CN108671943A - A kind of micron of slot structure accelerates the application of bubble spilling in electrode evolving hydrogen reaction - Google Patents
A kind of micron of slot structure accelerates the application of bubble spilling in electrode evolving hydrogen reaction Download PDFInfo
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- CN108671943A CN108671943A CN201810449531.7A CN201810449531A CN108671943A CN 108671943 A CN108671943 A CN 108671943A CN 201810449531 A CN201810449531 A CN 201810449531A CN 108671943 A CN108671943 A CN 108671943A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 44
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000001257 hydrogen Substances 0.000 title claims abstract description 34
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 40
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims description 13
- 238000011065 in-situ storage Methods 0.000 claims description 12
- 238000006555 catalytic reaction Methods 0.000 claims description 9
- 238000012512 characterization method Methods 0.000 claims description 5
- 230000004927 fusion Effects 0.000 abstract description 27
- 239000007772 electrode material Substances 0.000 abstract description 13
- 239000007789 gas Substances 0.000 abstract description 12
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 229910052982 molybdenum disulfide Inorganic materials 0.000 abstract description 6
- 230000000737 periodic effect Effects 0.000 abstract description 5
- 238000002493 microarray Methods 0.000 abstract description 3
- 230000005587 bubbling Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- 230000009257 reactivity Effects 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 230000010287 polarization Effects 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 4
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 235000018660 ammonium molybdate Nutrition 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000007910 cell fusion Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- -1 thio ammonium molybdate Chemical compound 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- 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
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- 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
- 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
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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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
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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)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
A kind of micron of slot structure accelerates the application of bubble spilling in electrode evolving hydrogen reaction, belongs to inorganic advanced technical field of nano material.The influence of bubbling behaviour during the periodic size micrometer structure that material surface has reacts gas evolution.It includes the molybdenum disulfide array electrode that surface has different groove sizes, and different influences is generated to Bubble behavior in gas evolution reaction.The invention further relates to the wellabilities that the surface has the electrode material of different groove size microarrays.The electrode material of surface controlled dimensions microarray is applied to evolving hydrogen reaction by the present invention, promotes to react being rapidly separated for bubble by promoting the fusion phenomenon of bubble, the more reactivity sites of exposure promote catalytic performance.The protrusion of the present invention is 10 μm, and groove is respectively 40 μm of material, and Bubble surface size is 50~70 μm, is greatly reduced the detachment frequency of bubble, improves catalytic performance.
Description
Technical field
The invention belongs to inorganic advanced technical field of nano material, are related to a kind of micron of slot structure in electrode evolving hydrogen reaction
The application more particularly to a kind of surface for accelerating bubble spilling have the electrode material of periodic micrometer slot structure in evolving hydrogen reaction
Application.
Background technology
The electrocatalytic reaction that gas participates in is that the gas molecule of charge driving is the catalysis reaction of product or raw material.It generates
Object is that the electrocatalytic reaction of gas is referred to as bubbing reaction.How to improve the catalytic performance of electrocatalytic reaction is to be concerned
The problem of, nowadays researcher is mainly to improve catalytic performance by finding novel catalysis material.In journal article
Ultrahigh Hydrogen Evolution Performance of Under-Water“Superaerophobic”
MoS2Nanostructured Electrodes, DOI:10.1002/adma.201304759 proposing for gas evolution
Reaction, the bubble of generation into guild are seriously adhered to electrode surface with reaction, this is that bubbing reaction is common existing
Problem.The adherency of bubble can cause the active site of electrode surface to greatly reduce, while electrolyte can not touch electrode material
Surface, prevent reaction further generation.The solution direction of currently the majority is all the chemical composition by catalyst itself
Start with, the catalyst of synthesizing new；How to start with from the morphosis of material surface, design size it is controllable, suitably urge
Change the sticking problem that material surface structure solves bubble, is the another quantum jump progress for improving catalyst performance.
Invention content
It is an object of the invention to provide a kind of direction of new optimization electrode material catalytic performance in view of the above problems, lead to
It crosses electrode surface size controllably to design to improve catalytic performance, that is, finding an electrode surface, there is micro groove structure can pass through adjusting
Size allows the bubble generated in evolving hydrogen reaction to overcome by the surface energy that fusion phenomenon discharges viscous with substrate material surface
(this adhesive attraction cuts continuous three-phase line of contact originally due to the presence of material surface micrometer structure, discontinuously for attached effect
Three-phase line of contact so that adhesion strength is reduced) may be implemented that electrode surface can be rapidly separated under the size of very little, avoid bubble
It largely is adhered to material surface, to promote electrocatalysis characteristic.
A kind of micron of slot structure accelerates the application of bubble spilling in electrode evolving hydrogen reaction, which is characterized in that in electrode table
Face prepares the molybdenum sulfide catalysis material of the micron grooves lattice structure equipped with periodicity arrangement.
The molybdenum sulfide catalysis material of the micron grooves lattice structure of periodicity arrangement is that molybdenum sulfide only forms micron grooves grid
The protrusion of lattice structure, bottom portion of groove are electrode material, and bottom portion of groove does not have molybdenum sulfide.
The molybdenum sulfide catalysis material of the micron grooves lattice structure of periodicity arrangement carries out hydrophilic modifying, such as uses
Plasma is surface-treated.
The micron grooves lattice structure ledge width of periodicity arrangement is 10 μm, and recess width is 20-80 μm；It is raised high
5-10 μm of degree.It includes preparing periodic molybdenum sulfide (in the used method of the prior art) based on capillary microscopic model method that it, which is prepared,
(the periodic structure size on such as surface is that protrusion is constant respectively to catalysis material, is 10 μm；Groove is 20 μm respectively, 40 μm, 60
μm and 80 μm, can accordingly be represented sequentially as 10/20 μm, 10/40 μm, 10/60 μm and 10/80 μm).
Size is overflowed by adjusting recess width adjustment bubble, overflows speed so as to adjust bubble.
Under constant current, captured in real-time characterization evolving hydrogen reaction in situ generates the action process of bubble.Constant current is preferably
2mA。
Compared with the existing technology, the present invention achieves following advantageous effect：
1, promote to merge between bubble by using the quantitative controllable design of material surface micrometer structure in the present invention
Phenomenon, total surface area reduces while total volume is constant after bubble fusion during this, discharges certain surface energy, can overcome
The adhesive attraction of bubble and substrate, while adhesive attraction here is due to the presence of micrometer structure, the continuous three-phase of cutting script
Contact line, it is a degree of to reduce adhesion strength, to which bubble can leave electrode surface with smaller size.This mode can compare
Bubble is individually grown until volume increase makes itself suffered buoyancy increase realize disengaging electrode surface more to overcome adhesion strength
Efficiently.It obtains a kind of new mode and is overflowed in the electrode surface the phenomenon that accelerate bubble in gas evolution reaction, avoid bubble tight
The problem of adhering to again.
2, the present invention can be such that bubble in evolving hydrogen reaction realizes by the microflute size of quantitatively regulating and controlling electrode surface to study
It is precipitated with the size of very little after rapid fusion, to promote the catalytic performance of electrode.The electrode material for being 10/20 μm for size,
Most of air bubble growth, will be closer due to separation to 50 μm or so, promotes that fusion phenomenon occurs.If individually only leaning on bubble
It grows alone and is detached from electrode surface until volume increase, most of bubble will grow into 100 μm or so and can be only achieved bigger
Buoyancy overcome adhesion strength, to being detached from catalyst surface.Although but this size is the problem is that some bubble meetings
Fusion phenomenon occurs, but since the surface energy of the too small bubble fusion release of volume is not enough to overcome adhesive attraction, occurs the
Electrode surface can be trapped in after Single cell fusion phenomenon, continued growth is until leave electrode surface, or continue to melt with adjacent bubbles
It closes and leaves electrode surface.
3, by two key factors of balance influence Bubble electrode surface gas is precipitated in evolving hydrogen reaction in the present invention
The diameter and bubble of bubble and the adhesion strength of electrode surface analyze the relationship of the two factors and material surface groove size, find
One for size that evolving hydrogen reaction is optimal material surface microflute.It is analysis that the size of surface periodic pattern, which is 10/40 μm,
The optimal selection of hydrogen reaction is compared after the same terms processing with the material of other three sizes, and possessing lower adhesion strength is
14.1 μ N can make bubble that electrode surface be precipitated with smaller size, and about 60 μm or so i.e. protrusion is 10 μm, and groove is 40 μm
Material, Bubble surface diameter size be 50~70 μm.Compared to the material of other three sizes, tool in evolving hydrogen reaction
There is most fast cathode current to increase speed for 0.32mA mV-1。
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photo figure of the material prepared in embodiments of the present invention.A, b, c, d are 10/ successively
The surface micro-structure of the electrode material of 20 μm, 10/40 μm, 10/60 μm and 10/80 μm 4 different cycles sizes.
Fig. 2 is the EDS Elemental redistributions test for preparing material in embodiments of the present invention, observes that Mo and S are completely distributed
In the position of raised rib, and do not have substantially in groove.
Fig. 3 is morphology characterization figure of four size materials under video camera in the embodiment of the present invention.Station meter is amplification
150 μm under multiple.A, b, c, d are 10/20 μm, 10/40 μm, 10/60 μm and 10/80 μm successively.
Fig. 4 is adhesion strength and capture bubble contact angle of four various sizes of materials after hydrophilic treated in the embodiment of the present invention
Test.Adhesion strength is 32 μ N successively, 14.1 μ N, 12.5 μ N and 5.8 μ N, capture bubble contact angle be respectively 148 °, 147 °, 149 ° and
148°.A, b, c, d are 10/20 μm, 10/40 μm, 10/60 μm and 10/80 μm successively.
Fig. 5 is in the embodiment of the present invention 1 in 10/20 μm of electrode Bubble row in evolving hydrogen reaction of video camera in-situ observation
To indicate bubble nucleating growth, fusion and the state that electrode surface is precipitated successively.Station meter：150μm.
Fig. 6 is in the embodiment of the present invention 2 in 10/40 μm of electrode Bubble row in evolving hydrogen reaction of video camera in-situ observation
To indicate bubble nucleating growth, fusion and the state that electrode surface is precipitated successively.Station meter：150μm
Fig. 7 is in the embodiment of the present invention 3 in 10/60 μm of electrode Bubble row in evolving hydrogen reaction of video camera in-situ observation
To indicate bubble nucleating growth, fusion and the state that electrode surface is precipitated successively.Station meter：150μm
Fig. 8 is that in 10/80 μm of sample electrode of video camera in-situ observation, bubble is analysed in evolving hydrogen reaction in the embodiment of the present invention 4
Trip is to indicate bubble nucleating growth, fusion and the state that electrode surface is precipitated successively.Station meter：150μm
Fig. 9 is the polarization curve of 4 different size electrodes in the embodiment of the present invention, and wherein size is 10/40 μm of electrode material
The electric current of material is increased speed maximum.
Figure 10 is the diameter and sample of bubble in the evolving hydrogen reaction of four different size materials in the embodiment of the present invention
The relational graph of the adhesion strength on product surface and the groove size of sample surfaces, size are that 10/40 μm of sample is that best HER is electric
Pole.
Specific implementation mode
The present invention will be described in further detail with reference to the accompanying drawings and examples, it should be appreciated that implements in detail below
Example is only used for illustrating the present invention, without limiting the scope of the invention in any way.
1, it is 2mA in constant current, there are four various sizes of surface tiny array electrodes to generate gas for the tool of observation in real time in situ
The difference of the pick-up behavior of bubble.
2, under shooting in situ, the shadow that the electrode with different size micrometer structures merges bubble and is precipitated is observed
It rings, the rule that diameter is presented with the change of surface groove size when statistics large result obtains Bubble electrode surface.
In preferred embodiments, constant current chooses 2mA, the speed of Bubble can be preferably controlled, at this
The bubble generated under a current value can be more prone to shoot and observe pick-up behavior.
In preferred embodiments, in order to balance light-inletting quantity, clarity and dynamic shooting effect, in shooting bubble
In the dynamic process of precipitation, 4 various sizes of materials, set microscope magnification is different, but station meter
It is 150 μm under current multiple.
Embodiment 1
It is 10 μm that protrusion, which will be carried, and groove is incited somebody to action after 20 μm of silicon chip carries out silicic acid anhydride with the PTFE solution of 1wt%
Basic liquid is 10 with curing agent mass ratio:The PDMS of 1 proportioning, which is cast in, to be carved on figuratum silicon chip, and 60 DEG C of oven drying continues
6 hours, the PDMS film peeled carried the pattern opposite with die size.Hydrochloric acid is used after the titanium sheet of 2cm*2cm is flattened,
Absolute ethyl alcohol is cleaned by ultrasonic with deionized water.By predecessor 50mg four thio ammonium molybdates, the DMF solution of 5mL, 30 points of ultrasound is added
Clock.It will be placed in titanium sheet substrate, four thio ammonium molybdate solution be dripped along groove direction, due to hair with figuratum PDMS films
The effect of thin power, solution are flowed into groove, are then freeze-dried.After PDMS films are taken off, 170 DEG C of tube furnace calcining, 30
Minute.It is 10 μm that size of the surface with cyclic array, which be can be obtained, as protrusion, and groove is 20 μm of molybdenum disulfide electrode material
Expect (method forefathers made above used).The scanning electron microscope of resulting materials is referring to (a) in attached drawing 1, the video camera table on surface
Figure is levied referring to (a) in attached drawing 3, hydrophilicity-imparting treatment (being surface-treated with plasma, radio-frequency power 100W, time 30s) infiltrates afterwards
Property characterization include capture bubble contact angle and adhesion strength test chart referring to (a) in attached drawing 4, adhesion strength is compared to other sizes reason bigger than normal
The micrometer structure surface of size is smaller to the cutting degree of three-phase line of contact thus.It is in constant current 2mA, in-situ observation bubble row
It is procedure chart referring to attached drawing 5, is followed successively by bubble nucleating growth, fusion phenomenon, the table discharged after fusion occur for the bubble of adjacent ribs
Face can overcome adhesive attraction to be detached from electrode surface three phases.It counts mass data and obtains, most air bubble growth to 40
After~60 μm, fusion phenomenon will occur.And when fusion phenomenon does not occur, most of bubble will grow into 90~
100 μm of buoyancy that can be only achieved bigger overcome adhesion strength, to be detached from catalyst surface.The polarization curve of its evolving hydrogen reaction is joined
See attached drawing 9.
Embodiment 2
The method in embodiment 1 is participated in, using being 10 μm with protrusion, groove is 40 μm of silicon chip, prepares surface tool
The size of cyclic array is that protrusion is 10 μm, and groove is 40 μm of molybdenum disulfide electrode material.The scanning electricity of resulting materials
Mirror is referring to (b) in attached drawing 1, and the video camera phenogram on surface is referring to (b) in attached drawing 3, and wellability characterizes after hydrophilicity-imparting treatment
Including capture bubble contact angle and adhesion strength test chart referring to (b) in attached drawing 4, adhesion strength is subtracted compared to the material in embodiment 1
It is few, the reason is that the material surface of this size increases the cutting degree of three-phase line of contact.It is in constant current 2mA, in-situ observation gas
Action process figure is steeped referring to attached drawing 6, is followed successively by bubble nucleating growth, adjacent ribs bubble occurs fusion phenomenon, discharged after fusion
Surface energy overcomes adhesive attraction to be detached from electrode surface three phases.It counts the analysis of mass data and obtains, most bubble
After growing into 50~70 μm, fusion phenomenon will occur.And when fusion phenomenon does not occur, most of bubble will be grown
The buoyancy that can be only achieved bigger to 80~100 μm overcomes adhesion strength, to be detached from catalyst surface.The polarization of its evolving hydrogen reaction
Curve show that the material current of this size is increased speed maximum referring to attached drawing 9.Diameter, the surface adhesion of its bubble
The relational graph of power and groove size is referring to attached drawing 10, it can be deduced that this size is the most preferred microarray sizes of evolving hydrogen reaction.
Embodiment 3
The method in embodiment 1 is participated in, using being 10 μm with protrusion, groove is 60 μm of silicon chip, prepares surface tool
The size of cyclic array is that protrusion is 10 μm, and groove is 60 μm of molybdenum disulfide electrode material.The scanning electricity of resulting materials
Mirror is referring to (c) in attached drawing 1, and the video camera phenogram on surface is referring to (c) in attached drawing 3, and wellability characterizes after hydrophilicity-imparting treatment
Including capture bubble contact angle and adhesion strength test chart referring to (c) in attached drawing 4, adhesion strength is compared to the material in Examples 1 and 2
It reduces, the reason is that the material surface of this size increases the cutting degree of three-phase line of contact.It is in constant current 2mA, in-situ observation
Bubbling behaviour procedure chart is followed successively by bubble nucleating growth referring to attached drawing 7, and adjacent ribs bubble occurs fusion phenomenon, discharged after fusion
Surface energy overcome adhesive attraction be detached from electrode surface three phases.It counts the analysis of mass data and obtains, most gas
After bubble grows into 70~90 μm, fusion phenomenon will occur.And when fusion phenomenon does not occur, most of bubble will give birth to
The buoyancy that 120~140 μm can be only achieved bigger is grown to overcome adhesion strength, to be detached from catalyst surface.Its evolving hydrogen reaction
Polarization curve is referring to attached drawing 9.
Embodiment 4
The method in embodiment 1 is participated in, using being 10 μm with protrusion, groove is 80 μm of silicon chip, prepares surface tool
The size of cyclic array is that protrusion is 10 μm, and groove is 80 μm of molybdenum disulfide electrode material.The scanning electricity of resulting materials
Mirror is referring to (d) in attached drawing 1, and the video camera phenogram on surface is referring to attached drawing 3 (d), wellability characterization packet after hydrophilicity-imparting treatment
Capture bubble contact angle is included with adhesion strength test chart referring to attached drawing 4 (d), adhesion strength is subtracted compared to the material in embodiment 1,2 and 3
It is few, the reason is that the material surface of this size increases the cutting degree of three-phase line of contact.It is in constant current 2mA, in-situ observation gas
Action process figure is steeped referring to attached drawing 8, is followed successively by bubble nucleating growth, adjacent ribs bubble occurs fusion phenomenon, discharged after fusion
Surface energy overcomes adhesive attraction to be detached from electrode surface three phases.It counts the analysis of mass data and obtains, most bubble
After growing into 90~110 μm, fusion phenomenon will occur.And when fusion phenomenon does not occur, most of bubble will give birth to
The buoyancy that 140~160 μm can be only achieved bigger is grown to overcome adhesion strength, to be detached from catalyst surface.Its evolving hydrogen reaction
For polarization curve referring to attached drawing 9, catalytic performance is worst.
Claims (8)
1. a kind of micron of slot structure accelerates the application of bubble spilling in electrode evolving hydrogen reaction, which is characterized in that in electrode surface
Prepare the molybdenum sulfide catalysis material of the micron grooves lattice structure equipped with periodicity arrangement.
2. a kind of micron of slot structure described in accordance with the claim 1 accelerates the application of bubble spilling in electrode evolving hydrogen reaction,
It is characterized in that, the molybdenum sulfide catalysis material of the micron grooves lattice structure of periodicity arrangement is that molybdenum sulfide only forms micron grooves grid
The protrusion of lattice structure, bottom portion of groove do not have molybdenum sulfide.
3. a kind of micron of slot structure described in accordance with the claim 1 accelerates the application of bubble spilling in electrode evolving hydrogen reaction,
It is characterized in that, the molybdenum sulfide catalysis material of the micron grooves lattice structure of periodicity arrangement is hydrophilic using ultraviolet light progress
It is modified.
4. a kind of micron of slot structure described in accordance with the claim 1 accelerates the application of bubble spilling in electrode evolving hydrogen reaction,
It is characterized in that, the micron grooves lattice structure ledge width of periodicity arrangement is 10 μm, and recess width is 20-80 μm；Protrusion
5-10 μm of height.
5. a kind of micron of slot structure described in accordance with the claim 1 accelerates the application of bubble spilling in electrode evolving hydrogen reaction,
It is characterized in that, overflows size by adjusting recess width adjustment bubble, overflow speed so as to adjust bubble.
6. a kind of micron of slot structure described in accordance with the claim 1 accelerates the application of bubble spilling in electrode evolving hydrogen reaction,
It is characterized in that, under constant current, captured in real-time characterization evolving hydrogen reaction in situ generates the action process of bubble.
7. a kind of micron of slot structure accelerates the application of bubble spilling in electrode evolving hydrogen reaction according to claim 6,
It is characterized in that, constant current 2mA.
8. a kind of micron of slot structure accelerates the application of bubble spilling in electrode evolving hydrogen reaction according to claim 7,
It is characterized in that, protrusion is 10 μm, the material that groove is 40 μm, and Bubble surface diameter size is 50~70 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810449531.7A CN108671943B (en) | 2018-05-11 | 2018-05-11 | Application of micron groove structure in accelerating bubble overflow in electrode hydrogen evolution reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810449531.7A CN108671943B (en) | 2018-05-11 | 2018-05-11 | Application of micron groove structure in accelerating bubble overflow in electrode hydrogen evolution reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108671943A true CN108671943A (en) | 2018-10-19 |
| CN108671943B CN108671943B (en) | 2020-06-26 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110133093A (en) * | 2019-06-11 | 2019-08-16 | 北京化工大学 | A kind of porous electrode working performance comprehensive tester and test method and purposes |
| CN113355689A (en) * | 2021-05-07 | 2021-09-07 | 北京仿生界面科学未来技术研究院 | Qinqi-dispelling and qi-dispelling cooperative confinement electrode and preparation method thereof |
| CN114134528A (en) * | 2021-10-21 | 2022-03-04 | 中国空间技术研究院 | Micron array electrode structure, preparation method and application thereof |
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| CN105483751A (en) * | 2015-12-08 | 2016-04-13 | 天津市大陆制氢设备有限公司 | Efficient Ni-S-Mo hydrogen evolution electrode and preparation method thereof |
| CN105483744A (en) * | 2015-11-30 | 2016-04-13 | 苏州大学 | Porous hydrogen evolution catalyst, preparation method of porous hydrogen evolution catalyst and electrode containing hydrogen evolution catalyst |
| CN107557806A (en) * | 2017-08-28 | 2018-01-09 | 天津市大陆制氢设备有限公司 | A kind of Co O high efficiency composition hydrogen-precipitating electrodes being covered on Co Mo O and preparation method thereof |
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| CN105483744A (en) * | 2015-11-30 | 2016-04-13 | 苏州大学 | Porous hydrogen evolution catalyst, preparation method of porous hydrogen evolution catalyst and electrode containing hydrogen evolution catalyst |
| CN105483751A (en) * | 2015-12-08 | 2016-04-13 | 天津市大陆制氢设备有限公司 | Efficient Ni-S-Mo hydrogen evolution electrode and preparation method thereof |
| CN107557806A (en) * | 2017-08-28 | 2018-01-09 | 天津市大陆制氢设备有限公司 | A kind of Co O high efficiency composition hydrogen-precipitating electrodes being covered on Co Mo O and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110133093A (en) * | 2019-06-11 | 2019-08-16 | 北京化工大学 | A kind of porous electrode working performance comprehensive tester and test method and purposes |
| CN110133093B (en) * | 2019-06-11 | 2020-10-02 | 北京化工大学 | Comprehensive tester for working performance of porous electrode, testing method and application |
| CN113355689A (en) * | 2021-05-07 | 2021-09-07 | 北京仿生界面科学未来技术研究院 | Qinqi-dispelling and qi-dispelling cooperative confinement electrode and preparation method thereof |
| CN113355689B (en) * | 2021-05-07 | 2023-03-31 | 北京蕴超仿生智能科技发展有限公司 | Qinqi-dispelling and qi-dispelling cooperative confinement electrode and preparation method thereof |
| CN114134528A (en) * | 2021-10-21 | 2022-03-04 | 中国空间技术研究院 | Micron array electrode structure, preparation method and application thereof |
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