CN110523418A - Graphene/preparation method of molybdenum sulfide composite aerogel elctro-catalyst and its method of inspection of electrocatalytic hydrogen evolution performance - Google Patents
Graphene/preparation method of molybdenum sulfide composite aerogel elctro-catalyst and its method of inspection of electrocatalytic hydrogen evolution performance Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 73
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 46
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000004964 aerogel Substances 0.000 title claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000001257 hydrogen Substances 0.000 title claims abstract description 36
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000007689 inspection Methods 0.000 title claims abstract description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 36
- 238000012360 testing method Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000000017 hydrogel Substances 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 238000004502 linear sweep voltammetry Methods 0.000 claims description 10
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 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 description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000002484 cyclic voltammetry Methods 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000005518 electrochemistry Effects 0.000 claims description 5
- 239000005416 organic matter Substances 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920000557 Nafion® Polymers 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001453 impedance spectrum Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000002441 reversible effect Effects 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 3
- 239000010439 graphite Substances 0.000 abstract description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 abstract description 2
- 229940010552 ammonium molybdate Drugs 0.000 abstract description 2
- 235000018660 ammonium molybdate Nutrition 0.000 abstract description 2
- 239000011609 ammonium molybdate Substances 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- -1 Aluminum ions Chemical class 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052961 molybdenite Inorganic materials 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- PDMMFKSKQVNJMI-BLQWBTBKSA-N Testosterone propionate Chemical group C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H](OC(=O)CC)[C@@]1(C)CC2 PDMMFKSKQVNJMI-BLQWBTBKSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- 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
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
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Abstract
The present invention proposes a kind of graphene/preparation method of molybdenum sulfide composite aerogel elctro-catalyst and its method of inspection of electrocatalytic hydrogen evolution performance, compared with the prior art, prepared graphene/molybdenum sulfide composite aerogel raw materials are mainly thiocarbamide, ammonium molybdate, graphite etc., material therefor is conveniently easy to get；Preparation process is simple, at low cost, pollutes the environment small compared with conventional method；Prepared graphene/molybdenum sulfide composite aerogel active site quantity is more, is conducive to the efficiency for improving electrocatalytic hydrogen evolution.
Description
Technical field
The present invention relates to the preparation fields of the catalyst of electrolysis water liberation of hydrogen, and it is compound especially to design a kind of graphene/molybdenum sulfide
The preparation method of aeroge elctro-catalyst and its method of inspection of electrocatalytic hydrogen evolution performance.
Background technique
Molecular hydrogen (H2) had always been considered as being energy carrier since early 1970s.Due to can the energy such as wind again
Can, water energy, the unstability of biomass energy may generate the extra energy that can not be connected to the grid in time, and by these energy
Source is with H2Form store, electric energy can be then converted to, be directly used as fuel, or be used as and maintain following " methanol economy "
Pillar, this will greatly promote the service efficiency of the energy.By H2It is desirable as energy carrier, because it is unit energy density
Highest molecule, when burning within the engine or becoming electric power in a fuel cell, it only produces water as byproduct.It compares
Under, carbon-based fuel generates water and carbon dioxide.Although hydrogen is the most abundant element on the earth, it is not as free molecular flow
It is existing, it is therefore desirable to effective and sustainable H2Production technology.Nowadays, most of H2It is the process that is converted by steam from change
It is generated in stone resource, steam and hydrocarbon reaction generate H2And CO2.This H2Production method consumption of fossil fuels and still
So discharge CO2.So cleaning and reproducible H2Production method is using renewable energy, especially solar energy electrolyzing water.Electrification
It learns water decomposition and is divided into two half-reactions: evolving hydrogen reaction (HER) and oxygen evolution reaction (OER).HER and OER require catalyst
Reduce electrochemical overpotential (difference applied between potential and thermodynamic electric potential that overpotential is given electrochemical reaction).Platinum family
Metal is the most effective catalyst of HER, can drive the significant electric current close to thermodynamics potential.However, these noble metals are ground
Rare element on ball, and extensive HER is realized in insufficient support, so the liberation of hydrogen catalyst of exploitation Cheap highly effective is imperative
's.
Summary of the invention
It is an object of the invention to propose a kind of economic, simple and efficiently graphene/molybdenum sulfide composite aerogel electricity
The preparation method of catalyst and its method of inspection of electrocatalytic hydrogen evolution performance.
In order to achieve the above objectives, the present invention proposes a kind of preparation side of graphene/molybdenum sulfide composite aerogel elctro-catalyst
Method, comprising the following steps:
Step 1: weighing ammonium heptamolybdate, thiocarbamide and aluminum nitrate；
Step 2: by the ammonium heptamolybdate, thiocarbamide and aluminum nitrate are dissolved in graphene oxide solution, obtain mixed solution；
Step 3: the mixed solution is placed in the reaction of reaction kettle high temperature；
Step 4: by the mixed solution natural cooling, obtaining compound hydrogel；
Step 5: washing the mixture hydrogel；
Step 6: being freeze-dried the mixture hydrogel and obtain composite aerogel catalyst.
Preferably, in step 2, the graphene oxide solution is to be prepared by graphite powder by Hummers method, described
The concentration of graphene oxide water solution is 2mg/mL；The capacity of the graphene oxide solution is 50ml.
Preferably, in step 2, the atomic ratio of molybdenum and sulphur is 1:5.
Preferably, in step 2, the amount of the aluminum nitrate is 0.5mmol, and the theoretical atomic ratio of aluminium and molybdenum is 7:100.
Preferably, the mass ratio of molybdenum sulfide and graphene is 95:5.
Preferably, in step 3, the mixed solution is placed in the reaction kettle of 50ml, 24 is reflected at a temperature of 180 degree
Hour.
Preferably, in steps of 5, practical alcohol and deionized water are washed described mixture hydrogel 5 times.
Preferably, in step 6, the mixture hydrogel is dried in vacuo 2 days at -90 DEG C, obtains composite aerogel
Catalyst.
The present invention also proposes a kind of inspection party of graphene/molybdenum sulfide composite aerogel catalyst electrocatalytic hydrogen evolution performance
Method, comprising the following steps:
Step 1: weighing composite aerogel catalyst and be scattered in isopropanol/water in the mixed solvent, obtain catalyst solution；
Step 2: the catalyst solution is placed in ultrasonic disperse in ultrasonic machine；
Step 3: the dissolved oxygen of the electrolyte in removal electrocatalytic hydrogen evolution test electrolytic cell, and removal catalyst surface
Organic matter and other impurities；
Step 4: by the catalyst solution be added dropwise in obtained on rotating circular disk glass-carbon electrode, and after drying have catalysis
The rotating disk electrode (r.d.e) of agent film；
Step 5: the electrochemistry Hydrogen Evolution Performance of the rotating disk electrode (r.d.e) is tested using standard three electrode system.
Preferably, in step 1, it weighs composite aerogel catalyst described in 4mg and is scattered in addition 30uL Nafion solution
1mL volume ratio be 5:1 the isopropanol/water in the mixed solvent.
Preferably, in step 3, with nitrogen purged solution half an hour to remove in electrocatalytic hydrogen evolution test electrolytic cell
The dissolved oxygen of electrolyte, and cyclic voltammetry test several times is carried out between 0V-0.8V to remove the catalyst surface
Organic matter and other impurities, by all potential converting potentials for relative to reversible hydrogen electrode.
Preferably, in step 4, the catalyst solution is taken out 14uL dropwise addition with liquid-transfering gun is being 5mm's for diameter
On the rotating circular disk glass-carbon electrode, spontaneously dries obtain within 1 hour the rotating circular disk with catalyst film at room temperature
Electrode.
Preferably, the step 5 the following steps are included:
Step 5.1: Xiang Suoshu rotating circular disk glass-carbon electrode application -0.23V potential, test 0.01-100000Hz frequency electricity
Chemical impedance spectrum, and solution resistance Rs is calculated from the electrochemical impedance spectroscopy picture；
Step 5.2: using the rotating disk electrode (r.d.e) to carry out linear sweep voltammetry (LSV) test as working electrode and obtain
To the LSV curve of the electrocatalytic hydrogen evolution of composite material.Tower Fil curve graph can also be obtained by the data for the LSV curve that converts；
Step 5.3: cyclic voltammetry test (CV) is carried out to the rotating disk electrode (r.d.e) with catalyst film；
Step 5.4: m- testing current (I-T) when being carried out to the rotating disk electrode (r.d.e) with catalyst film；
Compared with prior art, of the invention to be advantageous in that:
1. molybdenum sulfide/graphene composite aerogel raw materials prepared by are mainly thiocarbamide, ammonium molybdate, graphite etc.,
Material therefor is conveniently easy to get；
2. preparation process is simple, at low cost, pollute the environment small compared with conventional method；
3. molybdenum sulfide/graphene composite aerogel active site quantity prepared by is more, is conducive to improve electrocatalytic hydrogen evolution
Efficiency.
Detailed description of the invention
The XRD diagram (a) of Fig. 1 composite catalyst, Raman spectrum (b) and 0.5Al-G5M95, G5M95 and pure MoS2FTIR light
It composes (c), the MoS of one pot of hydrothermal synthesis Al doping2With the schematic diagram (d) of GA composite aerogel.
The pure GA (a) of Fig. 2, pure MoS2 (b), the scanning electron microscope image of G5M95 (c) and 0.5Al-G5M95 (d).
Fig. 3 catalyst 0.5Al-G5M95Transmission electron microscope (TEM) (a, b) and high-resolution projection electron microscope
(HRTEM) (c) image, EDS map (d), and Mo element is yellow, and S element is purple, and C element is red, and Al element is blue) and N
Element is green.Scheme the upper right corner a and is inserted into selective electron diffraction (SAED) pattern.
Fig. 4 catalyst 0.5Al-G5M95And G5M95XPS spectrum comparison (a) and Al 2p position partial enlarged view (b),
0.5Al-G5M95Mo 3d (c), S 2p (d), C 1s (d), O 1s (e) Al 2p (f) and N 1s (g) high-resolution deconvolution
XPS spectrum figure.
MoS after synthesis of the Fig. 5 with different GA contents (a) and with different Al ion doping concentration (b)2The compound gas of@GA
The LSV curve of gel catalyst, corresponding Tafel figure (c) and EIS spectrogram (d).
Fig. 6 catalyst 0.5Al-G5M95Cyclical stability (a) and current versus time curve figure (b).
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be made below into
Illustrate to one step.
The present invention proposes a kind of preparation method of graphene/molybdenum sulfide composite aerogel elctro-catalyst, comprising the following steps:
Step 1: weighing ammonium heptamolybdate, thiocarbamide and aluminum nitrate；
Step 2: by ammonium heptamolybdate, thiocarbamide and aluminum nitrate are dissolved in graphene oxide solution, obtain mixed solution；
Step 3: mixed solution is placed in the reaction of reaction kettle high temperature；
Step 4: by mixed solution natural cooling, obtaining compound hydrogel；
Step 5: washing mixture hydrogel；
Step 6: freeze drying mixture hydrogel obtains composite aerogel catalyst.
In the present embodiment, in step 2, graphene oxide solution is to be prepared by graphite powder by Hummers method, oxygen
The concentration of graphite aqueous solution is 2mg/mL；The volume of graphene oxide solution is 30ml.In order to prove in composite material really
Real storage is in graphene, and as shown in figure Fig. 1 b and Fig. 1 c, we have carried out Raman test and infrared test, composite wood to composite material
The Raman test result figure of material shows apparent D, oxygen-containing in the peak G and its infrared test, and nitrogen-containing functional group demonstrates multiple
The presence of graphene in condensation material.
In the present embodiment, in step 2, the atomic ratio of molybdenum and sulphur is 1:5.
In the present embodiment, in step 2, the amount of aluminum nitrate is 0.5mmol, and the theoretical atomic ratio of aluminium and molybdenum is 7:100.
Aluminum ions addition can cause the distortion of molybdenum sulfide lattice to improve the Hydrogen Evolution Performance of composite material, can see from Fig. 1 a
Aluminum ions introducing is so that the 2H phase content of molybdenum sulfide increases.In order to prove that Al-doping enters in composite material, Wo Menjin
Gone test x-ray photoelectron spectroscopy (XPS) test, as shown in figure 4, the doping of aluminium can be proven in XPS map really.
In the present embodiment, the mass ratio of molybdenum sulfide and graphene is 95:5, and the graphene aerogel of high-specific surface area was both
The exposed area that molybdenum sulfide can be improved can increase the defect of molybdenum sulfide again.As shown in figure 3, Flied emission projection electron microscope
Shown in the picture clapped, wherein there is a large amount of defect in graphene nano on piece in the nanometer sheet vertical-growth of molybdenum sulfide,
And these defects contribute to improve the electrocatalytic hydrogen evolution performance of the composite material.
In the present embodiment, in step 3, mixed solution is placed in the reaction kettle of 50ml, is reacted at a temperature of 180 degree
24 hours, the reaction temperature of 180 degree was advantageously formed with more defects, the more molybdenum sulfide nanometers of active edge site exposure
Piece.In addition, 240 degree of preparation temperatures relative to traditional molybdenum sulfide, the reaction temperature of 180 degree can also be formed make molybdenum sulfide from
2H phase transition is the better 1T phase of electric conductivity.As shown in Figure 1a, all occur the molybdenum sulfide of 1T phase in composite material, and scheming
It can also be seen that the interplanar distance of 2H phase molybdenum sulfide is the interplanar distance of (002) crystal face of 0.62nm and the molybdenum sulfide of 1T phase in 3
For (002) crystal face of 1nm.This all illustrates that the temperature of 180 degree is conducive to generate the molybdenum sulfide of the better 1T phase of electric conductivity, thus
Improve the electrocatalytic hydrogen evolution performance of composite material.
In the present embodiment, in steps of 5, it is washed mixture hydrogel 5 times using alcohol and deionized water.
In the present embodiment, in step 6, mixture hydrogel is dried in vacuo 2 days at -90 DEG C, obtains compound airsetting
Glue catalyst.As shown in Fig. 2, molybdenum sulfide is grown in conduct shown in the picture that the scanning electron microscope of middle composite material is clapped
On the graphene aerogel of carrier.
The present invention also proposes a kind of inspection party of graphene/molybdenum sulfide composite aerogel catalyst electrocatalytic hydrogen evolution performance
Method, comprising the following steps:
Step 1: weighing composite aerogel catalyst and be scattered in isopropanol/water in the mixed solvent, obtain catalyst solution；
Step 2: catalyst solution is placed in ultrasonic disperse in ultrasonic machine；
Step 3: the dissolved oxygen of the electrolyte in removal electrocatalytic hydrogen evolution test electrolytic cell, and removal catalyst surface
Organic matter and other impurities；
Step 4: catalyst solution being added dropwise thin with catalyst in being obtained on rotating circular disk glass-carbon electrode, and after drying
The rotating disk electrode (r.d.e) of film；
Step 5: using the electrochemistry Hydrogen Evolution Performance of standard three electrode system test rotating disk electrode (r.d.e).
In the present embodiment, in step 1, weigh 4mg composite aerogel catalyst be scattered in be added 30uL Nafion it is molten
The 1mL volume ratio of liquid is the isopropanol/water in the mixed solvent of 5:1.
In the present embodiment, in step 3, with nitrogen purged solution half an hour to remove electrocatalytic hydrogen evolution test electrolysis
The dissolved oxygen of electrolyte in pond, and cyclic voltammetry test several times is carried out between 0V-0.8V to remove catalyst surface
Organic matter and other impurities, by all potential converting potentials for relative to reversible hydrogen electrode.
In the present embodiment, in step 4, catalyst solution is taken out 14uL and be added dropwise in diameter with liquid-transfering gun is 5mm's
On rotating circular disk glass-carbon electrode, 1 hour rotating disk electrode (r.d.e) for obtaining that there is catalyst film is spontaneously dried at room temperature.
In the present embodiment, step 5 the following steps are included:
Step 5.1: to rotating circular disk glass-carbon electrode application -0.23V potential, testing 0.01-100000Hz frequency electrochemistry
Impedance spectrum, and solution resistance Rs is calculated from electrochemical impedance spectroscopy picture, as fig 5d；
Step 5.2: using the rotating disk electrode (r.d.e) to carry out linear sweep voltammetry (LSV) test as working electrode and obtain
To the LSV curve of the electrocatalytic hydrogen evolution of composite material, as shown in Fig. 5 a and b.It can also be obtained by the data for the LSV curve that converts
Tower Fil curve graph, as shown in Figure 5 c；
Step 5.3: cyclic voltammetry test (CV) being carried out to the rotating disk electrode (r.d.e) with catalyst film, such as
Shown in Fig. 6 a；
Step 5.4: m- testing current (I-T) when being carried out to the rotating disk electrode (r.d.e) with catalyst film, such as
Shown in Fig. 6 b；
The above is only a preferred embodiment of the present invention, does not play the role of any restrictions to the present invention.Belonging to any
Those skilled in the art, in the range of not departing from technical solution of the present invention, to the invention discloses technical solution and
Technology contents make the variation such as any type of equivalent replacement or modification, belong to the content without departing from technical solution of the present invention, still
Within belonging to the scope of protection of the present invention.
Claims (13)
1. a kind of graphene/molybdenum sulfide composite aerogel elctro-catalyst preparation method, which comprises the following steps:
Step 1: weighing ammonium heptamolybdate, thiocarbamide and aluminum nitrate；
Step 2: by the ammonium heptamolybdate, thiocarbamide and aluminum nitrate are dissolved in graphene oxide solution, obtain mixed solution；
Step 3: the mixed solution is placed in the reaction of reaction kettle high temperature；
Step 4: by the mixed solution natural cooling, obtaining compound hydrogel；
Step 5: washing the mixture hydrogel；
Step 6: being freeze-dried the mixture hydrogel and obtain composite aerogel catalyst.
2. graphene according to claim 1/molybdenum sulfide composite aerogel elctro-catalyst preparation method, feature exist
In in step 2, the graphene oxide solution is to be prepared by graphite powder by Hummers method, the graphene oxide water
The concentration of solution is 2mg/mL；The volume of the graphene oxide solution is 30ml.
3. graphene according to claim 1/molybdenum sulfide composite aerogel elctro-catalyst preparation method, feature exist
In in step 2, the atomic ratio of molybdenum and sulphur is 1:5.
4. graphene according to claim 1/molybdenum sulfide composite aerogel elctro-catalyst preparation method, feature exist
In in step 2, the amount of the aluminum nitrate is 0.5mmol, and the theoretical atomic ratio of aluminium and molybdenum is 7:100.
5. graphene according to claim 1/molybdenum sulfide composite aerogel elctro-catalyst preparation method, feature exist
In the mass ratio of molybdenum sulfide and graphene is 95:5.
6. graphene according to claim 1/molybdenum sulfide composite aerogel elctro-catalyst preparation method, feature exist
In in step 3, the mixed solution is placed in the reaction kettle of 50ml, is reacted 24 hours at a temperature of 180 degree.
7. graphene according to claim 1/molybdenum sulfide composite aerogel elctro-catalyst preparation method, feature exist
In, in steps of 5, use alcohol and deionized water washing it is described mixture hydrogel 5 times.
8. graphene according to claim 1/molybdenum sulfide composite aerogel elctro-catalyst preparation method, feature exist
In in step 6, the mixture hydrogel is dried in vacuo 2 days at -90 DEG C, obtains composite aerogel catalyst.
9. a kind of graphene/molybdenum sulfide composite aerogel catalyst electrocatalytic hydrogen evolution performance method of inspection, is wanted using such as right
Seek graphene described in any one of 1-8/molybdenum sulfide composite aerogel elctro-catalyst, which comprises the following steps:
Step 1: weighing composite aerogel catalyst and be scattered in isopropanol/water in the mixed solvent, obtain catalyst solution；
Step 2: the catalyst solution is placed in ultrasonic disperse in ultrasonic machine；
Step 3: the dissolved oxygen of the electrolyte in removal electrocatalytic hydrogen evolution test electrolytic cell, and removal catalyst surface are organic
Object and other impurities；
Step 4: the catalyst solution being added dropwise thin with catalyst in being obtained on rotating circular disk glass-carbon electrode, and after drying
The rotating disk electrode (r.d.e) of film；
Step 5: the electrochemistry Hydrogen Evolution Performance of the rotating disk electrode (r.d.e) is tested using standard three electrode system.
10. graphene according to claim 9/molybdenum sulfide composite aerogel catalyst electrocatalytic hydrogen evolution performance inspection party
Method, which is characterized in that in step 1, weigh composite aerogel catalyst described in 4mg and be scattered in addition 30uL Nafion solution
1mL volume ratio be 5:1 the isopropanol/water in the mixed solvent.
11. graphene according to claim 9/molybdenum sulfide composite aerogel catalyst electrocatalytic hydrogen evolution performance inspection party
Method, which is characterized in that in step 3, with nitrogen purged solution half an hour to remove in electrocatalytic hydrogen evolution test electrolytic cell
The dissolved oxygen of electrolyte, and cyclic voltammetry test several times is carried out between 0V-0.8V to remove the catalyst surface
Organic matter and other impurities, by all potential converting potentials for relative to reversible hydrogen electrode.
12. the inspection of graphene according to claim 9/molybdenum sulfide composite aerogel catalyst electrocatalytic hydrogen evolution performance
Method, which is characterized in that in step 4, it is being 5mm's for diameter that the catalyst solution, which is taken out 14uL dropwise addition with liquid-transfering gun,
On the rotating circular disk glass-carbon electrode, spontaneously dries obtain within 1 hour the rotating circular disk with catalyst film at room temperature
Electrode.
13. graphene according to claim 9/molybdenum sulfide composite aerogel catalyst electrocatalytic hydrogen evolution performance inspection party
Method, which is characterized in that the step 5 the following steps are included:
Step 5.1: Xiang Suoshu rotating circular disk glass-carbon electrode application -0.23V potential tests 0.01-100000Hz frequency electrochemistry
Impedance spectrum, and solution resistance Rs is calculated from the electrochemical impedance spectroscopy picture；
Step 5.2: using the rotating disk electrode (r.d.e) to carry out linear sweep voltammetry (LSV) test as working electrode and answered
The LSV curve of the electrocatalytic hydrogen evolution of condensation material.Tower Fil curve graph can also be obtained by the data for the LSV curve that converts；
Step 5.3: cyclic voltammetry test (CV) is carried out to the rotating disk electrode (r.d.e) with catalyst film；
Step 5.4: m- testing current when being carried out to the rotating disk electrode (r.d.e) with catalyst film.
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