CN114990607A - Simple and efficient preparation method based on surface modification electrode - Google Patents
Simple and efficient preparation method based on surface modification electrode Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000012986 modification Methods 0.000 title claims abstract description 11
- 230000004048 modification Effects 0.000 title claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 24
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 claims abstract description 21
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006260 foam Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- 239000012266 salt solution Substances 0.000 claims abstract description 12
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 6
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910001863 barium hydroxide Inorganic materials 0.000 claims abstract description 6
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 6
- 239000011575 calcium Substances 0.000 claims abstract description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 6
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 6
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 6
- 239000011651 chromium Substances 0.000 claims abstract description 6
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 6
- 239000010941 cobalt Substances 0.000 claims abstract description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052802 copper Inorganic materials 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims abstract description 6
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 6
- 239000011733 molybdenum Substances 0.000 claims abstract description 6
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 6
- 239000011591 potassium Substances 0.000 claims abstract description 6
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 6
- 239000011734 sodium Substances 0.000 claims abstract description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- 239000011701 zinc Substances 0.000 claims abstract description 6
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000007772 electrode material Substances 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 238000003912 environmental pollution Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000010411 electrocatalyst Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
-
- 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
- C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
-
- 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
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
- C25B11/061—Metal or alloy
-
- 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)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Abstract
The application discloses a simple and efficient preparation method based on a surface modified electrode, which comprises the steps of firstly soaking foamed nickel molybdenum in acetone, then ultrasonically cleaning with hydrochloric acid, and finally cleaning with distilled water; secondly, placing the pretreated foam nickel-molybdenum electrode into an inorganic salt solution containing one of metal calcium, potassium, sodium, iron, zinc, copper, manganese, cobalt, molybdenum or chromium for reacting for a plurality of times, taking out, and drying at room temperature; and finally, placing the foamed nickel-molybdenum electrode into one alkali solution of potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, ammonium hydroxide, sodium carbonate or sodium bicarbonate to react for a certain time, taking out the electrode, drying the electrode at room temperature, finally cleaning the electrode by using ethanol and distilled water, and drying the electrode in an oven to prepare the simple and efficient electrode based on surface modification.
Description
Technical Field
The invention belongs to the technical field of electrocatalyst materials for hydrogen evolution and oxygen evolution, and particularly relates to a simple and efficient preparation method based on a surface modified electrode.
Background
Nowadays, more and more energy environmental issues become one of the huge challenges. The energy problem becomes a hot topic, and is closely connected with the environmental problems caused by the environment, such as global warming, acid rain, nuclear waste and the like, and the relationship between the energy and the environment is expanded to the benefit maximization so as to jointly maintain the environment. Hydrogen energy is a promising green energy source, and compared with a series of environmental pollution problems caused by dependence on fossil fuels, the hydrogen energy is converted into practical application, so that air and environmental pollution are remarkably reduced. Green trips which are publicized vigorously nowadays, such as electric cars; but also by wind or sun, etc. In pursuit of different ways of energy conversion, every industry is struggling with solutions to environmental pollution problems to improve the solution of these global threat factors, and the preparation of some efficient and economical electrocatalysts has played a crucial role in this, such as the production of hydrogen by electrolysis of water. The preparation of the electrode usually needs time and labor consumption, even certain economic cost is invested, and the maximization of economy needs to be considered emphatically, wherein the economy is not only the cost but also whether the whole set of procedures of the preparation early stage, the preparation process and the preparation end is energy-saving and green or not, and whether the real economy is achieved or not. In the invention, an economic and efficient preparation method is developed, the whole preparation is simple and quick, extra energy investment is not needed, and the final performance also shows a more optimistic trend, so that the preparation method is also an environment-friendly electrode material and provides a certain technical basis for the energy and environment problems in China.
Disclosure of Invention
The technical problem to be solved is as follows:
aiming at the defects of the prior art, the technical problems of environmental pollution and the like at present are solved, a simple and efficient preparation method based on the surface modified electrode is provided, the purpose is to develop a simple, economical, convenient and efficient surface modified electrode material for hydrogen evolution and oxygen evolution reaction of electrolyzed water, and a reference way worth of reference is developed for the problems of energy environmental pollution and shortage.
The technical scheme is as follows:
in order to achieve the purpose, the application is realized by the following technical scheme:
a simple and efficient preparation method based on a surface modification electrode specifically comprises the following steps:
firstly, pretreating foam nickel-molybdenum without any treatment: firstly, soaking foamed nickel-molybdenum in acetone for 1-35 minutes;
then ultrasonically washing the glass substrate for 1 to 30 minutes by using 1 to 6M hydrochloric acid, and finally cleaning the glass substrate by using distilled water;
secondly, putting the foamed nickel molybdenum obtained after the pretreatment in the first step into an inorganic salt solution for reaction: placing the pretreated foamed nickel-molybdenum electrode into 0.1-5M inorganic salt solution to react for 1-150 s, taking out, and drying at room temperature for 1-500 minutes;
and thirdly, placing the foamed nickel-molybdenum electrode into 0.1-5M alkali solution to react for 1-150 seconds, taking out, drying at room temperature for 1-500 minutes, finally cleaning with ethanol and distilled water, and drying at the temperature of a 60 ℃ drying oven to obtain the simple and efficient electrode based on surface modification.
Further, the acetone soaking time in the first step is 5min, 10min, 15min, 20min, 25min, 30min or 35 min.
Further, the ultrasonic cleaning time in the first step is 5min, 10min, 15min, 20min, 25min or 30 min.
Further, the concentration of hydrochloric acid in the first step is 1M, 2M, 3M, 4M, 5M or 6M.
Further, the inorganic salt solution in the second step is an inorganic salt solution containing metal calcium, potassium, sodium, iron, zinc, copper, manganese, cobalt, molybdenum or chromium.
Further, the reaction time in the second step is 1s, 3s, 5s, 10s, 15s, 25s, 30s, 45s, 60s, 80s, 90s, 105s, 120s, 135s, or 150 s.
Further, the drying time in the second step is 5min, 10min, 15min, 30min, 45min, 60min, 80min, 120min, 160min, 240min, 260min, 300min, 360min, 420min or 480 min.
Further, the alkali solution in the third step is potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, ammonium hydroxide, sodium carbonate or sodium bicarbonate solution.
Further, the reaction time in the third step is 1s, 3s, 5s, 10s, 15s, 25s, 30s, 45s, 60s, 80s, 90s, 105s, 120s, 135s, or 150 s.
Further, the drying time in the third step is 5min, 10min, 15min, 30min, 45min, 60min, 80min, 120min, 160min, 240min, 260min, 300min, 360min, 420min or 480 min.
The simple and efficient preparation method based on the surface modified electrode has the working principle that: and carrying out simple two-step experiments on different substrates, wherein the process is simple and economic, and no other extra consumption is caused, so that the optimal surface modified electrode material is obtained.
Has the advantages that:
compared with the prior art, the simple and efficient preparation method based on the surface modification electrode has the following beneficial effects:
1. the preparation method is simple and efficient, and no additional condition factors harmful to the environment are generated, so that the resources can be utilized to the maximum extent.
2. The preparation method provides inspiration and reference ways for preparing efficient and economical electrode materials in the field of electrocatalysis.
3. Compared with different electrode substrate materials which are not treated, the foamed nickel molybdenum is treated by the simple and efficient preparation method based on surface modification, and the performance is obviously improved.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the teachings of the present invention, and equivalents may also fall within the scope of the claims of the present application.
Example 1:
the simple and efficient preparation method based on the surface modification electrode material comprises the following steps:
firstly, soaking foamed nickel molybdenum in acetone for 1-35 minutes, then ultrasonically washing with 1-6M hydrochloric acid for 1-30 minutes, and finally cleaning with distilled water;
secondly, placing the pretreated foam nickel-molybdenum electrode into 0.1-5M of inorganic salt solution containing metal calcium, potassium, sodium, iron, zinc, copper, manganese, cobalt, molybdenum or chromium for reacting for 1-150 seconds, taking out, and drying at room temperature for 1-500 minutes;
and finally, placing the foamed nickel-molybdenum electrode into 0.1-5M potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, ammonium hydroxide, sodium carbonate or sodium bicarbonate to react for 1-150 seconds, taking out, drying at room temperature for 1-500 minutes, finally cleaning with ethanol and distilled water, and drying at the oven temperature of 60 ℃.
Example 2:
firstly, soaking foamed nickel in acetone for 1-35 minutes, then ultrasonically washing with 1-6M hydrochloric acid for 1-30 minutes, and finally, cleaning with distilled water;
secondly, placing the pretreated foam nickel electrode into 0.1-5M salt solution containing metal calcium, potassium, sodium, iron, zinc, copper, manganese, cobalt, molybdenum or chromium for reacting for 1-150 seconds, taking out, and drying at room temperature for 1-500 minutes;
and finally, placing the foamed nickel electrode into 0.1-5M potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, ammonium hydroxide, sodium carbonate or sodium bicarbonate to react for 1-150 seconds, taking out, drying at room temperature for 1-500 minutes, finally cleaning with ethanol and distilled water, and drying at the oven temperature of 60 ℃.
Example 3:
firstly, soaking the foam iron in acetone for 1-35 minutes, then ultrasonically washing the foam iron for 1-30 minutes by using 1-6M hydrochloric acid, and finally, cleaning the foam iron by using distilled water;
secondly, placing the pretreated foam iron electrode into 0.1-5M inorganic salt solution containing metal calcium, potassium, sodium, iron, zinc, copper, manganese, cobalt, molybdenum or chromium for reacting for 1-150 seconds, taking out, and drying at room temperature for 1-500 minutes;
and finally, placing the foam iron electrode into 0.1-5M potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, ammonium hydroxide, sodium carbonate or sodium bicarbonate to react for 1-150 seconds, taking out, drying at room temperature for 1-500 minutes, finally cleaning with ethanol and distilled water, and drying at the oven temperature of 60 ℃.
Comparative example 1:
this comparative example directly used foam nickel molybdenum without any treatment as the electrode.
Comparative example 2:
this comparative example directly used foamed nickel without any treatment as an electrode.
Comparative example 3:
this comparative example directly used foam iron without any treatment as an electrode.
Analysis of electrode catalytic performance:
and respectively carrying out hydrogen evolution and oxygen evolution electrocatalysis performance tests on the electrodes obtained in examples 1-3 and comparative examples 1-3 by adopting a linear voltammetry scanning test method. The test used a three-electrode system, the electrode obtained in this example was a working electrode, Hg/HgO (1 mol/L potassium hydroxide solution filled therein) was a reference electrode, Pt/C was a counter electrode, 1mol/L potassium hydroxide solution was used as the electrolyte, and the scanning rate was 5mV s -1 The scanning range is 0-1V. The electrocatalytic performance was tested on an electrochemical workstation (CHI 660E, shanghai chenhua instruments ltd) and the test results corresponded to tables 1 and 2.
TABLE 1 overpotential of hydrogen evolution reaction at certain current density for different test electrodes
TABLE 2. overpotential of oxygen evolution reaction at certain current density for different test electrodes
As can be seen from tables 1 and 2 above, the same experimental tests were carried out with different substratesThe obtained hydrogen evolution and oxygen evolution reactions are obviously improved, and particularly, the electrode material prepared by adopting foamed nickel molybdenum is 100mAcm -2 The overpotentials required for hydrogen evolution and oxygen evolution under the current density are 241 mV and 253 mV, respectively, 147 mV and 190 mV are reduced by the purer foam nickel-molybdenum electrode, obviously, the overpotentials are greatly improved, and meanwhile, the potential of the foam nickel-molybdenum electrode material with the best performance is increased by 4 mV and 3 mV after continuous hydrogen evolution and oxygen evolution reaction for 25 hours.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A simple and efficient preparation method based on a surface modified electrode is characterized by comprising the following steps:
firstly, foam nickel molybdenum without any treatment is pretreated: firstly, soaking foamed nickel-molybdenum in acetone for 1-35 minutes; then ultrasonically washing the substrate for 1 to 30 minutes by using 1 to 6M hydrochloric acid, and finally cleaning the substrate by using distilled water;
secondly, putting the foamed nickel molybdenum obtained after the pretreatment in the first step into an inorganic salt solution for reaction: placing the pretreated foamed nickel-molybdenum electrode into 0.1-5M inorganic salt solution to react for 1-150 s, taking out, and drying at room temperature for 1-500 minutes;
and thirdly, placing the foamed nickel-molybdenum electrode into 0.1-5M alkali solution to react for 1-150 seconds, taking out, drying at room temperature for 1-500 minutes, finally cleaning with ethanol and distilled water, and drying at the temperature of a 60 ℃ drying oven to obtain the simple and efficient electrode based on surface modification.
2. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: the acetone soaking time in the first step is 5min, 10min, 15min, 20min, 25min, 30min or 35 min.
3. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: the ultrasonic cleaning time in the first step is 5min, 10min, 15min, 20min, 25min or 30 min.
4. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: the concentration of hydrochloric acid in the first step is 1M, 2M, 3M, 4M, 5M or 6M.
5. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: the inorganic salt solution in the second step is an inorganic salt solution containing metal calcium, potassium, sodium, iron, zinc, copper, manganese, cobalt, molybdenum or chromium.
6. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: the reaction time in the second step is 1s, 3s, 5s, 10s, 15s, 25s, 30s, 45s, 60s, 80s, 90s, 105s, 120s, 135s or 150 s.
7. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: the drying time in the second step is 5min, 10min, 15min, 30min, 45min, 60min, 80min, 120min, 160min, 240min, 260min, 300min, 360min, 420min or 480 min.
8. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: and in the third step, the alkali solution is potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, ammonium hydroxide, sodium carbonate or sodium bicarbonate solution.
9. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: the reaction time in the third step is 1s, 3s, 5s, 10s, 15s, 25s, 30s, 45s, 60s, 80s, 90s, 105s, 120s, 135s or 150 s.
10. The simple and efficient surface-modified electrode-based preparation method according to claim 1, characterized in that: the drying time in the third step is 5min, 10min, 15min, 30min, 45min, 60min, 80min, 120min, 160min, 240min, 260min, 300min, 360min, 420min or 480 min.
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| CN113046775A (en) * | 2021-03-09 | 2021-06-29 | 南通大学 | Electrode based on dual effects of induction and sacrifice and preparation method thereof |
| CN114293215A (en) * | 2021-11-23 | 2022-04-08 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of cathode for hydrogen production by water electrolysis |
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| CN114293215A (en) * | 2021-11-23 | 2022-04-08 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of cathode for hydrogen production by water electrolysis |
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