And single nano titania
The photosensitive wavelength of material is general in ultra-violet (UV) band, and due to bad dispersibility, easily stack and interact, so as to reduce optical electro-chemistry
Activity, is unfavorable for practical application.Therefore, R＆D costs are low, prepare the nano titania material of simple bloom electro-chemical activity
Material has important scientific meaning and application value.
Molybdenum disulfide（Chemical formula is MoS2）Nano material, is most widely used solid profit with two-dimensional layered structure
One of lubrication prescription.Sheet two-dimension nano materials after its stripping, are the semiconductor nano materials of excellent performance, except with big ratio
Surface area, can improve load capacity as catalyst and the carrier of biological antibody, while also having as co-catalyst excellent
Electron transmission performance.
At present, most synthesizing mean is all after being separately synthesized, then catalyst and carrier are combined, and process is numerous
Trivial, yield is not high.Therefore, for In-situ reaction prepare with superior catalytic performance catalyst be with a wide range of applications and
Important scientific meaning.
In summary, designed on suitable carrier, prepare bloom electro-chemical activity, the titanium dioxide of high dispersion stability
Nanometer sheet, be prepare titanium dioxide nano material and and then prepare bloom electro-chemical activity two dimensional nano electrodes material key
Technology.
The content of the invention
It is an object of the invention to provide a kind of doping of non precious metal, cost is low, it is simple to prepare, lived with high optical electro-chemistry
The two dimensional nano electrodes material of property.
The technical solution adopted by the present invention is as follows：
1. a kind of preparation method of two dimensional nano electrodes material, described two dimensional nano electrodes material is Copper-cladding Aluminum Bar dioxy
Change the two-dimensional nano composite Cu-TiO of titanium nano square In-situ reaction molybdenum disulfide2/MoS2, it is characterised in that it is described
Cu-TiO2/MoS2Preparation process be：
（1）Because molybdenum disulfide is two-dimensional layered structure, it is possible to use lithium ion carries out intercalation processing to it, to reach profit
In peeling off so as to prepare the purpose of laminated structure molybdenum disulfide thin layer two-dimension nano materials, therefore, the present invention takes 0.6 g bis- first
Vulcanization molybdenum powder and 0.2 ~ 2.0 mmol mantoquitas are added in 3 ~ 10 mL n-butyllithium solutions jointly, in nitrogen protection and 30
At ~ 60 DEG C, stir 12 ~ 48 hours, the reaction is inserted in succession using the smaller lithium ion of radius and the larger copper ion of radius
Layer is layers-separated by molybdenum disulfide block materials into molybdenum disulfide, after reaction fully, obtains reacted solution；
（2）Utilize non-polar solven washing step（1）In reacted solution, use aperture for 450 μm filter membrane carry out
Filtering, gained solid is dissolved in ethanol water, and water bath sonicator processing is then carried out at 30 ~ 60 DEG C, by lithium ion and
The molybdenum disulfide of copper ion intercalation carries out ultrasonic stripping, after handle, the solution after recycling ethanol carrying out washing treatment, by radius compared with
After small lithium ion washing is removed, vacuum drying obtains the molybdenum disulfide nano material of copper intercalation, due to the curing after stripping
Molybdenum sheet shape dimensional thinlayer nano material, with larger specific surface area, has adsorbed the copper ion in reaction, therefore obtained copper
The molybdenum disulfide nano material of intercalation is the molybdenum disulfide sheet two-dimension nano materials for being adsorbed with copper ion；
（3）Take 10 ~ 500 mg steps（2）The molybdenum disulfide nano material of obtained copper intercalation is added to 5 mL metatitanic acids four
In butyl ester, after stirring 1 hour, 0.5 ~ 0.8 mL hydrofluoric acid is slowly added to while stirring, then in reaction at 160 ~ 180 DEG C
Reacted 18 ~ 20 hours in kettle so that titanium dioxide nanoplate In-situ reaction, shape on molybdenum disulfide sheet two-dimension nano materials
Into composite nano materials, because the copper ion adsorbed on molybdenum disulfide sheet two-dimension nano materials grows in titanium dioxide nanoplate
During, course of reaction is participated in, the nano titania square material of Copper-cladding Aluminum Bar has been obtained, and be dispersed in molybdenum disulfide well
On sheet two-dimension nano materials；
（4）By step（3）The reaction product of gained is true at 50 DEG C after ultra-pure water and absolute ethyl alcohol centrifuge washing three times
Sky is dried, that is, Cu-TiO is made2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described mantoquita is selected from one of following：Copper sulphate, copper chloride, copper nitrate, organocopper compound；
Described non-polar solven is selected from one of following：Hexane, hexamethylene, carbon tetrachloride, benzene, toluene；
The volume ratio of second alcohol and water is 0.5 ~ 3 in described ethanol water, the aqueous solution（Ethanol）：1（Water）；
Described water bath sonicator processing, processing time is 1 hour.
The useful achievement of the present invention
（1）Two dimensional nano electrodes material preparation method of the present invention is simple, quick, and non precious metal doping, cost are low,
With market development prospect；
（2）The present invention is prepared for novel nano electrode material Cu-TiO using the method for In-situ reaction first2/MoS2, the party
Method mainly has two advantages：One is, is fully received due to growth in situ of the copper on nano titania square with titanium dioxide
Rice square contact, is acted on using the metal surface plasma body of copper, effectively prevents photo-generate electron-hole to being combined, greatly
Ground improves photocatalytic activity, due to the effect of metal ion, with having widened photosensitive wavelength scope, with realizing in visible region
Opto-electronic conversion, utilization ratio, is imitated although solving two-dimentional titanium dioxide nano material photocatalysis with drastically increasing sunshine
It is really good, but the technical problem that photocatalysis effect is poor, photoelectric conversion rate is low under sunshine irradiation；Two are, due to molybdenum disulfide
The load characteristic and nano titania square of sheet two-dimension nano materials are fully dispersed thereon, solve two-dimentional titanium dioxide
Titanium nano material is unfavorable for scattered and reduces the technical problem of photoelectric conversion rate；Three are, because copper ion had both been made in this process
It is that intercalation material is used as reaction dopant material again, one pot of system of the composite is finally realized using the method for In-situ reaction
It is standby, time, spillage of material are not only saved, and enable the nano titania square of the Copper-cladding Aluminum Bar prepared preferably equal
It is even to be distributed to above molybdenum disulfide sheet two-dimension nano materials.Therefore, effective preparation of the material, with important scientific meaning
And application value；
（3）Nano-electrode material Cu-TiO prepared by the present invention2/MoS2, due to photocatalytic activity height, with efficient light
Electric transformation efficiency, it is easy to film forming, and the good biocompatibility of itself, big specific surface area, high surface mesoporous characterization of adsorption,
Various kinds of sensors can be prepared as host material, such as optical electro-chemistry sensor, Electrochemiluminescsensor sensor, electrochemistry are passed
Sensor etc., with extensive potential use value.
Embodiment
The Cu-TiO of embodiment 12/MoS2Preparation
（1）0.6 g molybdenum disulfide powders and 0.2 mmol mantoquitas is taken to be added to jointly in 3 mL n-butyllithium solutions, in nitrogen
At gas shielded and 60 DEG C, stir 12 hours, obtain reacted solution；
（2）Utilize non-polar solven washing step（1）In reacted solution, water bath sonicator is then carried out at 60 DEG C
Processing, after having handled, recycles the solution after non-polar solven carrying out washing treatment, vacuum drying obtains the molybdenum disulfide of copper intercalation
Nano material；
（3）Take 500 mg steps（2）The molybdenum disulfide nano material of obtained copper intercalation is added to 5 mL butyl titanates
In, after stirring 1 hour, 0.5 mL hydrofluoric acid is slowly added to while stirring, is then reacted in a kettle. 18 hours at 160 DEG C；
（4）By step（3）The reaction product of gained is true at 50 DEG C after ultra-pure water and absolute ethyl alcohol centrifuge washing three times
Sky is dried, that is, Cu-TiO is made2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described mantoquita is copper sulphate；
Described non-polar solven is hexane；
Described water bath sonicator processing, processing time is 1 hour.
The Cu-TiO of embodiment 22/MoS2Preparation
（1）0.6 g molybdenum disulfide powders and 1.0 mmol mantoquitas are taken to be added to jointly in 5 mL n-butyllithium solutions, in nitrogen
At gas shielded and 30 DEG C, stir 24 hours, obtain reacted solution；
（2）Utilize non-polar solven washing step（1）In reacted solution, water bath sonicator is then carried out at 30 DEG C
Processing, after having handled, recycles the solution after non-polar solven carrying out washing treatment, vacuum drying obtains the molybdenum disulfide of copper intercalation
Nano material；
（3）Take 200 mg steps（2）The molybdenum disulfide nano material of obtained copper intercalation is added to 5 mL butyl titanates
In, after stirring 1 hour, 0.6 mL hydrofluoric acid is slowly added to while stirring, is then reacted in a kettle. 20 hours at 180 DEG C；
（4）By step（3）The reaction product of gained is true at 50 DEG C after ultra-pure water and absolute ethyl alcohol centrifuge washing three times
Sky is dried, that is, Cu-TiO is made2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described mantoquita is copper chloride；
Described non-polar solven is carbon tetrachloride；
Described water bath sonicator processing, processing time is 1 hour.
The Cu-TiO of embodiment 32/MoS2Optical electro-chemistry test
By the Cu-TiO prepared by embodiment 12/MoS2It is soluble in water, the Cu-TiO that concentration is 5 mg/mL is made2/MoS2
Colloidal sol, takes 0.02 mL Cu-TiO2/MoS2Sol-Modified is in ITO electrode, using saturated calomel electrode as reference electrode, platinum filament
Electrode collectively constitutes three-electrode system as auxiliary electrode, is connected on optical electro-chemistry detection device；Successively add in a cell
Enter 15mL pH=5.4 Tris-HCl cushioning liquid and the mmol/L of 5 mL 10 L-AA -2- tricresyl phosphate sodium salts AAP it is molten
Liquid；Using i-t means of testing, test gained photo-current intensity can reach 0.2 mA, illustrate the Cu-TiO prepared by the present invention2/
MoS2With actual application value.
The Cu-TiO of embodiment 42/MoS2Photocatalytic activity test
By the Cu-TiO prepared by embodiment 22/MoS2It is soluble in water, the Cu-TiO that concentration is 5 mg/mL is made2/MoS2
Colloidal sol, takes 0.02 mL Cu-TiO2/MoS2Sol-Modified is in ITO electrode, using saturated calomel electrode as reference electrode, platinum filament
Electrode collectively constitutes three-electrode system as auxiliary electrode, is connected on optical electro-chemistry detection device；Successively add in a cell
Enter 15mL pH=5.4 Tris-HCl cushioning liquid and the mmol/L of 5 mL 10 L-AA -2- tricresyl phosphate sodium salts AAP it is molten
Liquid；Using i-t means of testing, test gained photo-current intensity can reach 0.2 mA, illustrate the Cu-TiO prepared by the present invention2/
MoS2With actual application value.
Claims (1)
1. a kind of preparation method of two dimensional nano electrodes material, described two dimensional nano electrodes material is received for copper-doped titanium dioxide
The two-dimensional nano composite Cu-TiO of rice square In-situ reaction molybdenum disulfide2/MoS2, it is characterised in that described Cu-TiO2/
MoS2Preparation process be：
（1）0.6 g molybdenum disulfide powders and 0.2 ~ 2.0 mmol mantoquitas is taken to be added to 3 ~ 10 mL n-butyllithium solutions jointly
In, at nitrogen protection and 30 ~ 60 DEG C, stir 12 ~ 48 hours, obtain reacted solution；
（2）Utilize non-polar solven washing step（1）In reacted solution, water bath sonicator is then carried out at 30 ~ 60 DEG C
Processing, after having handled, recycles the solution after non-polar solven carrying out washing treatment, vacuum drying obtains the molybdenum disulfide of copper intercalation
Nano material；
（3）Take 10 ~ 500 mg steps（2）The molybdenum disulfide nano material of obtained copper intercalation is added to 5 mL butyl titanates
In, after stirring 1 hour, 0.5 ~ 0.8 mL hydrofluoric acid is slowly added to while stirring, then at 160 ~ 180 DEG C in a kettle.
Reaction 18 ~ 20 hours；
（4）By step（3）The reaction product of gained, after ultra-pure water and absolute ethyl alcohol centrifuge washing three times, vacuum is done at 50 DEG C
It is dry, that is, Cu-TiO is made2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described mantoquita is selected from one of following：Copper sulphate, copper chloride, copper nitrate, organocopper compound；
Described non-polar solven is selected from one of following：Hexane, hexamethylene, carbon tetrachloride, benzene, toluene；
Described water bath sonicator processing, processing time is 1 hour.
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