CN106702450B - Mix cuprous oxide bilayer liberation of hydrogen optoelectronic pole and the preparation of the modification of phase tungsten sulfide - Google Patents
Mix cuprous oxide bilayer liberation of hydrogen optoelectronic pole and the preparation of the modification of phase tungsten sulfide Download PDFInfo
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- CN106702450B CN106702450B CN201611186402.0A CN201611186402A CN106702450B CN 106702450 B CN106702450 B CN 106702450B CN 201611186402 A CN201611186402 A CN 201611186402A CN 106702450 B CN106702450 B CN 106702450B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/50—Processes
- C25B1/55—Photoelectrolysis
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- C—CHEMISTRY; METALLURGY
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- 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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- 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
- C25B11/093—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 at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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 kind of the cuprous oxide bilayer liberation of hydrogen optoelectronic poles and preparation method of the modification of mixing phase tungsten sulfide.The electrode is using FTO glass as substrate, the cuprous film layer of deposited oxide thereon, and the thickness of film layer is 0.8 1.0 μm, is mixing phase tungsten sulfide film layer on the film layer, mixing phase is by 2H WS2With 1T WS2It constitutes, the thickness of the film layer is 0.2 0.4 μm, and the mass ratio of two film layers is 1:0.15~0.30.Preparation method includes the electro-deposition preparation Cu on FTO glass2O films, to WS2Intercalation removes to obtain M WS2Solution, by Cu2O films are in M WS2Mixing phase tungsten sulfide film layer is made in solution.The electrode decomposes water for photoelectrocatalysis and prepares hydrogen.It is an advantage of the current invention that preparation process is simple, obtained electrode is without precious metal, and cost is relatively low, and photoelectricity liberation of hydrogen is efficient.
Description
Technical field
The present invention relates to a kind of the cuprous oxide bilayer liberation of hydrogen optoelectronic poles and preparation method of the modification of mixing phase tungsten sulfide, belong to
In optoelectronic pole technical field.
Background technology
Energy shortage is the Tough questions faced 21st century, and finding the sustainable and clean energy can not only solve
The various social concerns certainly caused by energy shortage, can also reduce the environmental pollution caused by combustion of fossil fuel.It is photoelectrochemical
It is an emerging energy technology to learn liberation of hydrogen technology, and photoelectric conversion process and electrolysis hydrogen process are combined by it, can be by the sun
It can be converted into electric energy, and the electric energy is further used for by electrolysis water by liberation of hydrogen catalyst and prepares hydrogen, there is prodigious development
It is latent.
Cuprous oxide（Cu2O）It is a kind of typical p-type direct semiconductor, energy gap only has ~ 2.0 eV, is for number
Few can be by the semi-conducting material of excited by visible light, the nanometer Cu made of this material2O films can not only be carried significantly
The utilization ratio of high solar energy, and since its manufacturing cost is very low, have the foreground of industrialized production, therefore in solar energy
There is prodigious application potential in terms of utilization.However pure Cu2O has the shortcomings that following two as photochemical catalyst：（1）By
Light excitation generate electrons and holes be easy catalyst surface occur it is compound be converted into thermal energy, to reduce the light of catalytic process
Photoelectric transformation efficiency or hydrogen output；（2）Due to Cu2Cu in O is intermediate valence state（+1）, it is oxidized easily so that catalyst
Preservation it is more difficult, be easy to happen photoetch and reduce the reactivity of catalyst.
In Cu2Liberation of hydrogen catalyst is added on the surface of O, and such as noble metal gold, silver, platinum etc. can not only play the role of protective layer,
Enhance its anti-oxidant and anti-light corrosive power, electron acceptor can also be played, it can be by the excitation state on semiconductor conduction band
Electronics transfer keeps the efficiency of photoelectric conversion process also big to precious metal surface to achieve the purpose that promote hole-electron separation
It is big to improve, still, since noble metal cost is higher, limit its scale application.Tungsten sulfide（WS2）Due to special two
Layer structure is tieed up, and preparation method is easy, cost is relatively low, receives the concern of more and more researchers.The WS of stratiform2With two
The relatively stable phase of kind, is the 2H- WS with semiconductor property respectively2With the 1T- WS with metalline2, wherein 1T-
WS2Electrolysis hydrogen activity it is higher, and can be by commercialized WS2Solid powder carries out lithium intercalation processing preparation.With WS2
Semiconductor light-catalyst is modified instead of noble metal as liberation of hydrogen catalyst, cheap and efficient liberation of hydrogen photoelectricity can be obtained
Pole.
There has been no see the cuprous oxide bilayer liberation of hydrogen optoelectronic pole report in relation to being modified with tungsten sulfide at present.
Invention content
The purpose of the present invention is to provide a kind of mixing phase tungsten sulfides（M-WS2）The cuprous oxide of modification（Cu2O）It is double-deck
（M-WS2/Cu2O）Liberation of hydrogen optoelectronic pole and preparation method thereof.The liberation of hydrogen optoelectronic pole has prepares the efficient of hydrogen for electrolysis water
The characteristics of, preparation process is simple, at low cost.
The present invention is to be realized by the following technical programs.A kind of cuprous oxide of mixing phase tungsten sulfide modification is double
Hydrogen optoelectronic pole is chromatographed, the liberation of hydrogen optoelectronic pole is with the stannic oxide glass of Fluorin doped（FTO glass）For working electrode, Ag/AgCl makees
For reference electrode, platinum plate electrode is used as to electrode, which is characterized in that in stannic oxide glass is electro deposition oxidation on working electrode
The thickness of cuprous film layer, cuprous oxide film layer is 0.8-1.0 μm, is by with semiconductor on cuprous oxide film layer
The phase 2H- WS of property2 With the phase 1T- WS with metalline2Phase is in mass ratio（0.5-0.25）：（0.5-0.75）
The mixing phase tungsten sulfide of composition（M-WS2）The thickness of film layer, mixing phase tungsten sulfide film layer is 0.2~0.4 μm,
In, cuprous oxide film layer is 1 with the mass ratio for mixing phase tungsten sulfide film layer:0.15~0.30.
Above-mentioned mixing phase tungsten sulfide（M-WS2）The cuprous oxide of modification（Cu2O）It is double-deck（M-WS2/Cu2O）Liberation of hydrogen light
The preparation method of electrode, it is characterised in that including following procedure：
（1）Electro-deposition prepares Cu2O film photoelectric electrodes
With NaOH aqueous solutions by molar ratio be 1:1 Cu2SO4PH value adjusting with the mixed aqueous solution of trisodium citrate is arrived
10.8~11.5, in temperature 60oC~70oUnder C, by the stannic oxide glass of Fluorin doped（FTO glass）As working electrode, Ag/
AgCl is used as reference electrode and platinum plate electrode to electrode, and 0.5~2h is deposited under the conditions of -0.4V vs Ag/AgCl and is prepared
Cu2O film photoelectric electrodes；
（2）Intercalation removes WS2
By WS2Solid powder is added in Shrek pipe, in the inert gas environment of argon gas or nitrogen, by every gram of WS2It is required
N-BuLi is 0.2~0.8 gram, and the hexane solution of the n-BuLi of a concentration of 2.4 mol/l is added into Shrek pipe,
Temperature 60oC~70oAfter reacting 20h~60h under C, filters, water dissolution obtained solid is used in combination；It is then centrifuged for removing unstripped WS2
To get to contain mixing phase tungsten sulfide（M-WS2）Aqueous solution, wherein with metalline phase 1T-WS2Mass fraction
It is 50%~75%；
（3）The cuprous oxide for mixing the modification of phase tungsten sulfide is double-deck（M-WS2/Cu2O）The preparation of liberation of hydrogen optoelectronic pole
By step（2）It is obtained to contain mixing phase tungsten sulfide（M-WS2）Concentration of aqueous solution adjusts most 0.2 mg/mL,
In temperature 20~25oUnder C, with dipping-pulling method, by step（1）Cu obtained2O film photoelectrics pole surface is first immersed in the M-
WS2Then 8~10min in aqueous solution is that 30cm/s lifts out liquid level with speed, such dipping-lifting 5~10 times is mixed
The cuprous oxide for closing the modification of phase tungsten sulfide is double-deck（M-WS2/Cu2O）Liberation of hydrogen optoelectronic pole.
Mixing phase tungsten sulfide prepared by the above method（M-WS2）The cuprous oxide of modification（Cu2O）The double-deck liberation of hydrogen optoelectronic pole
Using in the aqueous sodium persulfate solution of 0.5M, photoelectrocatalysis decomposes water and prepares hydrogen, in 1.5 light sources of AM, 100 mW/ of light intensity
cm2Under the bias condition of 0.4V vs RHE, overpotential of hydrogen evolution is 0.08 ~ 0.09V vs RHE, and liberation of hydrogen rate is 9-10 μ
mol/h。
The advantage of the invention is that：The double-deck liberation of hydrogen optoelectronic pole made from this method, without precious metal, cost is relatively low, and
Preparation process is simple, and photoelectricity liberation of hydrogen is efficient.Tungsten sulfide（WS2）It is to study more liberation of hydrogen co-catalyst recently, there is uniqueness
Two-dimensional structure can obtain single layer or the nano-lamellar structure of multilayer after removing its intercalation, and can be by it from tool
There are the 2H- WS of semiconductor property2Phase is changed into 1T- WS with metallic character2Phase, the WS after stripping and phase transition2,
Its electrocatalytic hydrogen evolution activity greatly improves.Stripping conditions are controlled, prepares and contains 2H- WS simultaneously2With 1T- WS2Mix phase WS2
Nanostructure, and use it to modification Cu2O optoelectronic poles can significantly improve photoelectric conversion efficiency due to the generation of p-n heterojunction,
The WS of phase is mixed simultaneously2As efficient liberation of hydrogen catalyst, the effect that photoelectric current prepares hydrogen for electrolysis water can also be improved
Rate.
Description of the drawings
Fig. 1 is electro-deposition Cu2The SEM of O schemes；
Fig. 2 is the mixing phase WS after stripping2TEM figure；
Fig. 3 is mixing phase WS2High-resolution TEM figure, which shows 2H- WS2With 1T- WS2The lattice of two kinds of phases
Amplify appearance.
Specific implementation mode
Embodiment 1
Prepare CuSO4（0.05M）And trisodium citrate（0.05M）Mixed solution 50mL, then use 1M NaOH solutions will
Its pH value is adjusted to 11.0, and the mixed solution is heated to 65 using oil bathoC, then by FTO（1cm×2cm）Glass is as work
Make electrode, Ag/AgCl is used as reference electrode, platinum plate electrode to electrode electro-deposition 2 under the conditions of -0.4V vs Ag/AgCl
H prepares Cu2O film photoelectric electrodes.Weigh 2.38 g solids WS2（9.6 mM）Powder pours into the history of the 50ml of the drying equipped with magneton
In the pipe of Lake, air in tube is replaced using argon gas, the hexane solution of the n-BuLi of 6ml 2.4M is then added, after sealing
Utilize oil bath heating to 66oC, sustained response is for 24 hours.It filters, dries up product with argon gas, deionized water is added, then exists
Under the conditions of 14000rpm, it is centrifuged off unstripped solid WS2, you can obtain M-WS2Aqueous solution, 1T- WS2Account for mixing phase
Tungsten sulfide（M-WS2）For 50wt%.By the M-WS after stripping2Aqueous solution solubility is adjusted to 0.2 mg/mL, then using impregnating-carry
Daraf(reciprocal of farad) is by M-WS2It is supported on Cu2O membrane electrodes surface prepares the double-deck liberation of hydrogen optoelectronic pole（M-WS2/Cu2O）, electricity is dried up using nitrogen
This is extremely repeated afterwards impregnates-lifting process 5 times, gained Cu2O and M-WS2Mass ratio be 1:0.15.Using the optoelectronic pole as work
Electrode, platinum plate electrode is as working electrode, with 0.5M Na2SO4Solution is as electrolyte, overpotential of hydrogen evolution 0.08-0.09V
Vs RHE, and in 1.5 illumination conditions of AM（100 mW/cm2）, under the bias condition of -0.4V vs RHE, liberation of hydrogen rate is 9-
10 μmol/h。
Embodiment 2
Prepare Cu2SO4（0.06M）And trisodium citrate（0.06M）Mixed solution 50mL, then use 1M NaOH solutions will
Its pH value is adjusted to 11.0, and the solution is heated to 65 using oil bathoC, then by FTO（1cm×2cm）Glass is as work electricity
Pole, for Ag/AgCl as reference electrode, platinum plate electrode is used as to electrode electro-deposition 1.5h under the conditions of -0.4V vs Ag/AgCl
Prepare Cu2O film photoelectric electrodes.Weigh 2.38g solids WS2（6μm）Powder pours into the history of the clean anhydrous 50ml equipped with magneton
In the pipe of Lake, air in tube is replaced using argon gas, the hexane solution of the n-BuLi of 8ml 2.4M is then added, after sealing
Reactant is heated to 66 using oil bathoC, sustained response 30h.It filters, after drying up product with argon gas, deionized water is added, so
Afterwards under the conditions of 14000rpm, it is centrifuged off unstripped WS2, you can obtain M-WS2（1T- WS2Mass percent is 55%）.
By the M-WS after stripping2Aqueous solution solubility is adjusted to 0.2 mg/mL, then utilizes dipping-pulling method by M-WS2It is supported on Cu2O
Membrane electrode surface prepares the double-deck liberation of hydrogen optoelectronic pole（M-WS2/Cu2O）, it is dried up with argon gas after repeated impregnations-lifting process 10 times,
Obtain Cu2O and M-WS2Mass ratio be 1:0.18 M-WS2/Cu2O optoelectronic poles.Using the optoelectronic pole as working electrode, platinized platinum
Electrode is as working electrode, with 0.5M Na2SO4For solution as electrolyte, overpotential of hydrogen evolution is 0.085V vs RHE, and
1.5 illumination conditions of AM（100 mW/cm2）, under the bias condition of -0.4V vs RHE, liberation of hydrogen rate is 10 μm of ol/h.
Embodiment 3
Prepare Cu2SO4（0.08M）And trisodium citrate（0.08M）Mixed solution 50mL, then use 1M NaOH solutions will
Its pH value is adjusted to 11.0, and the solution is heated to 65 using oil bathoC, then by FTO（1cm×2cm）Glass is as work electricity
Pole, for Ag/AgCl as reference electrode, platinum plate electrode is used as to electrode electro-deposition 1h systems under the conditions of -0.4V vs Ag/AgCl
Standby Cu2O film photoelectric electrodes.Weigh 2.38g solids WS2（6μm）Powder pours into the clean anhydrous Shrek pipe equipped with magneton
（50ml）In, air in tube is replaced using argon gas, the hexane solution of the n-BuLi of 10ml 2.4M is then added, after sealing
Utilize oil bath heating to 66oC continues 36h.It filters, dries up product with argon gas, deionized water is added, then in 14000rpm items
Under part, it is centrifuged off unstripped WS2, you can obtain mixing phase WS2（1T- WS2Mass fraction is 65%）.After stripping
Mix phase WS2Aqueous solution solubility is adjusted to 0.2 mg/mL, then utilizes dipping-pulling method by M-WS2It is supported on Cu2O films
Electrode surface prepares M-WS2/Cu2It is sub- to obtain oxidation by being dried up with argon gas after dipping-lifting 15 times for O bilayer liberation of hydrogen optoelectronic poles
The mass ratio of copper and tungsten sulfide is 1:The 0.2 double-deck liberation of hydrogen optoelectronic pole（M-WS2/Cu2O）.Using the optoelectronic pole as working electrode,
Platinum plate electrode is as working electrode, with 0.5M Na2SO4For solution as electrolyte, overpotential of hydrogen evolution is 0.09V vs RHE, and
In 1.5 illumination conditions of AM（100 mW/cm2）, under the bias condition of -0.4V vs RHE, liberation of hydrogen rate is 9 μm of ol/h.
Embodiment 4
Prepare Cu2SO4（0.1M）And trisodium citrate（0.1M）Mixed solution 50mL, then use 1M NaOH solutions by its
PH value is adjusted to 11.0, utilizes oil bath heating solution to 65oC, then by FTO（1cm×2cm）Glass is as working electrode, Ag/
For AgCl as reference electrode, platinum plate electrode is used as electro-deposition 45min preparations under the conditions of -0.4V vs Ag/AgCl to electrode
Cu2O film photoelectric electrodes.Weigh 2.38g solids WS2（6μm）Powder pours into the clean anhydrous Shrek pipe equipped with magneton（50ml）
In, air in tube is replaced using argon gas, the hexane solution of the n-BuLi of 15ml 2.4M is then added, oil is utilized after sealing
Bath is heated to 66oC, sustained response 48h.It filters, after drying up product with argon gas, deionized water is added, then in 14000rpm items
Under part, it is centrifuged off unstripped WS2, you can obtain mixing phase WS2（1T- WS2Mass fraction is 75%）.After stripping
Mix phase WS2Aqueous solution solubility is adjusted to 0.2 mg/mL, then utilizes dipping-pulling method by M-WS2It is supported on Cu2O films
Electrode surface prepares M-WS2/Cu2O bilayer liberation of hydrogen optoelectronic poles are dried up after repeated impregnations-lifting process 20 times with argon gas, are obtained
Cu2O and M-WS2Mass ratio be 1:The 0.25 double-deck liberation of hydrogen optoelectronic pole（M-WS2/Cu2O）.Using the optoelectronic pole as work electricity
Pole, platinum plate electrode is as working electrode, with 0.5M Na2SO4For solution as electrolyte, overpotential of hydrogen evolution is 0.08V vs
RHE, and in 1.5 illumination conditions of AM（100 mW/cm2）, under the bias condition of -0.4V vs RHE, liberation of hydrogen rate is 9.5 μ
mol/h。
Claims (3)
1. a kind of cuprous oxide bilayer liberation of hydrogen optoelectronic pole of mixing phase tungsten sulfide modification, the liberation of hydrogen optoelectronic pole is with the two of Fluorin doped
Tin oxide glass is working electrode, and for Ag/AgCl as reference electrode, platinum plate electrode is used as carries out electrolytic preparation to electrode, special
Sign is, is the cuprous film layer of electro deposition oxidation on working electrode in stannic oxide glass, the thickness of cuprous oxide film layer is
0.8~1.0 μm, be by the phase 2H-WS with semiconductor property on cuprous oxide film layer2With the phase with metalline
State 1T-WS2Phase is in mass ratio（0.5-0.25）：（0.5-0.75）The mixing phase tungsten sulfide film layer of composition mixes phase
The thickness of tungsten sulfide film layer is 0.2~0.4 μm, wherein cuprous oxide film layer and the matter for mixing phase tungsten sulfide film layer
Amount is than being 1:0.15~0.30.
2. the preparation method of the cuprous oxide bilayer liberation of hydrogen optoelectronic pole of mixing phase tungsten sulfide modification as described in claim 1,
It is characterized by comprising following procedure：
（1）Electro-deposition prepares Cu2O film photoelectric electrodes
With NaOH aqueous solutions by molar ratio be 1:1 Cu2SO4It is adjusted to 10.8 with the pH value of the mixed aqueous solution of trisodium citrate
~11.5, in temperature 60oC~70oUnder C, using the stannic oxide glass of Fluorin doped as working electrode, Ag/AgCl as reference electricity
Pole and platinum plate electrode are used as to electrode, and 0.5~2h is deposited under the conditions of -0.4VvsAg/AgCl and prepares Cu2O film photoelectric electrodes；
（2）Intercalation removes WS2
By WS2Solid powder is added in Shrek pipe, in the inert gas environment of argon gas or nitrogen, by every gram of WS2Required positive fourth
Base lithium is 0.2~0.8 gram, the hexane solution of the n-BuLi of a concentration of 2.4mol/l is added into Shrek pipe, in temperature
60oC~70oAfter reacting 20h~60h under C, filters, water dissolution obtained solid is used in combination；It is then centrifuged for removing unstripped WS2, i.e.,
The aqueous solution containing mixing phase tungsten sulfide is obtained, wherein the 1T-WS with metalline phase2Mass fraction be 50%~
75%；
（3）Mix the preparation of the cuprous oxide bilayer liberation of hydrogen optoelectronic pole of phase tungsten sulfide modification
By step（2）It is obtained to adjust most 0.2mg/mL containing mixing phase tungsten sulfide concentration of aqueous solution, in temperature 20~25oC
Under, with dipping-pulling method, by step（1）Cu obtained2O film photoelectrics pole surface is first immersed in containing mixing phase tungsten sulfide
Then 8~10min in aqueous solution is that 30cm/s lifts out liquid level with speed, such dipping-lifting 5~10 times obtains mixed phase
The cuprous oxide bilayer liberation of hydrogen optoelectronic pole of state tungsten sulfide modification.
3. by the cuprous oxide bilayer liberation of hydrogen optoelectronic pole application of claim 2 method mixing phase tungsten sulfide modification obtained,
In the aqueous sodium persulfate solution of 0.5M, photoelectrocatalysis decomposes water and prepares hydrogen, in AM1.5 light sources, light intensity 100mW/cm2With
Under the bias condition of 0.4VvsRHE, overpotential of hydrogen evolution is 0.08 ~ 0.09VvsRHE, and liberation of hydrogen rate is 9~10 μm of ol/h.
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