CN105597785B - A kind of efficient Copper-cladding Aluminum Bar MoS2The preparation method of nano-chip arrays elctro-catalyst - Google Patents
A kind of efficient Copper-cladding Aluminum Bar MoS2The preparation method of nano-chip arrays elctro-catalyst Download PDFInfo
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- 238000003491 array Methods 0.000 title claims abstract description 41
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 31
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000005253 cladding Methods 0.000 title claims abstract description 31
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 24
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- INRYEEIIXAOXBN-UHFFFAOYSA-N acetonitrile;copper(1+) Chemical compound [Cu+].CC#N INRYEEIIXAOXBN-UHFFFAOYSA-N 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 2
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims 2
- 230000036571 hydration Effects 0.000 claims 2
- 238000006703 hydration reaction Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 19
- 239000010949 copper Substances 0.000 abstract description 12
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 238000000354 decomposition reaction Methods 0.000 abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052802 copper Inorganic materials 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 abstract 1
- 239000008346 aqueous phase Substances 0.000 abstract 1
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 229940010552 ammonium molybdate Drugs 0.000 description 3
- 235000018660 ammonium molybdate Nutrition 0.000 description 3
- 239000011609 ammonium molybdate Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000010148 water-pollination Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- -1 Ammonium Molybdate Tetrahydrates Chemical class 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- RHFUXPCCELGMFC-UHFFFAOYSA-N n-(6-cyano-3-hydroxy-2,2-dimethyl-3,4-dihydrochromen-4-yl)-n-phenylmethoxyacetamide Chemical compound OC1C(C)(C)OC2=CC=C(C#N)C=C2C1N(C(=O)C)OCC1=CC=CC=C1 RHFUXPCCELGMFC-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
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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
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of efficient Copper-cladding Aluminum Bar MoS2The preparation method of nano-chip arrays elctro-catalyst.The preparation method is the Ammonium Molybdate Tetrahydrate (Mo using the stainless wire mesh of 2300 mesh as base material7O24.6(NH4).4(H2O)), thiocarbamide (CH4N2S it is) raw material, material is synthesized under certain synthesis temperature, time in aqueous phase system；Gained MoS2Nano-chip arrays material further obtains efficient electro catalytic activity by copper doped.Product Green provided by the invention, environmental protection, can scale prepare, and there is efficient electrocatalytic decomposition water H2-producing capacity.
Description
Technical field
The present invention relates to inorganic nanometer functional Material Field, and in particular to a kind of efficient Copper-cladding Aluminum Bar MoS2Nanometer sheet battle array
The preparation method of row elctro-catalyst.
Background technology
With the development of society and economy, environmental pollution getting worse, and global fossil energy are also progressively exhausted.In order to
The sustainable development in the world, how to solve the problems, such as energy scarcity is one of most urgent, most the challenging of the task that the whole mankind faces.
In order to fundamentally solve this problem, it is badly in need of finding alternative green energy resource to reduce the mankind to non-renewable fossil fuel
Degree of dependence.Hydrogen is a kind of preferable clean energy resource.Comparatively speaking, water-splitting is that a kind of preferably green prepares hydrogen
Gas circuit line.At present, among thermal decomposition water, photochemical catalyzing and electrocatalytic decomposition water, electrocatalytic decomposition water is most actual
Application prospect.Therefore efficient elctro-catalyst is developed to be applied to decompose hot fields of the aquatic products hydrogen as current research.
At present, efficiency of energy utilization highest electrocatalytic decomposition aquatic products hydrogen catalyst is platinum, palladium one kind noble metal and its phase
Answer compound.But because its is expensive and energy storage is low, significantly limit reality of such material in terms of electro-catalysis should
With.Compare for noble metal, transient metal sulfide MoS2It is a kind of cheap, catalysis material of rich reserves.But block
MoS2Due to the exposure of its avtive spot less, the shortcomings of hydrophilicity is poor, superficial catalytic activation is weak, its electrocatalytic decomposition is water-based can be by
Limit.On the other hand, the MoS of document report at present2Elctro-catalyst is mostly powder, and its electricity is detected using being carried on after glass-carbon electrode
Water-based energy is catalytically decomposed.For practical applications, extensive hydrogen production by water decomposition, powder elctro-catalyst need immobilized in large area
On base material.
The content of the invention
In view of the shortcomings of the prior art, the present invention is intended to provide a kind of efficient Copper-cladding Aluminum Bar MoS2Nano-chip arrays electro-catalysis
The preparation method of agent, by solvent-thermal method directly in the MoS of stainless steel cloth area load Copper-cladding Aluminum Bar2Nano-chip arrays.The material
Material has the advantages that big specific surface area, good hydrophily, high superficial catalytic activation, shows outstanding electrocatalytic decomposition
Water activity, is expected to be applied to preparation of industrialization hydrogen.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of efficient Copper-cladding Aluminum Bar MoS2The preparation method of nano-chip arrays elctro-catalyst, comprises the following steps：
S1 synthesizes MoS2Nano-chip arrays：
1.1) by ammonium molybdate (Mo7O24.6(NH4).4(H2)) and thiocarbamide (CH O4N2S) it is sequentially placed into container, fills water,
Then ultrasonic dissolution is carried out；
1.2) stainless wire mesh piece and the isothermal reaction at 220 DEG C are put into the above-described container；Reaction is cooled to after terminating
Room temperature, products therefrom are dried after carrying out ultrasound respectively in second alcohol and water, produce MoS2Nano-chip arrays；
S2 synthesis Copper-cladding Aluminum Bars MoS2Nano-chip arrays elctro-catalyst：
2.1) by fluorophosphoric acid four acetonitrile copper (I) (C8H12CuF6N4P) it is put into the single necked round bottom flask by pretreatment, it is single
Mouth round-bottomed flask pretreatment mode is stand-by to be dried after the soaked overnight in pH=4 solution；
2.2) MoS being prepared toward single necked round bottom flask addition acetone and step S12Nano-chip arrays, then
Oil bath is carried out at 60 DEG C, question response, which terminates taking-up product after being cooled to room temperature, directly dries, and produces Copper-cladding Aluminum Bar MoS2Nanometer sheet
Array elctro-catalyst.
It should be noted that in step 1.1), ammonium molybdate (Mo is added7O24.6(NH4).4(H2)) and thiocarbamide (CH O4N2S)
Quality be respectively 123mg and 228mg, the volume of water is 35mL.
It should be noted that the container in step 1.1) uses the autoclave of polytetrafluoroethylliner liner.
It should be noted that in step 1.1), the ultrasonic dissolution time is 10min.
It should be noted that in step 1.2), the quantity of the twine of the stainless steel be it is a piece of, specification be 1cm ×
3cm。
It should be noted that isothermal reaction is specially in electric heating constant temperature forced air drying at 220 DEG C described in step 1.2)
220 DEG C of isothermal reaction 5h in case.
It should be noted that in step 1.2), the time that product carries out ultrasound respectively in second alcohol and water is 5min.
It should be noted that in step 2.1), hexafluorophosphoric acid four acetonitrile copper (I) (C8H12CuF6N4P quality) is 10-
60mg。
It should be noted that in step 2.2), the amount for adding acetone is 30mL.
It should be noted that in step 2.2), the oil bath time is 1h.
The beneficial effects of the present invention are：
1st, the present invention is simple to operate, required raw material green, and method is reproducible, can prepare on a large scale；
2、MoS2Nanometer sheet has big specific surface area, an abundant avtive spot, and array nanometer sheet is due to big coarse
Good hydrophily can be presented in degree；Stainless steel cloth is cheap, abundance, conducts electricity very well, electric beneficial to material is improved
Catalytic activity, copper doped then can further increase its superficial catalytic activation.Obtained Copper-cladding Aluminum Bar is prepared by the method for the present invention
MoS2Nano-chip arrays elctro-catalyst has well-regulated sheet-like array structure, and about 1 μm of height, easy Doped ions, exposure is more
Avtive spot, and there is super hydrophilic performance, beneficial to electrolyte solution ion material surface free transmission.
3rd, by the Copper-cladding Aluminum Bar MoS2Nano-chip arrays elctro-catalyst, which is used for electrocatalytic decomposition aquatic products hydrogen, has efficient electricity
Aquatic products hydrogen activity is catalytically decomposed, it is simple to operate, there is good practical value and application prospect.
Brief description of the drawings
Fig. 1 is MoS prepared by the present invention2The scanning electron microscope (SEM) photograph of nano-chip arrays, wherein 1a) be top view and 1b) it is to cut
Face figure.
Fig. 2 is Copper-cladding Aluminum Bar MoS prepared by the present invention2Powder X-ray-ray powder diffraction pattern of nano-chip arrays elctro-catalyst shows
It is intended to.
Fig. 3 is Copper-cladding Aluminum Bar MoS prepared by the present invention2The energy dispersive spectrum schematic diagram of nano-chip arrays elctro-catalyst.
Fig. 4 is Copper-cladding Aluminum Bar MoS2The ESEM picture of nano-chip arrays elctro-catalyst.
Fig. 5 is to load MoS in different base2The electrocatalysis characteristic figure of material.
Fig. 6 is that the electrocatalysis characteristic figure under Cu amounts is mixed in difference.
Fig. 7 is load MoS2The contact angle of stainless wire mesh afterwards.
Fig. 8 is to prepare material in the different impedance spectras mixed under Cu amounts.
Embodiment
Below with reference to accompanying drawing, the invention will be further described, it is necessary to which explanation, the present embodiment is with this technology side
Premised on case, detailed embodiment and specific operating process are given, but protection scope of the present invention is not limited to this reality
Apply example.
Embodiment 1
(1) MoS is synthesized2Nano-chip arrays
Weigh 123mg Ammonium Molybdate Tetrahydrates (Mo7O24.6(NH4).4(H2O)), 228mg thiocarbamides (CH4N2S) it is put into high pressure
After the polytetrafluoroethylliner liner (V=60mL) of reactor, 35mL water is added, the ultrasonic 10min dissolvings in instrument is cleaned by ultrasonic.
It is put into that the twine of 1cm × 3cm stainless steel is a piece of, and autoclave is in electric heating constant-temperature blowing drying box in this solution
220 DEG C of isothermal reaction 5h.Reaction is cooled to room temperature after terminating, and ultrasonic 5min can be put into drying to product respectively in ethanol, water
Dried for standby in case.Fig. 1 is the MoS obtained2The ESEM picture of nano-chip arrays, 1a) be top view and 1b) it is sectional view.
As can be seen from the figure the material is nano-chip arrays structure, about 1 μm of array heights.
(2) MoS of Copper-cladding Aluminum Bar is synthesized2Nano-chip arrays elctro-catalyst
Weigh hexafluorophosphoric acid four acetonitrile copper (I) (C of not same amount (20,40,60mg)8H12CuF6N4P) in anticipate (
Dried in pH=4 solution after soaked overnight stand-by) 50mL single necked round bottom flask in, add 30mL acetone and step
(1) MoS prepared in2Nanometer sheet battle array.The oil bath 1h at 60 DEG C, question response terminate taking-up product after being cooled to room temperature and directly dried
It is dry, produce the MoS of Copper-cladding Aluminum Bar2Nano-chip arrays elctro-catalyst.
Fig. 2 is the X-ray diffraction style of product, it was found from X-ray diffraction style, product MoS2.Energy dispersion X is penetrated
Line spectrum shows to contain copper (as shown in Figure 3) in product.Scanning electron microscopic observation shows, the later nano-chip arrays structure of Copper-cladding Aluminum Bar
Pattern does not have significant change (as shown in Figure 4).
The performance of the present invention will be further described by testing below.
Experiment 1
Same synthetic reaction condition, include copper, nickel, the MoS loaded on tungsten in different metal silk screen2With it is stainless in metal
MoS is loaded on steel wire2Catalytic activity compare.Using woven wire as working electrode, saturated calomel electrode is reference electrode, platinum
Silk is to electrode.Using linear voltammetric scan method, scanning range -0.8V-0.2V, sweep speed 5mV/s, as a result as shown in figure 5,
The MoS that stainless steel wire loads on the net2Electro-catalysis production hydrogen activity it is optimal.
Experiment 2
Study MoS2Nano-chip arrays material is in the case where difference mixes Cu amounts (20mg, 40mg, 60mg) in 0.5M H2SO4System
Middle electrocatalysis characteristic.
Test condition is identical with contrast experiment 1.H2-producing capacity as shown in fig. 6, it is all mix copper sample electro catalytic activity it is equal
Be better than undoped with MoS2Nano-chip arrays.When Copper-cladding Aluminum Bar amount is in 40 mg, catalytic performance is optimal.
Experiment 3
Study the hydrophily of the stainless steel cloth after supported copper.Test result indicates that water droplet is loading the MoS of the Copper-cladding Aluminum Bar2
Superhydrophilic is presented in the stainless steel wire net surface of nano-chip arrays (as shown in Fig. 7).Super hydrophilic material can preferably with water and electricity
Electrolyte solution contacts, and increases the electro catalytic activity of material.
Experiment 4
Research difference mixes amount of copper material in 0.5M H2SO4Charge transfer drag size in system.Test result indicates that with
The increase for mixing Cu amounts, its charge transfer resistance is less and less (Fig. 8), and therefore, the electric conductivity increase of material can be improved by mixing Cu
Its electrocatalysis characteristic.
For those skilled in the art, technical scheme that can be more than and design, make various corresponding
Change and deform, and all these change and deformation should be construed as being included within the protection domain of the claims in the present invention.
Claims (10)
- A kind of 1. efficient Copper-cladding Aluminum Bar MoS2The preparation method of nano-chip arrays elctro-catalyst, it is characterised in that including following step Suddenly：S1 synthesizes MoS2Nano-chip arrays：1.1) by four hydration ammonium heptamolybdate (Mo7O24·6(NH4)·4(H2)) and thiocarbamide (CH O4N2S) it is sequentially placed into container, fills out Water-filling, then carry out ultrasonic dissolution；1.2) stainless wire mesh piece and the isothermal reaction at 220 DEG C are put into the above-described container；Reaction is cooled to room temperature after terminating, Products therefrom is dried after carrying out ultrasound respectively in second alcohol and water, produces MoS2Nano-chip arrays；S2 synthesis Copper-cladding Aluminum Bars MoS2Nano-chip arrays elctro-catalyst：2.1) by hexafluorophosphoric acid four acetonitrile copper (I) (C8H12CuF6N4P) it is put into the single necked round bottom flask by pretreatment, single port Round-bottomed flask pretreatment mode is stand-by to be dried after the soaked overnight in pH=4 solution；2.2) MoS being prepared toward single necked round bottom flask addition acetone and step S12Nano-chip arrays, then 60 Oil bath is carried out at DEG C, question response, which terminates taking-up product after being cooled to room temperature, directly dries, and produces Copper-cladding Aluminum Bar MoS2Nano-chip arrays Elctro-catalyst.
- A kind of 2. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, it is special Sign is, in step 1.1), adds four hydration ammonium heptamolybdate (Mo7O24· 6(NH4)· 4(H2)) and thiocarbamide (CH O4N2S) Quality is respectively 123mg and 228mg, and the volume of water is 35mL.
- A kind of 3. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, it is special Sign is that the container in step 1.1) uses the autoclave of polytetrafluoroethylliner liner.
- A kind of 4. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, it is special Sign is, in step 1.1), the ultrasonic dissolution time is 10min.
- A kind of 5. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, it is special Sign is, in step 1.2), the twine piece of the stainless steel is the twine piece of the stainless steel of 2300 mesh, quantity one Piece, specification are 1cm × 3cm.
- A kind of 6. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, it is special Sign is that isothermal reaction specially 220 DEG C of constant temperature in electric heating constant-temperature blowing drying box are anti-at 220 DEG C described in step 1.2) Answer 5h.
- A kind of 7. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, it is special Sign is, in step 1.2), the time that product carries out ultrasound respectively in second alcohol and water is 5min.
- A kind of 8. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, it is special Sign is, in step 2.1), hexafluorophosphoric acid four acetonitrile copper (I) (C8H12CuF6N4P quality) is 10-60mg.
- A kind of 9. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, it is special Sign is, in step 2.2), the amount for adding acetone is 30mL.
- A kind of 10. efficient Copper-cladding Aluminum Bar MoS according to claim 12The preparation method of nano-chip arrays elctro-catalyst, its It is characterised by, in step 2.2), the oil bath time is 1h.
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