CN115110112B - Industrial preparation method of nickel-molybdenum electrode and nickel-molybdenum electrode - Google Patents
Industrial preparation method of nickel-molybdenum electrode and nickel-molybdenum electrode Download PDFInfo
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- CN115110112B CN115110112B CN202210725694.XA CN202210725694A CN115110112B CN 115110112 B CN115110112 B CN 115110112B CN 202210725694 A CN202210725694 A CN 202210725694A CN 115110112 B CN115110112 B CN 115110112B
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- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 45
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 26
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 22
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 22
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 4
- 239000000956 alloy Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000011230 binding agent Substances 0.000 claims description 16
- 230000001680 brushing effect Effects 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 238000000498 ball milling Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000007605 air drying Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- 239000012670 alkaline solution Substances 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 9
- 229920000557 Nafion® Polymers 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 18
- 239000001257 hydrogen Substances 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005868 electrolysis reaction Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000000713 high-energy ball milling Methods 0.000 abstract description 3
- 229910001092 metal group alloy Inorganic materials 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000003795 desorption Methods 0.000 abstract description 2
- 150000004678 hydrides Chemical class 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract description 2
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 239000011733 molybdenum Substances 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 238000000967 suction filtration Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- VREFGVBLTWBCJP-UHFFFAOYSA-N alprazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1 VREFGVBLTWBCJP-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 229910002065 alloy metal Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910000474 mercury oxide Inorganic materials 0.000 description 1
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
- C25B11/052—Electrodes comprising one or more electrocatalytic coatings on a substrate
-
- 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
-
- 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
- C25B11/073—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
- C25B11/089—Alloys
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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)
- Catalysts (AREA)
Abstract
The invention discloses a method for industrially preparing a nickel-molybdenum electrode and the nickel-molybdenum electrode. The industrial preparation method of the nickel-molybdenum electrode adopts high-energy ball milling to alloy nickel-aluminum alloy powder and molybdenum powder, and provides a new direction for metal alloy industrialization; the process of removing aluminum increases the specific surface area of the material; the calcination process in the muffle furnace results in a stronger bond between the catalyst and the electrode substrate. When the nickel-molybdenum electrode prepared by the method is applied to hydrogen production by alkaline water electrolysis, adsorbed hydrogen atoms formed on the surface of nickel can overflow to the surface of molybdenum for compound desorption, so that hydrogen evolution overpotential is obviously reduced, energy consumption is further reduced, and hydride generation on the surface of nickel is avoided.
Description
Technical Field
The invention relates to the technical field of hydrogen production by water electrolysis, in particular to a method for industrially preparing a nickel-molybdenum electrode and the nickel-molybdenum electrode.
Background
The energy problem is always a problem of common attention all over the world, but renewable energy power generation meets the requirement of a double-carbon target, but has volatility, a medium is needed to store the fluctuating renewable energy, and the hydrogen energy has two properties of substances and energy, and can convert electric energy into hydrogen energy for storage and transportation in a mode of producing hydrogen by electrolyzing water. The alkaline water electrolysis hydrogen production technology is mature in technology and relatively low in cost, is an industrial water electrolysis hydrogen production technology widely adopted at present, is particularly important in electrode cost in the process of alkaline water electrolysis hydrogen production, can effectively reduce the energy consumption of water electrolysis hydrogen production by reducing the hydrogen evolution overpotential of a cathode, and is a high-efficiency hydrogen evolution electrode widely researched in recent years, and the nickel-molybdenum alloy has the advantages of wide source, low price and unique structure, but is not suitable for a technical method for nickel-molybdenum electrode production in industry. Therefore, there is a need for a method for industrially producing a nickel-molybdenum electrode.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the related art to some extent.
The aim of the invention is to provide a method for the industrial production of a nickel-molybdenum electrode and a nickel-molybdenum electrode. When the nickel-molybdenum electrode prepared by the industrial preparation nickel-molybdenum electrolysis method is applied to hydrogen production by alkaline electrolyzed water, adsorbed hydrogen atoms formed on the surface of nickel can overflow to the surface of molybdenum for compound desorption, so that hydrogen evolution overpotential is obviously reduced, energy consumption is further reduced, and hydride generation on the surface of nickel is avoided.
In one aspect, the invention provides a method for industrially preparing a nickel-molybdenum electrode, comprising the following steps:
(1) The mass ratio is 1: mixing 0.5-1 of nickel-aluminum alloy powder and molybdenum powder, and then ball milling;
(2) Placing the ball-milled sample in an alkaline solution to remove aluminum in the sample, filtering, cleaning and drying to obtain catalyst powder;
(3) The mass ratio is 3-6: 1, uniformly mixing the catalyst powder with the adhesive, and coating the mixture on an electrode substrate;
(4) And (3) placing the sample obtained in the step (3) in a muffle furnace, and calcining at 500-650 ℃ for 3-5h to obtain the nickel-molybdenum electrode.
In some embodiments, the nickel aluminum alloy powder and the molybdenum powder both have particle sizes of 325-800 mesh.
In some embodiments, the nickel in the nickel-aluminum alloy powder is 50% -80% by mass.
In some embodiments, the ball milling speed of the ball mill is 400-700r/min and the ball milling time is 1-3h.
In some embodiments, the alkaline solution is a NaOH solution or a KOH solution.
In some embodiments, the step (3) is performed by brushing the catalyst powder and the binder on the front and back surfaces of the electrode substrate after mixing, brushing again after air drying, and repeating brushing for 3-5 times.
In some embodiments, the electrode substrate is a nickel mesh, foam nickel, or nickel sheet.
In some embodiments, the binder is present in a volume ratio of 1:40 to 60 of Nafion solution and ethanol solution.
In some embodiments, the muffle furnace has a heating rate of 10-40 ℃/min.
In another aspect, the invention provides a nickel-molybdenum electrode prepared by the industrial preparation method of the nickel-molybdenum electrode.
Compared with the prior art, the invention has the beneficial effects that:
the industrial preparation method of the nickel-molybdenum electrode can alloy nickel-aluminum alloy powder and molybdenum powder by adopting high-energy ball milling, and provides a new direction for metal alloy industrialization.
The industrial preparation method of the nickel-molybdenum electrode ensures that the catalyst and the electrode substrate are combined more firmly through the calcination process of the sample in the muffle furnace.
The industrial preparation method of the nickel-molybdenum electrode increases the specific surface area of the material in the process of removing aluminum.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic drawing of LSV test curve of the electrode prepared in example 1;
FIG. 2 is a schematic representation of the Tafil slope of the electrode prepared in example 1.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
The method for industrially preparing a nickel-molybdenum electrode and the nickel-molybdenum electrode according to the embodiments of the present invention are described below with reference to the accompanying drawings.
The industrial preparation method of the nickel-molybdenum electrode comprises the following steps:
(1) The mass ratio is 1: mixing 0.5-1 of nickel-aluminum alloy powder and molybdenum powder, and then ball milling;
(2) Placing the ball-milled sample in an alkaline solution to remove aluminum in the sample, filtering, cleaning and drying to obtain catalyst powder;
(3) The mass ratio is 3-6: 1, uniformly mixing the catalyst powder and the adhesive, and coating the mixture on an electrode substrate;
(4) And (3) placing the sample obtained in the step (3) in a muffle furnace, and calcining at 500-650 ℃ for 3-5h to obtain the nickel-molybdenum electrode.
In the step (1), the particle sizes of the nickel-aluminum alloy powder and the molybdenum powder are 325-800 meshes, the mass fraction of nickel in the nickel-aluminum alloy powder is 50% -80%, the ball milling rotating speed of ball milling operation is 400-700r/min, and the ball milling time is 1-3h. The ball milling can be performed by a planetary ball mill. Compared with the traditional method, the high-energy ball milling method has the characteristics of low reaction temperature, high yield and uniform powder particle size distribution, can effectively alloy metals, and provides a new direction for metal alloy industrialization. The nickel-aluminum alloy powder and the molybdenum powder can be alloyed by ball milling after being mixed.
In the step (2), the alkaline solution is NaOH solution or KOH solution, and the mass fraction of the alkaline solution is 15% -25%. The ball-milled sample is placed in an alkaline solution for the purpose of reacting aluminum with the alkaline solution, so that aluminum in the alloy powder is dissolved, and pore forming is performed to increase the specific surface area of the material. It is understood that the specific conditions for obtaining the catalyst powder after filtration, washing and drying are determined according to the actual situation, so long as the effect of obtaining clean and dry catalyst powder can be achieved.
In the step (3), the electrode base material is nickel screen, foam nickel or nickel sheet; the volume ratio of the adhesive is 1: 40-60 of Nafion solution and ethanol solution; the coating is to brush the catalyst powder and the adhesive on the front and back surfaces of the electrode substrate after mixing, brush the electrode substrate again after air drying, and brush the electrode substrate repeatedly for 3-5 times. Firstly, uniformly mixing catalyst powder and an adhesive in a certain mass ratio, and then brushing the mixture on an electrode substrate; then air-drying is carried out until the liquid does not drip; and (5) carrying out brushing for the next time after air drying, and repeatedly operating for 3-5 times. It will be appreciated that the air drying time and temperature are related to the area of the substrate, and that the specific conditions are set according to the specific circumstances. In addition, automatic brushing equipment can be used in industry for brushing. The function of this step is to attach the catalyst to the electrode substrate to allow it to act as a catalyst.
In the step (4), the temperature rising rate of the muffle furnace is 10-40 ℃/min. The high temperature calcination of the sample in the muffle furnace makes the combination of the catalyst and the electrode substrate stronger.
The nickel-molybdenum electrode provided by the invention is prepared by the method for preparing the nickel-molybdenum electrode in the industry, and the nickel-molybdenum electrode prepared by the method can be applied to the hydrogen production process of alkaline electrolyzed water.
Example 1:
s1, mixing nickel-aluminum alloy powder and molybdenum powder in a mass ratio of 1:1, and then ball-milling for 2 hours by using a planetary ball mill at a rotating speed of 500r/min, wherein the mass fraction of nickel in the nickel-aluminum alloy powder is 60%, the particle size of the nickel-aluminum alloy powder is 400 meshes, and the particle size of the molybdenum powder is 400 meshes;
s2, placing the ball-milled sample in a NaOH solution with the mass fraction of 20% for 1h to remove aluminum in the sample, and filtering, cleaning and drying after the reaction is completed to obtain catalyst powder, wherein the specific filtering, cleaning and drying steps are that the filtering is carried out by a suction filtration device, the suction filtration is repeated for 10 times, and then the catalyst powder is placed in a blast drying box at 50 ℃ for drying;
s3, uniformly mixing catalyst powder and a binder in a mass ratio of 4:1 to form a catalyst binder mixture, and brushing the catalyst binder mixture on a nickel screen; then air-drying is carried out until the liquid does not drip; after air drying, carrying out brushing for the next time, and repeating the operation for 5 times, wherein the adhesive is a mixed solution of Nafion solution and ethanol solution with the volume ratio of 1:40;
and S4, placing the sample obtained in the step S3 in a muffle furnace, and calcining for 3 hours at 500 ℃ to obtain the nickel-molybdenum electrode, wherein the heating rate of the muffle furnace is 20 ℃/min.
Example 2:
s1, mixing the following components in mass ratio of 1: mixing 0.8 of nickel-aluminum alloy powder and molybdenum powder, and then ball-milling for 1.5 hours by using a planetary ball mill at the rotating speed of 400r/min, wherein the mass fraction of nickel in the nickel-aluminum alloy powder is 50%, the particle size of the nickel-aluminum alloy powder is 450 meshes, and the particle size of the molybdenum powder is 450 meshes;
s2, placing the ball-milled sample in a NaOH solution with the mass fraction of 25% for 1h to remove aluminum in the sample, and filtering, cleaning and drying after the reaction is completed to obtain catalyst powder, wherein the specific filtering, cleaning and drying steps are that the filtering is carried out by a suction filtration device, the suction filtration is repeated for 10 times, and then the catalyst powder is placed in a blast drying box at 50 ℃ for drying;
s3, mixing the following components in mass ratio of 5:1, uniformly mixing the catalyst powder and the binder to form a catalyst binder mixture, and brushing the catalyst binder mixture on the nickel sheet; then air-drying is carried out until the liquid does not drip; and (3) carrying out brushing for the next time after air drying, and repeating the operation for 5 times, wherein the volume ratio of the adhesive is 1:50 of Nafion solution and ethanol solution;
and S4, placing the sample obtained in the step S3 in a muffle furnace, and calcining at 550 ℃ for 3.5 hours to obtain the nickel-molybdenum electrode, wherein the heating rate of the muffle furnace is 40 ℃/min.
Example 3:
s1, mixing the following components in mass ratio of 1:0.5 of nickel-aluminum alloy powder and molybdenum powder are mixed and ball-milled for 2 hours by using a planetary ball mill under the condition of 600r/min of rotating speed, wherein the mass fraction of nickel in the nickel-aluminum alloy powder is 55%, the particle size of the nickel-aluminum alloy powder is 700 meshes, and the particle size of the molybdenum powder is 700 meshes;
s2, placing the ball-milled sample in a 15% NaOH solution for 1h to remove aluminum in the sample, and filtering, cleaning and drying after the reaction is completed to obtain catalyst powder, wherein the specific filtering, cleaning and drying steps are that the filtering is carried out by a suction filtration device, the suction filtration is repeated for 10 times, and then the catalyst powder is placed in a 50 ℃ blast drying box for drying;
s3, mixing the following components in mass ratio of 5:1, uniformly mixing the catalyst powder and the binder to form a catalyst binder mixture, and brushing the catalyst binder mixture on the nickel sheet; then air-drying is carried out until the liquid does not drip; and (3) carrying out brushing for the next time after air drying, and repeating the operation for 4 times, wherein the volume ratio of the adhesive is 1:40 of Nafion and ethanol solution;
and S4, placing the sample obtained in the step S3 in a muffle furnace, and calcining for 3 hours at 500 ℃ to obtain the nickel-molybdenum electrode, wherein the heating rate of the muffle furnace is 30 ℃/min.
Taking the nickel-molybdenum electrode prepared in example 1 as an example, an LSV test overpotential was performed.
LSV test conditions: electrochemical performance test was performed by means of a Zahner IM6 workstation using a three-electrode system, the working electrode was the electrode prepared in example 1, the auxiliary electrode was a platinum sheet electrode (2 cm x 2 cm), the reference electrode was a mercury/mercury oxide electrode (Hg/HgO), and the electrolyte was a 30% (wt%) KOH solution.
Cathode polarization curve measurement is used for analyzing hydrogen evolution electrochemical performance of electrode, initial potential is-1V, end point potential is-2V, and scanning speed is 5 mV.s -1 . All electrocatalytic samples were activated to steady state using Cyclic Voltammetry (CV) scan of counter electrode, hydrogen evolution electrode scan range of-1.0V to-2.0V, oxygen evolution electrode scan range of 0.2V to 1.0V, scan rate of 50mV.s before LSV test -1 The scan was cycled through 30 turns. All potentials were internal resistance corrected (iR compensated). Converting the potential to a potential relative to a Reversible Hydrogen Electrode (RHE) according to formula (1), wherein E θ Hg/HgO The value was 0.098V and the pH of 30wt% KOH solution was 14.27.
As can be seen from FIGS. 1 and 2, the electrode prepared by the method has good electrochemical activity at 500mA/cm 2 The overpotential was 210mV, which was lower than most of the electrode levels reported in the literature, indicating excellent electrochemical performance of the electrode with a Tafil slope of 105.1mV/dec.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms may be directed to different embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (8)
1. A method for industrially preparing a nickel-molybdenum electrode, which is characterized by comprising the following steps:
(1) The mass ratio is 1: mixing 0.5-1 of nickel-aluminum alloy powder and molybdenum powder, and then performing ball milling to alloy the nickel-aluminum alloy powder and the molybdenum powder, wherein the mass fraction of nickel in the nickel-aluminum alloy powder is 50% -80%;
(2) Placing the ball-milled sample in an alkaline solution for 1h to remove aluminum in the sample, and filtering, cleaning and drying to obtain catalyst powder;
(3) The mass ratio is 3-6: 1 and a binder, wherein the binder is prepared by uniformly mixing the catalyst powder and the binder, and then coating the mixture on an electrode substrate, and the binder has the volume ratio of 1: 40-60 of a mixed solution of Nafion solution and ethanol solution;
(4) And (3) placing the sample obtained in the step (3) in a muffle furnace, and calcining at 500-650 ℃ for 3-5h to obtain the nickel-molybdenum electrode.
2. The method of claim 1, wherein the nickel aluminum alloy powder and the molybdenum powder each have a particle size of 325-800 mesh.
3. The method of claim 1, wherein the ball milling is performed at a ball milling speed of 400-700r/min for a ball milling time of 1-3 hours.
4. The method of claim 1, wherein the alkaline solution is a NaOH solution or a KOH solution.
5. The method of claim 1, wherein the step (3) is performed by mixing the catalyst powder with the binder and brushing the mixture on both sides of the electrode substrate, air-drying the mixture, brushing the mixture again, and repeating the brushing for 3 to 5 times.
6. The method of claim 1, wherein the electrode substrate is nickel mesh, foam nickel, or nickel flakes.
7. The method of claim 1, wherein the muffle has a ramp rate of 10-40 ℃/min.
8. A nickel molybdenum electrode prepared by the method of any one of claims 1-7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202210725694.XA CN115110112B (en) | 2022-06-24 | 2022-06-24 | Industrial preparation method of nickel-molybdenum electrode and nickel-molybdenum electrode |
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| CN202210725694.XA CN115110112B (en) | 2022-06-24 | 2022-06-24 | Industrial preparation method of nickel-molybdenum electrode and nickel-molybdenum electrode |
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| CN115110112A CN115110112A (en) | 2022-09-27 |
| CN115110112B true CN115110112B (en) | 2024-01-30 |
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| CN106191916A (en) * | 2016-07-06 | 2016-12-07 | 天津市大陆制氢设备有限公司 | A kind of efficient porous Ni Mo hydrogen-precipitating electrode and preparation method thereof |
| CN110760875A (en) * | 2019-10-30 | 2020-02-07 | 广东省新材料研究所 | All-solid-state rapid preparation method of alkaline electrolytic water electrode |
| CN114045505A (en) * | 2021-11-22 | 2022-02-15 | 天津大学 | High-activity large-size electrolytic water hydrogen evolution electrode and pulse laser preparation method thereof |
| CN114318361A (en) * | 2021-11-26 | 2022-04-12 | 中国华能集团清洁能源技术研究院有限公司 | Vanadium oxide modified Raney nickel alloy electrode preparation method, electrode and application |
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| CN106191916A (en) * | 2016-07-06 | 2016-12-07 | 天津市大陆制氢设备有限公司 | A kind of efficient porous Ni Mo hydrogen-precipitating electrode and preparation method thereof |
| CN110760875A (en) * | 2019-10-30 | 2020-02-07 | 广东省新材料研究所 | All-solid-state rapid preparation method of alkaline electrolytic water electrode |
| CN114045505A (en) * | 2021-11-22 | 2022-02-15 | 天津大学 | High-activity large-size electrolytic water hydrogen evolution electrode and pulse laser preparation method thereof |
| CN114318361A (en) * | 2021-11-26 | 2022-04-12 | 中国华能集团清洁能源技术研究院有限公司 | Vanadium oxide modified Raney nickel alloy electrode preparation method, electrode and application |
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