CN107442138A - A kind of preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth - Google Patents
A kind of preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth Download PDFInfo
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- CN107442138A CN107442138A CN201710452226.9A CN201710452226A CN107442138A CN 107442138 A CN107442138 A CN 107442138A CN 201710452226 A CN201710452226 A CN 201710452226A CN 107442138 A CN107442138 A CN 107442138A
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- carbon cloth
- hydrogen evolution
- mixed solution
- molybdenum disulfide
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 52
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 42
- 239000001257 hydrogen Substances 0.000 title claims abstract description 42
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 32
- 239000004744 fabric Substances 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 23
- 230000000694 effects Effects 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 15
- 150000001875 compounds Chemical class 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 13
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002604 ultrasonography Methods 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 229910052961 molybdenite Inorganic materials 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims 1
- AMWVZPDSWLOFKA-UHFFFAOYSA-N phosphanylidynemolybdenum Chemical compound [Mo]#P AMWVZPDSWLOFKA-UHFFFAOYSA-N 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 3
- 150000001787 chalcogens Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 229910003090 WSe2 Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910052798 chalcogen Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 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
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 239000012064 sodium phosphate buffer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000003643 water by type Substances 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
-
- 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
-
- 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
-
- 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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to electrocatalytic hydrogen evolution field, the preparation method of more particularly to a kind of compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth.The carbon cloth for being cut into regular shape is cleaned, it is placed in after drying in the mixed solution of phosphomolybdic acid and thiocarbamide, ultrasound causes mixed solution to soak carbon cloth completely, then by carbon cloth and mixed solution in being transferred in reactor, hydro-thermal naturally cools to room temperature after 24 hours under 180 degrees celsius, by washing, centrifugation, MoS is dried to obtain2/ CC composite catalysts.Molybdenum disulfide prepared by the present invention is grown on carbon cloth, is evenly distributed.Small compared to compared with molybdenum disulfide nano size obtained by traditional synthetic method, defect is enriched, and interlamellar spacing is wide, and then improves electrocatalytic hydrogen evolution activity.
Description
Technical field
The invention belongs to electrocatalytic hydrogen evolution field, more particularly to a kind of compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth
Preparation method.
Technical background
As global energy and environmental crisis are aggravated, it is to substitute conventional fossil fuel with effective to prepare hydrogen by electrolysis water
Solve growing energy crisis and the effective way of environmental pollution.However, it is necessary to efficiently elctro-catalyst carries out hydrogen precipitation instead
Answer (HER), to provide the high current of low potential.Pt races metal is well known as the most popular electro-catalysis material for evolving hydrogen reaction
Material.However, their high cost and rare deposit limit its application.Therefore, the water decomposition Novel electric of high efficiency low cost is developed
Catalyst is significant, but challenging.Recently, the two-dimentional chalcogen (LTMD) of (2D) stratiform transition metal two, such as
MoS2, WS2, MoSe2, and WSe2It is HER that some significant properties, which are shown, as elctro-catalyst.These materials, MoS2As work
Property HER catalyst has obtained great concern in acid.
MoS2 has the structure of two dimension (2D) layer similar with graphene, and it is shown by the interaction of weak Van der Waals force
S-Mo-S layers, theoretical and experimental study all show MoS2With catalytic activity edge site as HER elctro-catalysts.Therefore, such as
Fruit MoS2Size reduction to nanoscale, then significant increase is caused the increase of HER performances by active edge site.Such as have
The MoS of defect2Ultrathin nanometer piece, hollow ball nanostructured MoS2, edge exposure perforated membrane.In addition, researcher has found MoS2's
The increase of interlamellar spacing contributes to the high activity of Hydrogen evolving reaction.However, extremely low electrical conductivity is significant to reduce overall electro-catalysis analysis
Hydrogen efficiency.In addition, before HER tests, such catalyst need by active material and polymer adhesive (such as
Nafion) mix, this may reduce electric conductivity and block active site to reduce electrocatalysis characteristic.
Carbon cloth (CC) be it is a kind of be easily obtained with cheap carbon fiber, because cost is low, good conductivity, physical strength is high,
Pliability is good, has been widely used in different application field.Meanwhile contribute to connect the electrodes to practical application using carbon cloth
Device.
Present invention synthesis is a kind of to compare more traditional MoS2Fault in material is more, and size is small, MoS2The advantages that interlamellar spacing is wide promotes
Electrocatalytic decomposition aquatic products hydrogen is under full pH environment.There is presently no research to report MoS2Electro-catalysis analysis of the base catalyst under full pH
Hydrogen.
The content of the invention
A kind of preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth, is comprised the following steps that:Established practice will be cut
The then carbon cloth cleaning of shape, is placed in the mixed solution of phosphomolybdic acid and thiocarbamide, ultrasound causes mixed solution to soak completely after drying
Carbon cloth, then by carbon cloth and mixed solution in being transferred in reactor, hydro-thermal natural cooling after 24 hours under 180 degrees celsius
To room temperature, by washing, centrifugation, MoS is dried to obtain2/ CC composite catalysts.
Described regular shape refers to 1cm × 2cm size identical rectangles;The cleaning refers in acetone, ethanol and goes successively
It is cleaned by ultrasonic 10min in ionized water respectively.
The phosphomolybdic acid and thiocarbamide are according to Mo:S molar ratio is 1:4, be successively dissolved in deionized water stir 1-2 hours obtain
The mixed solution of phosphomolybdic acid and thiocarbamide;In mixed solution, per cm2Carbon cloth corresponding to phosphomolybdic acid addition scope be
0.0135mM-0.08mM, by adjusting MoS2The amount being supported on carbon cloth prepares a series of electrocatalytic hydrogen evolution materials;It is preferred that
0.04mM。
Molybdenum disulfide prepared by the present invention is grown on carbon cloth, is evenly distributed.It is made compared to more traditional synthetic method
Molybdenum disulfide nano size it is small, defect is enriched, and interlamellar spacing is wide, so improve electrocatalytic hydrogen evolution activity.
Brief description of the drawings
Fig. 1 is prepared MoS2The XRD diffraction spectrograms of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction agent of/CC.
Fig. 2 is prepared MoS2The microscopic appearance of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction agent of/CC.(a, b) MoS2/ CC scanning electron microscope (SEM) photographs
(SEM);(c) MoS2/CC field emission scanning electron microscopes figure (FESEM);(d)MoS2Transmission electron microscope picture (TEM);(e) MoS2 height is clear
Penetrate electron microscope (HRTEM);(f)MoS2Energy dispersion X-ray figure (EDX).
Fig. 3 electrocatalysis materials of the present invention are in acidity (0.5M H2SO4) in hydrogen evolution activity.(a)MoS2/ CC is in 0.5M
H2SO4In polarization curve;(b) the Tafel slopes corresponding to (a).
Hydrogen evolution activity of Fig. 4 electrocatalysis materials of the present invention under different pH.(a)MoS2/ CC is in 0.5M H2SO4,1M KOH,
Polarization curve in 0.5M PBS;(b) the Tafel slopes corresponding to (a).
Embodiment
The preparation of 1 molybdenum disulfide of embodiment/carbon cloth composite catalyst
Weigh 582.7mg phosphomolybdic acids and 1165.3mg thiocarbamides and be successively dissolved in 46ml deionized waters and stir 1-2 hours and obtain
Mixed solution, 4ml, 6ml, 12ml, 24ml is then taken (to be respectively labeled as MoS respectively2/CC-1,MoS2/CC-2,MoS2/CC-3,
MoS2/ CC-4) solution move into 50ml reactors in, be then diluted to 30ml respectively.Carbon cloth is placed in ultrasound in solution, makes solution
Soak carbon cloth completely, hydro-thermal naturally cools to room temperature after 24 hours under 180 degrees celsius, products therefrom is spent successively from
Sub- water and ethanol are cleaned, filtering, are positioned in vacuum drying chamber 60 degrees Celsius and are dried 8 hours.
The MoS of embodiment 22The phenetic analysis of/CC composite catalysts
As shown in figure 1, as can be seen from the figure there is MoS2With the diffraction maximum of carbon cloth, other dephasigns, and MoS are had no2's
(002) peak corresponding to crystal face is transferred to 9.8 °, illustrates that the molybdenum disulfide interlamellar spacing that we obtain broadens.
As shown in Fig. 2 it can be seen that molybdenum disulfide is uniformly raw on carbon cloth from figure a, b.Figure d can be seen that curing
Molybdenum nanometer sheet about 100-150nm, e figure are it can be seen that molybdenum disulfide is rich in many defects, and to can see interlamellar spacing wide for embedding figure
About 0.75-0.82nm.
As shown in figure 3, MoS is apparent that in figure2/ CC composite electrocatalysts have excellent electro-catalysis in acidity
Hydrogen Evolution Performance.MoS2/ CC-3 electrocatalytic hydrogen evolution activity highest.
As shown in figure 4, it can be seen that MoS in figure2/ CC composite electrocatalysts all have good in acid, neutral, alkalescence
Electrocatalytic hydrogen evolution performance.Electrocatalytic hydrogen evolution activity highest in acidity.
The MoS of embodiment 32The electrocatalytic hydrogen evolution activity experiment of/CC composite catalysts
Using three-electrode system to MoS2The electrocatalytic hydrogen evolution performance of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction materials of/CC is tested, with
For graphite rod to be reference electrode to electrode, saturated calomel electrode (SCE), catalyst is working electrode;Tester is Shanghai occasion
Magnificent CHI 760e type electrochemical workstations;Test the H that solution is 0.5mol/L2SO4Solution, 0.5mol/L sodium phosphate buffer are molten
Liquid, 1mol/L KOH solution.
Test parameter:LSV sweeps fast 5mV/s when testing.
In electrocatalytic hydrogen evolution the performance test results such as Fig. 3 of the composite electro catalytic liberation of hydrogen material of the present invention in acidity, MoS2/
The electrocatalytic hydrogen evolution reaction of CC-3 composite electro catalytic liberation of hydrogen materials plays peak overpotential minimum, reaches 94mV, MoS2/ CC-1 plays peak
Overpotential reaches 128mV, MoS2/ CC-2 plays peak overpotential and reaches 110mV, MoS2/ CC-4 plays peak overpotential and reaches 120mV, physics
Mix MoS2/ CC plays peak overpotential and reaches 130mV;When current density is 10mA/cm2When, MoS2/ CC-3 composite electro catalytic liberations of hydrogen
The test overpotential of material reaches 160mV.
MoS of the present invention2/ CC-3 composite electro catalytic liberation of hydrogen materials are in acidity, neutral, the electrocatalytic hydrogen evolution performance survey in alkalescence
In test result such as Fig. 4, MoS2The electrocatalytic hydrogen evolution of/CC-3 composite electro catalytic liberation of hydrogen materials is reacted in 10mA/cm2Under current density
Test overpotential it is acid, it is neutral, respectively reach 160mV, 230mV, 188mV in alkalescence.
Claims (4)
- A kind of 1. preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth, it is characterised in that:Regular shape will be cut into The carbon cloth cleaning of shape, is placed in after drying in the mixed solution of phosphomolybdic acid and thiocarbamide, and ultrasound causes mixed solution to soak carbon cloth completely, Then by carbon cloth and mixed solution in being transferred in reactor, hydro-thermal naturally cools to room after 24 hours under 180 degrees celsius Temperature, by washing, centrifugation, it is dried to obtain MoS2/ CC composite catalysts.
- 2. a kind of preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth as claimed in claim 1, its feature exist In:Described regular shape refers to 1cm × 2cm size identical rectangles;The cleaning refers to successively in acetone, ethanol and deionized water It is middle to be cleaned by ultrasonic 10min respectively.
- 3. a kind of preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth as claimed in claim 1, its feature exist In:The phosphomolybdic acid and thiocarbamide are according to Mo:S molar ratio is 1:4, be successively dissolved in deionized water stir 1-2 hours obtain phosphorus molybdenum The mixed solution of acid and thiocarbamide;In mixed solution, per cm2Carbon cloth corresponding to phosphomolybdic acid addition scope be 0.0135mM- 0.08mM, by adjusting MoS2The amount being supported on carbon cloth prepares a series of electrocatalytic hydrogen evolution materials.
- 4. a kind of preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth as claimed in claim 3, its feature exist In:In mixed solution, per cm2Carbon cloth corresponding to phosphomolybdic acid addition scope be 0.04mM.
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Cited By (25)
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CN108281297A (en) * | 2018-01-29 | 2018-07-13 | 广东工业大学 | A kind of preparation method and applications of polyaniline-coated molybdenum disulfide flexible electrode |
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