CN105597785A - Method for preparing efficient copper-doped MoS2 nano-sheet array electrocatalyst - Google Patents
Method for preparing efficient copper-doped MoS2 nano-sheet array electrocatalyst Download PDFInfo
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- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 33
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title abstract description 9
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title abstract description 4
- 239000002135 nanosheet Substances 0.000 title abstract 3
- 239000010411 electrocatalyst Substances 0.000 title abstract 2
- 239000010949 copper Substances 0.000 claims abstract description 42
- 229910052802 copper Inorganic materials 0.000 claims abstract description 37
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000003491 array Methods 0.000 claims description 39
- 239000003054 catalyst Substances 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 16
- 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
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 150000002825 nitriles Chemical class 0.000 claims description 5
- VMQMZMRVKUZKQL-UHFFFAOYSA-N Cu+ Chemical compound [Cu+] VMQMZMRVKUZKQL-UHFFFAOYSA-N 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 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 3
- 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 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 9
- 238000000354 decomposition reaction Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 2
- 238000003786 synthesis reaction Methods 0.000 abstract 2
- 238000006555 catalytic reaction Methods 0.000 description 11
- 239000010935 stainless steel Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 230000005611 electricity Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000000243 solution Substances 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
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000002083 X-ray spectrum Methods 0.000 description 1
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 description 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 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design 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
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 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
- 238000001228 spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000007704 transition 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
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- 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
-
- B01J35/33—
-
- B01J35/60—
-
- 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
Abstract
The invention discloses a method for preparing an efficient copper-doped MoS2 nano-sheet array electrocatalyst. The preparing method includes the steps that a 2,300-mesh stainless wire mesh serves as a substrate material, Mo7O24.6 (NH4).4(H2O) and CH4N2S serve as raw materials, and a material is synthesized at the certain synthesis temperature and the certain synthesis time in a water phase system; the efficient electrocatalytic activity of the obtained MoS2 nano-sheet array material is further obtained by doping copper. By means of the method, the product is environmentally friendly, can be prepared in a large-scale mode and has the efficient water electrocatalytic decomposition hydrogen generation performance.
Description
Technical field
The present invention relates to inorganic nanometer functional Material Field, be specifically related to the doping of a kind of copper efficientlyMoS2The preparation method of nano-chip arrays eelctro-catalyst.
Background technology
Along with the development of society and economy, environmental pollution is day by day serious, and global fossil energyAlso progressively exhausted. For the sustainable development in the world, how solving energy scarcity problem is total manThat class faces is the most urgent, one of the task of tool challenge. In order fundamentally to address this problem,Be badly in need of finding alternative green energy resource and reduce the dependence of the mankind to non-renewable fossil fuelDegree. Hydrogen is a kind of desirable clean energy resource. Comparatively speaking, water-splitting is a kind of reasonThe green of thinking is prepared hydrogen route. At present, in thermal decomposition water, photochemical catalyzing and electro-catalysisIn the middle of decomposition water, electro-catalysis decomposition water has actual application prospect most. Therefore exploitation electricity efficientlyCatalyst is applied to decomposition aquatic products hydrogen becomes the hot fields of current research.
At present, it is platinum, palladium one that aquatic products hydrogen catalyst is decomposed in the electro-catalysis that efficiency of energy utilization is the highestClass noble metal and corresponding complexes thereof. But because it is expensive and energy storage is low, limit greatlyMake the practical application of such material aspect electro-catalysis. The noble metal of comparing, transition goldBelong to sulfide M oS2It is catalysis material a kind of cheapness, that reserves are abundant. But block MoS2ByIn its avtive spot expose less, hydrophilicity is poor, the active shortcoming such as weak of surface catalysis, its electricity is urgedChange decomposition water performance limited. On the other hand, the MoS of current bibliographical information2Eelctro-catalyst is mostlyPowder, detects its electro-catalysis decomposition water performance after employing is carried on glass-carbon electrode. Should for realityWith, extensive hydrogen production by water decomposition, powder eelctro-catalyst needs immobilized in large-area substrates materialOn material.
Summary of the invention
For the deficiencies in the prior art, the present invention aims to provide a kind of doping of copper efficiently MoS2The preparation method of nano-chip arrays eelctro-catalyst, by solvent-thermal method directly at stainless steel cloth tableThe MoS of face supported copper doping2Nano-chip arrays. This material has large specific area, goodHydrophily, the advantages such as high surface catalysis activity, present outstanding electro-catalysis decomposition water activity,Be expected to be applied to preparation of industrialization hydrogen.
To achieve these goals, the present invention adopts following technical scheme:
A kind of doping of copper efficiently MoS2The preparation method of nano-chip arrays eelctro-catalyst, comprise asLower step:
S1 synthesizes MoS2Nano-chip arrays:
1.1) by ammonium molybdate (Mo7O24.6(NH4).4(H2) and thiocarbamide (CH O)4N2S) put successivelyEnter in container, fill water, then carry out ultrasonic dissolution;
1.2) in described container, put into stainless wire mesh sheet isothermal reaction at 220 DEG C;After reaction finishes, be cooled to room temperature, products therefrom carries out respectively ultrasonic rear dry in second alcohol and water,Obtain MoS2Nano-chip arrays;
The synthetic copper doping of S2 MoS2Nano-chip arrays eelctro-catalyst:
2.1) by fluorophosphoric acid tetrem nitrile copper (I) (C8H12CuF6N4P) put into through pretreatedIn single necked round bottom flask, single necked round bottom flask pretreatment mode is to soak in the solution of pH=4The post-drying of spending the night is stand-by;
2.2) MoS that adds acetone and step S1 to prepare toward described single necked round bottom flask2Nano-chip arrays then carries out oil bath at 60 DEG C, and question response is got after finishing to be cooled to room temperatureGo out product and directly dry, obtain copper doping MoS2Nano-chip arrays eelctro-catalyst.
It should be noted that step 1.1) in, add ammonium molybdate (Mo7O24.6(NH4).4(H2O))And thiocarbamide (CH4N2S) quality is respectively 123mg and 228mg, and the volume of water is 35mL.
It should be noted that step 1.1) in container adopt the high pressure of polytetrafluoroethylliner linerStill.
It should be noted that step 1.1) in, the ultrasonic dissolution time is 10min.
It should be noted that step 1.2) in, the quantity of the twine of described stainless steel isA slice, specification is 1cm × 3cm.
It should be noted that step 1.2) described at 220 DEG C isothermal reaction be specially220 DEG C of isothermal reaction 5h in electric heating constant-temperature blowing drying box.
It should be noted that step 1.2) in, product carries out respectively ultrasonic in second alcohol and waterTime be 5min.
It should be noted that step 2.1) in, hexafluorophosphoric acid tetrem nitrile copper (I) (C8H12CuF6N4P)Quality be 10-60mg.
It should be noted that step 2.2) in, the amount that adds acetone is 30mL.
It should be noted that step 2.2) in, the oil bath time is 1h.
Beneficial effect of the present invention is:
1, the present invention is simple to operate, needed raw material green, and method is reproducible, can advise greatlyMolded standby;
2、MoS2Nanometer sheet has large specific area, abundant avtive spot, and array is receivedRice sheet is because large roughness can present good hydrophily; Stainless steel cloth is cheap,Enriching, conduct electricity very well in source, is beneficial to and improves material electro catalytic activity, and copper doped can be enteredOne step increases its surface catalysis activity. The copper doping MoS preparing by the inventive method2The well-regulated sheet-like array structure of nano-chip arrays eelctro-catalyst tool, highly approximately 1 μ m, easily mixesHeteroion, exposes more avtive spots, and has super hydrophilic performance, is beneficial to electrolyte solutionIon is in the free transmission of material surface.
3, by described copper doping MoS2Nano-chip arrays eelctro-catalyst decomposes aquatic products for electro-catalysisHydrogen has efficient electro-catalysis and decomposes aquatic products hydrogen activity, simple to operate, has good practical valencyValue 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) beTop view and 1b) be sectional view.
Fig. 2 is copper doping MoS prepared by the present invention2The powder X-ray of nano-chip arrays eelctro-catalyst-X ray diffraction style schematic diagram.
Fig. 3 is copper doping MoS prepared by the present invention2The energy look of nano-chip arrays eelctro-catalystLoose spectrum schematic diagram.
Fig. 4 is copper doping MoS2The ESEM picture of nano-chip arrays eelctro-catalyst.
Fig. 5 is at different base load MoS2The electrocatalysis characteristic figure of material.
Fig. 6 be difference mix under Cu amount electrocatalysis characteristic figure.
Fig. 7 is load MoS2After the contact angle of stainless wire mesh.
Fig. 8 prepares material to mix the impedance spectrogram under Cu amount in difference.
Detailed description of the invention
Below with reference to accompanying drawing, the invention will be further described, it should be noted that this realityExecute example taking the technical program as prerequisite, provided detailed embodiment and concrete operating process,But protection scope of the present invention is not limited to the present embodiment.
Embodiment 1
(1) synthetic MoS2Nano-chip arrays
Take 123mg Ammonium Molybdate Tetrahydrate (Mo7O24.6(NH4).4(H2O)), 228mg thiocarbamide(CH4N2S) put into after the polytetrafluoroethylliner liner (V=60mL) of autoclave, add35mL water, in ultrasonic cleaning instrument, ultrasonic 10min dissolves. In this solution, put into 1cmTwine a slice of the stainless steel of × 3cm, autoclave is in electric heating constant-temperature blowing drying box220 DEG C of isothermal reaction 5h. After reaction finishes, be cooled to room temperature, product divides in ethanol, waterNot not ultrasonic 5min can put into drying box dried for standby. Fig. 1 is the MoS obtaining2Nanometer sheetThe ESEM picture of array, 1a) be top view and 1b) be sectional view. As can be seen from the figureThis material is nano-chip arrays structure, array height approximately 1 μ m.
(2) MoS of synthetic copper doping2Nano-chip arrays eelctro-catalyst
Take hexafluorophosphoric acid tetrem nitrile copper (the I) (C of different amounts (20,40,60mg)8H12CuF6N4P)Mono-in the 50mL that anticipates (in the solution at pH=4, soaked overnight post-drying is stand-by)In mouth round-bottomed flask, add the acetone of 30mL and the MoS of the middle preparation of step (1)2NanometerSheet battle array. Oil bath 1h at 60 DEG C, question response finishes to be cooled to and takes out product after room temperature and directly dryDry, obtain the MoS that copper adulterates2Nano-chip arrays eelctro-catalyst.
Fig. 2 is the X-ray diffraction style of product, from X-ray diffraction style, productFor MoS2. Energy dispersion X ray spectrum shows to contain in product copper (as shown in Figure 3). ScanningElectron microscopic observation shows, the pattern of the nano-chip arrays structure that copper adulterates later does not have significant change(as shown in Figure 4).
Below will be further described performance of the present invention by experiment.
Experiment 1
Same synthetic reaction condition, comprises load on copper, nickel, tungsten at different metal silk screenMoS2With at the online load MoS of metal stainless steel wire2Catalytic activity comparison. Taking woven wire asWorking electrode, saturated calomel electrode is reference electrode, platinum filament is to electrode. Adopt linear volt-ampere to sweepRetouch method, sweep limits-0.8V-0.2V, sweep speed 5mV/s, result as shown in Figure 5,At the MoS of the online load of stainless steel wire2Electro-catalysis produce hydrogen activity the best.
Experiment 2
Research MoS2Nano-chip arrays material is mixed Cu amount (20mg, 40mg, 60mg) in differenceUnder at 0.5MH2SO4Electrocatalysis characteristic in system.
Test condition is identical with contrast experiment 1. Produce hydrogen performance as shown in Figure 6, all copper samples of mixingThe electro catalytic activity of product is all better than unadulterated MoS2Nano-chip arrays. When copper doping is 40When mg, catalytic performance the best.
Experiment 3
The hydrophily of the stainless steel cloth after research supported copper. Experimental result shows that water droplet is in loadThe MoS of this copper doping2The stainless steel wire net surface of nano-chip arrays presents Superhydrophilic (as Fig. 7Shown in). Super water wetted material can better contact with water and electrolyte solution, increases the electricity of materialCatalytic activity.
Experiment 4
Research difference is mixed copper amount material at 0.5MH2SO4Charge transfer drag size in system.Experimental result shows along with the increase of mixing Cu amount, its charge transfer resistance more and more less (Fig. 8),Therefore, mix the electric conductivity that Cu can improve material and increase its electrocatalysis characteristic.
For a person skilled in the art, can be according to above technical scheme and design,Make various corresponding changes and distortion, and these all changes and distortion all should be included inWithin the protection domain of the claims in the present invention.
Claims (10)
1. an efficient copper doping MoS2The preparation method of nano-chip arrays eelctro-catalyst, itsBe characterised in that, comprise the steps:
S1 synthesizes MoS2Nano-chip arrays:
1.1) by ammonium molybdate (Mo7O24.6(NH4).4(H2) and thiocarbamide (CH O)4N2S) put successivelyEnter in container, fill water, then carry out ultrasonic dissolution;
1.2) in described container, put into stainless wire mesh sheet isothermal reaction at 220 DEG C;After reaction finishes, be cooled to room temperature, products therefrom carries out respectively ultrasonic rear dry in second alcohol and water,Obtain MoS2Nano-chip arrays;
The synthetic copper doping of S2 MoS2Nano-chip arrays eelctro-catalyst:
2.1) by fluorophosphoric acid tetrem nitrile copper (I) (C8H12CuF6N4P) put into through pretreatedIn single necked round bottom flask, single necked round bottom flask pretreatment mode is to soak in the solution of pH=4The post-drying of spending the night is stand-by;
2.2) MoS that adds acetone and step S1 to prepare toward described single necked round bottom flask2Nano-chip arrays then carries out oil bath at 60 DEG C, and question response is got after finishing to be cooled to room temperatureGo out product and directly dry, obtain copper doping MoS2Nano-chip arrays eelctro-catalyst.
2. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 1.1) in, add ammonium molybdate(Mo7O24.6(NH4).4(H2) and thiocarbamide (CH O)4N2S) quality is respectively 123mg and 228mg,The volume of water is 35mL.
3. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 1.1) in container adopt polytetrafluoroethyl-neThe autoclave of alkene inner bag.
4. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 1.1) in, the ultrasonic dissolution time is 10min.
5. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 1.2) in, described stainless steelTwine sheet is the twine sheet of 2300 object stainless steels, and quantity is a slice, specification be 1cm ×3cm。
6. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 1.2) described at 220 DEG C constant temperatureReaction is specially 220 DEG C of isothermal reaction 5h in electric heating constant-temperature blowing drying box.
7. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 1.2) in, product is in second alcohol and waterCarrying out respectively the ultrasonic time is 5min.
8. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 2.1) in, hexafluorophosphoric acid tetrem nitrile copper(I)(C8H12CuF6N4P) quality is 10-60mg.
9. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 2.2) in, the amount that adds acetone is 30mL。
10. the efficient copper doping of one according to claim 1 MoS2Nano-chip arrays electricityThe preparation method of catalyst, is characterized in that step 2.2) in, the oil bath time is 1h.
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Cited By (8)
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| CN106381481A (en) * | 2016-09-18 | 2017-02-08 | 河南师范大学 | Preparation method of metal doping molybdenum disulfide thin film |
| CN106994357A (en) * | 2016-01-22 | 2017-08-01 | 天津大学 | The molybdenum disulfide material and its synthetic method of a kind of witch culture |
| CN107149940A (en) * | 2017-05-05 | 2017-09-12 | 燕山大学 | A kind of fluorine, nitrogen co-doped method for preparing molybdenum disulfide |
| CN108118362A (en) * | 2018-01-09 | 2018-06-05 | 国家纳米科学中心 | A kind of molybdenum disulfide electro-catalysis production hydrogen electrode and its preparation method and application |
| CN108654656A (en) * | 2018-04-28 | 2018-10-16 | 江苏大学 | The preparation method and applications of phosphatization cobalt porous nano line/stainless steel composite electrocatalyst |
| CN108686685A (en) * | 2018-05-09 | 2018-10-23 | 南京邮电大学 | A kind of copper nano particles/black phosphorus nanosheet composite material and the preparation method and application thereof |
| CN110106519A (en) * | 2019-06-20 | 2019-08-09 | 温州大学 | TiO2/MoS2The preparation method of ultrathin nanometer chip arrays composite material |
| CN110368959A (en) * | 2019-07-15 | 2019-10-25 | 大连理工大学 | A kind of preparation method and applications of the nanocatalyst of efficient process trimethylamine polluted gas |
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| CN106994357A (en) * | 2016-01-22 | 2017-08-01 | 天津大学 | The molybdenum disulfide material and its synthetic method of a kind of witch culture |
| CN106994357B (en) * | 2016-01-22 | 2019-07-19 | 天津大学 | A kind of the molybdenum disulfide material and its synthetic method of witch culture |
| CN106381481A (en) * | 2016-09-18 | 2017-02-08 | 河南师范大学 | Preparation method of metal doping molybdenum disulfide thin film |
| CN106381481B (en) * | 2016-09-18 | 2018-09-14 | 河南师范大学 | A kind of preparation method of metal-doped molybdenum disulfide film |
| CN107149940A (en) * | 2017-05-05 | 2017-09-12 | 燕山大学 | A kind of fluorine, nitrogen co-doped method for preparing molybdenum disulfide |
| CN107149940B (en) * | 2017-05-05 | 2020-07-28 | 燕山大学 | Preparation method of fluorine and nitrogen co-doped molybdenum disulfide |
| CN108118362A (en) * | 2018-01-09 | 2018-06-05 | 国家纳米科学中心 | A kind of molybdenum disulfide electro-catalysis production hydrogen electrode and its preparation method and application |
| CN108654656A (en) * | 2018-04-28 | 2018-10-16 | 江苏大学 | The preparation method and applications of phosphatization cobalt porous nano line/stainless steel composite electrocatalyst |
| CN108686685A (en) * | 2018-05-09 | 2018-10-23 | 南京邮电大学 | A kind of copper nano particles/black phosphorus nanosheet composite material and the preparation method and application thereof |
| CN110106519A (en) * | 2019-06-20 | 2019-08-09 | 温州大学 | TiO2/MoS2The preparation method of ultrathin nanometer chip arrays composite material |
| CN110368959A (en) * | 2019-07-15 | 2019-10-25 | 大连理工大学 | A kind of preparation method and applications of the nanocatalyst of efficient process trimethylamine polluted gas |
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