Jackfruit shell grain-shaped alkaline electrolytic water hydrogen production electrode as well as preparation method and application thereof

By constructing a jackfruit shell-shaped nickel hydroxide limited domain carrier in an electrolytic water-producing hydrogen electrode and coupling platinum atoms, the problems of carbon support corrosion and high cost are solved, and efficient and low-energy hydrogen production is achieved, and stability is maintained under industrial conditions.

CN119593012APending Publication Date: 2025-03-11XIAN TAIJIN NEW ENERGY & MATERIALS SCI TECH CO LTD
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Patent Information

Application Number
CN202411966950.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2025-03-11

AI Technical Summary

Technical Problem

In the prior art, carbon support is easily corroded in a strong acid-base and strong redox environment of electrolyzed water to produce hydrogen, resulting in the agglomeration and inactivation of metal atoms, and the high cost and production inconsistency limit large-scale mass production.

Method used

By adjusting the electrodeposition parameters, a uniform and continuous jackfruit shell-shaped nickel hydroxide limit domain support is constructed on the nickel support, and platinum atom deposition and dispersion is coupled on its surface to achieve cost reduction and efficiency of precious metal catalysts.

Benefits of technology

It is achieved to ensure the number of effective active sites of the platinum catalyst while reducing the platinum load, improve the conductivity of the catalytic layer, promote the orderly migration of hydrogen species, enhance the hydrogen evolution reaction effect, reduce hydrogen production energy consumption, and maintain stable operation under industrial conditions.

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Abstract

The invention belongs to the technical field of water electrolysis hydrogen production, and particularly relates to a jack fruit shell grain-shaped alkaline water electrolysis hydrogen production electrode and a preparation method and application thereof. The alkaline electrolytic water hydrogen production electrode comprises a nickel support body and micron-sized granular nickel hydroxide uniformly distributed on the surface of the nickel support body, wherein a platinum catalyst is grown on the surface of the micron-sized granular nickel hydroxide in situ; the preparation method of the alkaline electrolytic water hydrogen production electrode comprises the following steps: immersing a nickel support body into a first electrolyte for first electrochemical deposition to obtain a nickel-supported nickel hydroxide electrode, and immersing the nickel-supported nickel hydroxide electrode into a second electrolyte for second electrochemical deposition to obtain a nickel-supported platinum-loaded nickel hydroxide electrode; according to the preparation method, by selecting a first electrolyte formula, a second electrolyte formula and electrodeposition parameters, the prepared hydrogen production electrode can improve the overall conductivity of a catalyst layer, the limiting space of the hydrogen production electrode promotes ordered migration of hydrogen species on different active sites of platinum / nickel hydroxide, and the hydrogen production electrode is lower in hydrogen production energy consumption and adapts to stable operation of a working condition environment.
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Description

Technical Field

[0001] The invention belongs to the technical field of water electrolysis hydrogen production, and particularly relates to a jackfruit shell grain-shaped alkaline water electrolysis hydrogen production electrode and a preparation method and application thereof. Background Art

[0002] As an energy material that is both clean and energy-dense, hydrogen is driving the green transformation of the global economy and becoming the most promising new energy carrier to break free from the constraints of traditional fossil fuels. However, the large-scale use of hydrogen energy still faces major challenges. In the context of the rapid development of new energy, electrocatalytic water decomposition driven by renewable energy such as wind or solar energy is considered to be the green hydrogen technology that best complies with the sustainable development strategy. When evaluating the economic and cost-effective feasibility of hydrogen production, the energy consumption requirements and equipment costs of the electrolysis process must be carefully considered. The alkaline water electrolysis hydrogen production technology route is the most mature and is the main electrolysis hydrogen production method on the market. The design of high-performance electrode materials with high activity, low energy consumption and long life will help improve hydrogen production capacity, reduce the overall hydrogen production cost and promote the large-scale industrial application of water electrolysis hydrogen production technology.

[0003] Although traditional non-precious metal electrodes have made some application progress in alkaline electrolyzers due to their low cost, from the perspective of long-term high hydrogen production efficiency and reduced electrolysis energy consumption, platinum-based materials have the best ability to combine with hydrogen and are still considered to be the most active electrocatalytic HER (Hydrogen Evolution Reaction) catalysts. However, the application progress of platinum-based precious metal materials is limited by their low abundance in the earth's crust and relatively higher costs. Reducing the precious metal loading while ensuring its high activity is currently the optimal solution; single-atom catalytic strategy provides an effective way to reduce the cost and increase the efficiency of precious metal catalysts. As the size of the catalyst decreases, the utilization rate of active atoms will gradually increase. Therefore, single-atom catalysts can make the utilization rate of precious metal atoms reach 100%. Carbon materials, as common carriers, are widely used in single-atom confinement.

[0004] The spatial confinement strategy directionally confines or encapsulates active species within a certain space by constructing confined template carriers such as interlayer confinement, lattice confinement, and metal bond confinement; coupling metal sites with carrier sites can achieve independent dispersion of metal active species in spatial distribution, and also make it easier for reaction intermediates to transfer within the confined space, effectively ensuring the high activity, high selectivity, and high stability of the catalyst.

[0005] In the prior art, the invention patent application with publication number "CN113258088B" and name "A Carbon-supported Multi-element Single Atom Metal Catalyst" uses transient Joule heating method to achieve uniform dispersion of metal single atoms on the surface of the carbon carrier, and has good catalytic activity in the field of catalytic oxygen reduction reaction of fuel cells; however, in the strong acid and alkali and strong redox working conditions of water electrolysis to produce hydrogen, the carbon carrier is easily corroded and dissolved, resulting in the agglomeration and inactivation of the coupled metal atoms.

[0006] In the prior art, the invention patent application with publication number "CN118910644A" and titled "A cactus-shaped nickel hydroxide multi-level nanostructured material and its preparation method and application" synthesizes nickel hydroxide nanocrystals assembled by hierarchical nanowires and nanosheets by a solvothermal method, and uses morphology optimization to adjust the active site density and local electronic structure to improve catalytic performance. However, this method has a high production cost, and the product consistency is difficult to control, making it difficult to achieve large-scale mass production.

[0007] In the prior art, an invention patent application with publication number "CN117661023A" and titled "A Method for Preparing Nano-Nickel Alkaline Hydrogen Evolution Electrode" discloses a method for obtaining a nickel hydroxide / nanodendrite nickel electrode supported on a nickel substrate by electrodeposition to achieve multi-interface chemical bonding. Since the nickel hydroxide carrier structure is single and the growth of anchored atoms is not confined, the nickel metal grows into a large-sized dendrite nickel structure. Summary of the invention

[0008] In order to overcome the shortcomings of the above-mentioned prior art, the purpose of the present invention is to propose a jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode and a preparation method and application thereof, wherein the hydrogen production electrode preparation method adjusts the electrodeposition parameters in the hydrogen production electrode preparation process to construct a uniform and continuous jackfruit shell-shaped nickel hydroxide confined carrier on the electrode support, and couples platinum atoms to deposit and disperse on the nickel hydroxide confined carrier, thereby achieving cost reduction and efficiency improvement of precious metal catalysts for alkaline water electrolysis hydrogen production electrodes.

[0009] In a first aspect, a jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode comprises a nickel support, on the surface of which micron-sized granular nickel hydroxide is evenly distributed, and on the surface of which a platinum catalyst is in-situ grown.

[0010] Furthermore, the particle size of the micron-sized granular nickel hydroxide is in the range of 0.7-1.4 microns, and the micron-sized granular nickel hydroxide has a jackfruit shell-like structure.

[0011] In a second aspect, a method for preparing a jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode comprises the following steps:

[0012] Step 1: Add a nickel source compound and citric acid to a first solvent in sequence, and stir until completely dissolved to form a first electrolyte;

[0013] Step 2: immersing the nickel support into the first electrolyte in step 1 to perform a first electrochemical deposition to obtain a nickel-supported nickel hydroxide electrode (Ni / Ni(OH)x);

[0014] Step 3: Add a platinum source compound and sodium tartrate to the second solvent in sequence, and stir until completely dissolved to form a second electrolyte;

[0015] Step 4: immersing the nickel-supported nickel hydroxide electrode (Ni / Ni(OH)x) in step 2 into the second electrolyte in step 3 for a second electrochemical deposition to obtain a nickel-supported platinum-loaded nickel hydroxide electrode (Ni / Pt-Ni(OH)x);

[0016] Preferably, in step 1 or step 3, the first solvent or the second solvent is any one or more of pure water, Tris buffer, Tris hydrochloric acid buffer, and isopropanol, and the first solvent or the second solvent may be the same or different;

[0017] Preferably, the nickel source compound in step 1 is any one or more of nickel chloride, nickel nitrate, nickel sulfate, nickel sulfamate, and nickel acetate;

[0018] Preferably, the nickel support in step 2 is any one of nickel foam, nickel mesh, and nickel felt;

[0019] Preferably, the platinum source compound in step 3 is any one of chloroplatinic acid and dinitrosodiammineplatinum.

[0020] Furthermore, in step 1, the nickel source ion concentration in the first electrolyte is 0.05-0.2 mol / L, and the mass percentage of citric acid is 5-30 wt%;

[0021] Preferably, the nickel source ion concentration in the first electrolyte is any one of 0.05 mol / L, 0.1 mol / L, 0.15 mol / L, and 0.2 mol / L;

[0022] Preferably, the mass percentage of citric acid in the first electrolyte is any one of 5wt%, 10wt%, 20wt%, and 30wt%;

[0023] Furthermore, before immersing the nickel support in the first electrolyte, the nickel support in step 2 is first immersed in a 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 1-20 min to remove surface oxides and other impurities, and then the nickel support after ultrasonic cleaning is rinsed with ultrapure water and vacuum dried.

[0024] Furthermore, the specific process of the first electrochemical deposition in step 2 is: using a three-electrode system, the nickel support is used as a cathode and an anode respectively, silver / silver chloride is used as a reference electrode, the cathode, the anode and the reference electrode are immersed in a first electrolyte, and a multi-current step is used to perform constant current deposition on the nickel source ions in the first electrolyte, and the reaction system temperature in the first electrochemical deposition is controlled to be 20-50°C, the stirring speed in the first electrolyte is 200-600r / min, and the constant current density is 5-30mA / cm 2 The first deposition time is 10 to 90 minutes, and after the first electrochemical deposition is completed, a nickel-supported nickel hydroxide electrode (Ni / Ni(OH)x) is obtained;

[0025] Preferably, the temperature of the reaction system is any one of 20°C, 30°C, 40°C, and 50°C;

[0026] Preferably, the stirring speed in the first electrolyte is any one of 200r / min, 300r / min, 400r / min, 500r / min, and 600r / min;

[0027] Preferably, the constant current density is 5 mA / cm 2 , 10mA / cm 2 , 20mA / cm 2 、30mA / cm 2 Any value in ;

[0028] Preferably, the first deposition time is any one of 10 min, 30 min, 60 min and 90 min.

[0029] Furthermore, in step 3, the concentration of platinum source ions in the second electrolyte is 0.02-0.1 mol / L, and the mass percentage of sodium tartrate is 5%-30wt%;

[0030] Preferably, the concentration of platinum source ions in the second electrolyte is any one of 0.02 mol / L, 0.04 mol / L, 0.06 mol / L, 0.08 mol / L, and 0.1 mol / L;

[0031] Preferably, the mass percentage of sodium tartrate in the second electrolyte is any one of 5wt%, 10wt%, 20wt% and 30wt%.

[0032] Furthermore, in step 4, the specific process of the second electrochemical deposition is as follows: a three-electrode system is used, the nickel-supported nickel hydroxide electrode is used as a cathode, and a platinum sheet electrode is used as an anode, the cathode and the anode are immersed in a second electrolyte, and cyclic voltammetry is used to perform electroreduction limited deposition on the platinum source ions in the second electrolyte, and the voltage range in the second electrochemical deposition is controlled to be 0 to -0.5V, the scanning rate is 50 to 200mV / s, and the cycle period is 20 to 100 circles;

[0033] Preferably, the scanning rate is any one of 50mV / s, 100mV / s, 150mV / s, and 200mV / s;

[0034] Preferably, the cycle period is any value among 20 circles, 40 circles, 60 circles, 80 circles, and 100 circles.

[0035] Furthermore, a method for preparing an alkaline water electrolysis hydrogen production electrode comprises the following steps:

[0036] Step 9.1: Add nickel sulfate and citric acid to a 1 mol / L, pH=8.5 Tris buffer, and stir until completely dissolved to obtain a first electrolyte with a nickel sulfate concentration of 0.1 mol / L and a citric acid mass percentage of 10 wt%;

[0037] Step 9.2: Using the three-electrode system of the Chenhua electrochemical workstation, take two pre-treated commercial foamed nickel (FN) sheets and clamp them with platinum electrode clamps as cathode and anode respectively, and silver / silver chloride as reference electrode. Add the first electrolyte in step 9.1 until the pre-treated FN is submerged 1 cm below the first electrolyte. 2 and put in a stirrer; set the water bath temperature of the first electrolyte in the electrolytic cell to 40°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 200r / min; select multiple current steps (ISTEP), set the current size to 0.01A, that is, the constant current density is 10mA / cm 2 After 60 min of deposition, the FN after cathode pretreatment was removed, rinsed with pure water and vacuum dried to obtain a nickel hydroxide electrode supported by nickel foam (FN / Ni(OH)x);

[0038] Step 9.3: Add chloroplatinic acid and sodium tartrate to pure water, and stir until completely dissolved to obtain a second electrolyte with a chloroplatinic acid concentration of 0.08 mol / L and a sodium tartrate mass percentage of 5 wt%;

[0039] Step 9.4: Using the three-electrode system of Chenhua electrochemical workstation, the FN / Ni(OH)x obtained in step 9.2 was clamped with a platinum electrode clamp as the cathode, the platinum electrode as the anode, and silver / silver chloride as the reference electrode. The second electrolyte in step 9.3 was added until the FN / Ni(OH)x was submerged 1 cm below the second electrolyte. 2 And put in a stirring bar; set the water bath temperature of the second electrolyte in the electrolytic cell to 30°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 600r / min; use cyclic voltammetry (CV) with a voltage range of 0 to -0.5V and a scan rate of 50mV / s. After 20 cycles, remove the cathode FN / Ni(OH)x, rinse with pure water and vacuum dry to obtain a foam nickel-supported platinum-loaded nickel hydroxide electrode (FN / Pt-Ni(OH)x).

[0040] The third aspect is the application of a jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode in alkaline water electrolysis hydrogen production.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] 1. The jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode provided by the present invention has a water contact angle of less than 2° for the nickel-supported nickel hydroxide electrode compared with traditional commercial nickel foam or nickel mesh electrodes, and has better hydrophilicity and air repellency and a larger specific surface area.

[0043] 2. The jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode provided by the present invention, compared with the pure platinum precious metal electrode, the nickel-supported platinum-loaded nickel hydroxide electrode can reduce the platinum loading while ensuring the number of effective active sites of the platinum catalyst. While improving the overall conductivity of the catalytic layer, the confined space promotes the orderly migration of adsorbed hydrogen species on different active sites of platinum and nickel hydroxide in the nickel-supported platinum-loaded nickel hydroxide electrode of the present invention, thereby enhancing the hydrogen overflow effect and thus strengthening the hydrogen evolution reaction process.

[0044] 3. In step 1 of the present invention, citric acid is used as a chelating agent of the first electrolyte to stabilize the nickel source ions to form chelates and evenly disperse them in different pH solvent systems. In step 2, the first electrodeposition process parameters are further adjusted to construct the nickel source ions by electrodeposition, thereby achieving the autonomous controllability of uniform and continuous high-quality loading of the nickel hydroxide particle structure on the nickel support.

[0045] 4. In step 3 of the present invention, sodium tartrate is used as a complexing agent of the second electrolyte to stabilize the platinum source ions to form chelates and evenly disperse them in different pH solvent systems. In step 4, the second electrodeposition process parameters are further adjusted to preferentially electro-reduced and deposit the platinum source ions at the tips of the nickel hydroxide particles, thereby achieving autonomous controllability of the nickel hydroxide carrier island in spatial confinement of platinum atoms.

[0046] In summary, the present invention sets reaction parameters to achieve uniform distribution of micron-sized granular nickel hydroxide on the surface of the nickel support, and in-situ growth of a platinum catalyst on the surface of the micron-sized granular nickel hydroxide. This can reduce the platinum loading while fully ensuring the number of effective active sites of the platinum catalyst. It has lower energy consumption for hydrogen production, can adapt to stable operation in the working environment, and has industry-leading electrocatalytic activity performance in the alkaline water electrolysis process. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 This is a scanning electron microscope image of the jackfruit shell-shaped nickel-supported nickel hydroxide electrode prepared in Example 4 of the present invention.

[0048] Figure 2 This is a scanning electron microscope image of the jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrode prepared in Example 4 of the present invention.

[0049] Figure 3 This is a mapping diagram of the nickel element distribution of the jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrode prepared in Example 4 of the present invention.

[0050] Figure 4 This is a platinum element distribution mapping diagram of the jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrode prepared in Example 4 of the present invention.

[0051] Figure 5 This is an overlay diagram of the nickel and platinum multi-element distribution of the jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrode prepared in Example 4 of the present invention.

[0052] Figure 6 This is a statistical diagram of the particle size of the jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrode prepared in Example 4 of the present invention.

[0053] Figure 7 The water contact angles of the jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrodes prepared in Comparative Example 1 and Example 4 of the present invention.

[0054] Figure 8 Linear sweep voltammetry (LSV) curves of the alkaline water electrolysis hydrogen evolution reaction of the jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrode prepared in Comparative Example 1 and Example 4 of the present invention.

[0055] Fig. 9 This is a constant current curve of the alkaline water electrolysis hydrogen evolution reaction of the jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrode prepared in Example 4 of the present invention. DETAILED DESCRIPTION

[0056] Combine the following Figures 1 to 9The present invention is further described in detail with reference to the examples and comparative examples. Unless otherwise specified, the reagents used in the examples of the present application are all analytically pure reagents purchased on the market, and the equipment and instruments used are all conventional equipment and instruments in the art.

[0057] In a first aspect, a jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode comprises a nickel support, on the surface of which micron-sized granular nickel hydroxide is evenly distributed, and on the surface of which a platinum catalyst is in-situ grown.

[0058] Furthermore, the particle size of the micron-sized granular nickel hydroxide is in the range of 0.7-1.4 microns, the average particle size is in the range of 1 micron, and the micron-sized granular nickel hydroxide has a jackfruit shell grain structure.

[0059] In a second aspect, a method for preparing a jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode comprises the following steps:

[0060] Step 1: Add a nickel source compound and citric acid to a first solvent in sequence, and stir until completely dissolved to form a first electrolyte;

[0061] Step 2: Immerse the nickel support in the first electrolyte of step 1 to perform a first electrochemical deposition to obtain a nickel-supported nickel hydroxide electrode (Ni / Ni(OH)x); the nickel hydroxide in the Ni / Ni(OH)x is a jackfruit shell-like micron-sized granular nickel hydroxide, and the jackfruit shell-like micron-sized granular nickel hydroxide is loaded on the surface of the nickel support;

[0062] Step 3: Add a platinum source compound and sodium tartrate to the second solvent in sequence, and stir until completely dissolved to form a second electrolyte;

[0063] Step 4: Immerse the Ni / Ni(OH)x described in step 2 into the second electrolyte in step 3 for a second electrochemical deposition to obtain a nickel-supported platinum-loaded nickel hydroxide electrode (Ni / Pt-Ni(OH)x), wherein the water bath temperature of the second electrolyte is 20-60°C.

[0064] The invention relates to a jackfruit shell grain-shaped alkaline water electrolysis hydrogen production electrode and a preparation method and application thereof. By selecting a first electrolyte formula formed by an optimal nickel source, a first solvent and citric acid, and first electrochemical deposition process parameters such as electrodeposition temperature, electrolyte stirring speed, constant current density, and deposition time; by selecting a second electrolyte formula formed by an optimal platinum source, a second solvent and sodium tartrate, and second electrochemical deposition process parameters such as scanning rate and cycle period, uniform and continuous nickel hydroxide confined carrier islands are finally obtained on a nickel support, and platinum atoms are effectively restricted to be stably dispersed on the surface of the nickel hydroxide support. While improving the overall conductivity of the catalytic layer, the confined space promotes the orderly migration of adsorbed hydrogen species on different active sites of platinum and nickel hydroxide in the nickel-supported platinum-loaded nickel hydroxide electrode of the invention, thereby enhancing the hydrogen overflow effect and thus strengthening the hydrogen evolution reaction process.

[0065] Embodiment 1:

[0066] Nickel support pretreatment:

[0067] Cut the commercial nickel foam (FN) into 1*2cm 2 The size was immersed in 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 20 min to remove surface oxides and other impurities, and then the FN after ultrasonic cleaning was rinsed with ultrapure water and vacuum dried to obtain the pretreated FN.

[0068] Step 1: Prepare the first electrolyte, namely nickel ion electrolyte

[0069] Add a certain proportion of nickel chloride and citric acid to a 1 mol / L, pH=8.5 Tris buffer, and stir until completely dissolved to obtain a first electrolyte with a nickel chloride concentration of 0.2 mol / L and a citric acid mass percentage of 5 wt%;

[0070] Step 2: Electrodeposition of Nickel Hydroxide (Ni(OH)x)

[0071] Using the three-electrode system of Chenhua electrochemical workstation, take 2 pretreated FN sheets, clamp them with platinum electrode clamps, use them as cathode and anode respectively, silver / silver chloride is used as reference electrode, add the first electrolyte until the pretreated FN is submerged 1cm below the first electrolyte 2 and put in a stirrer; set the water bath temperature of the first electrolyte in the electrolytic cell to 20°C, and stabilize it for 30 minutes after reaching the temperature; adjust the magnetic stirring speed in the first electrolyte to 500r / min; select multiple current steps (ISTEP), set the current size to 0.005A, that is, the constant current density is 5mA / cm 2 After 90 minutes of electrodeposition, the FN after cathode pretreatment was removed, rinsed with pure water and vacuum dried to obtain FN / Ni(OH)x, i.e., nickel hydroxide electrode supported by nickel foam;

[0072] Step 3: Prepare the second electrolyte, i.e., platinum ion electrolyte

[0073] Add a certain proportion of dinitrosodiammineplatinum and sodium tartrate to a 1 mol / L, pH=6.8 Tris hydrochloric acid buffer, and stir until completely dissolved to obtain a second electrolyte with a dinitrosodiammineplatinum concentration of 0.02 mol / L and a mass percentage of sodium tartrate of 30 wt%;

[0074] Step 4: Electrodeposition of Platinum

[0075] Using the three-electrode system of Chenhua electrochemical workstation, the FN / Ni(OH)x obtained in step 2 was clamped with a platinum electrode clamp as the cathode, the platinum electrode as the anode, and silver / silver chloride as the reference electrode. The second electrolyte was added until the FN / Ni(OH)x was submerged 1 cm below the second electrolyte. 2 And put in a stirring bar; set the water bath temperature of the second electrolyte in the electrolytic cell to 30°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 200r / min; select cyclic voltammetry (CV) with a voltage range of 0 to -0.5V and a scan rate of 200mV / s. After 100 cycles, remove the FN / Ni(OH)x at the cathode, rinse with pure water and vacuum dry to obtain FN / Pt-Ni(OH)x, i.e., a platinum-loaded nickel hydroxide electrode supported by nickel foam.

[0076] Embodiment 2:

[0077] Nickel support pretreatment

[0078] Cut the commercial nickel mesh (NM) into 1*2cm 2 The size was immersed in 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 15 min to remove surface oxides and other impurities, and then the NM after ultrasonic cleaning was rinsed with ultrapure water and vacuum dried to obtain the pretreated NM.

[0079] Step 1: Prepare nickel ion electrolyte

[0080] Add a certain proportion of nickel sulfamate and citric acid to pure water, and stir until completely dissolved to obtain a first electrolyte with a nickel sulfamate concentration of 0.15 mol / L and a citric acid mass percentage of 30 wt%;

[0081] Step 2: Electrodeposition of Nickel Hydroxide (Ni(OH)x)

[0082] Using the three-electrode system of Chenhua electrochemical workstation, take two pretreated NMs, clamp them with platinum electrode clamps, use them as cathode and anode respectively, and use saturated calomel as reference electrode. Add the first electrolyte until the pretreated NMs are submerged 1 cm below the first electrolyte.2 A mechanical stirring paddle was placed; the water bath temperature of the first electrolyte in the electrolytic cell was set to 30°C, and the temperature was stabilized for 30 minutes; the mechanical stirring speed in the first electrolyte was adjusted to 400 r / min; multiple current steps (ISTEP) were selected, and the current size was set to 0.03A, that is, the constant current density was 30 mA / cm 2 , after 10 min of electrodeposition, the NM after cathode pretreatment was removed, rinsed with pure water and vacuum dried to obtain NM / Ni(OH)x (nickel hydroxide electrode supported by nickel mesh);

[0083] Step 3: Prepare platinum ion electrolyte

[0084] Add a certain proportion of chloroplatinic acid and sodium tartrate to a 1 mol / L, pH=6.8 Tris hydrochloric acid buffer, and stir until completely dissolved to obtain a second electrolyte with a chloroplatinic acid concentration of 0.04 mol / L and a sodium tartrate mass percentage of 10 wt%;

[0085] Step 4: Electrodeposition of Platinum

[0086] Using the three-electrode system of Chenhua electrochemical workstation, the NM / Ni(OH)x obtained in step 2 was clamped with a platinum electrode clamp as the cathode, the platinum electrode as the anode, and saturated calomel as the reference electrode. The second electrolyte was added until the NM / Ni(OH)x was submerged 1 cm below the second electrolyte. 2 A mechanical stirring paddle was added; the water bath temperature of the second electrolyte in the electrolytic cell was set to 40°C, and the mixture was stabilized for 30 minutes after reaching the temperature; the mechanical stirring speed was adjusted to 600 r / min; cyclic voltammetry (CV) was used with a voltage range of 0 to -0.5 V and a scan rate of 150 mV / s. After 80 cycles, the cathode NM / Ni(OH)x was removed, rinsed with pure water and dried in vacuum to obtain NM / Pt-Ni(OH)x (platinum-loaded nickel hydroxide electrode supported by a nickel mesh).

[0087] Embodiment 3:

[0088] Nickel support pretreatment

[0089] Commercial nickel felt (Nickel Felt, NF) was cut into 1*2 cm 2 The size was immersed in 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 10 min to remove surface oxides and other impurities, and then the NF after ultrasonic cleaning was rinsed with ultrapure water and vacuum dried to obtain the pretreated NF.

[0090] Step 1: Prepare nickel ion electrolyte

[0091] Add a certain proportion of nickel acetate and citric acid to a mixture of pure water and isopropanol in a volume ratio of 1:1, and stir until completely dissolved to obtain a first electrolyte with a nickel acetate concentration of 0.05 mol / L and a citric acid mass percentage of 20 wt%;

[0092] Step 2: Electrodeposition of Nickel Hydroxide (Ni(OH)x)

[0093] Using the three-electrode system of Chenhua electrochemical workstation, take two pre-treated NFs, clamp them with platinum electrode clamps, use them as cathode and anode respectively, silver / silver chloride is used as reference electrode, add the first electrolyte until the pre-treated NF is submerged 1cm below the first electrolyte 2 and put in a stirrer; set the water bath temperature of the first electrolyte in the electrolytic cell to 50°C, and stabilize it for 30 minutes after reaching the temperature; adjust the magnetic stirring speed in the first electrolyte to 300r / min; select multiple current steps (ISTEP), set the current size to 0.02A, that is, the constant current density is 20mA / cm 2 After 30 min of deposition, the NF after cathode pretreatment was removed, rinsed with pure water and vacuum dried to obtain NF / Ni(OH)x (nickel hydroxide electrode supported by nickel felt);

[0094] Step 3: Prepare platinum ion electrolyte

[0095] Add a certain proportion of diamine dinitrosoplatinum and sodium tartrate to pure water, and stir until completely dissolved to obtain a second electrolyte with a diamine dinitrosoplatinum concentration of 0.06 mol / L and a mass percentage of sodium tartrate of 20 wt%;

[0096] Step 4: Electrodeposition of Platinum

[0097] Using the three-electrode system of Chenhua electrochemical workstation, the NF / Ni(OH)x obtained in step 2 was clamped with a platinum electrode clamp as the cathode, and a pretreated NF was clamped with a platinum electrode clamp as the anode, and silver / silver chloride was used as the reference electrode. The second electrolyte was added until the NF / Ni(OH)x was submerged 1 cm below the second electrolyte. 2 And put in a stirring bar; set the water bath temperature of the second electrolyte in the electrolytic cell to 60°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 300r / min; select cyclic voltammetry (CV) with a voltage range of 0 to -0.5V and a scanning rate of 100mV / s. After 60 cycles, remove the NF / Ni(OH)x at the cathode, rinse with pure water and vacuum dry to obtain NF / Pt-Ni(OH)x (platinum-loaded nickel hydroxide electrode supported by nickel felt).

[0098] Embodiment 4:

[0099] Nickel support pretreatment

[0100] Cut the commercial nickel foam (FN) into 1*10cm 2 The size was immersed in 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 20 min to remove surface oxides and other impurities, and then the FN after ultrasonic cleaning was rinsed with ultrapure water and vacuum dried to obtain the pretreated FN.

[0101] Step 1: Prepare nickel ion electrolyte

[0102] A certain proportion of nickel sulfate and citric acid are added to a 1 mol / L, pH=8.5 Tris buffer, and stirred until completely dissolved to obtain a first electrolyte with a nickel sulfate concentration of 0.1 mol / L and a citric acid mass percentage of 10 wt%;

[0103] Step 2: Electrodeposition of Nickel Hydroxide (Ni(OH)x)

[0104] Using the three-electrode system of Chenhua electrochemical workstation, take two pretreated FN sheets and clamp them with platinum electrode clamps as cathode and anode respectively, silver / silver chloride as reference electrode, add the first electrolyte until the pretreated FN is submerged 1cm below the first electrolyte 2 and put in a stirrer; set the water bath temperature of the first electrolyte in the electrolytic cell to 40°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 200r / min; select multiple current steps (ISTEP), set the current size to 0.01A, that is, the constant current density is 10mA / cm 2 , after 60 min of deposition, the FN after cathode pretreatment was removed, rinsed with pure water and vacuum dried to obtain FN / Ni(OH)x;

[0105] Step 3: Prepare platinum ion electrolyte

[0106] Add a certain proportion of chloroplatinic acid and sodium tartrate to pure water, and stir until completely dissolved to obtain a second electrolyte with a chloroplatinic acid concentration of 0.08 mol / L and a sodium tartrate mass percentage of 5 wt%;

[0107] Step 4: Electrodeposition of Platinum

[0108] Using the three-electrode system of Chenhua electrochemical workstation, the FN / Ni(OH)x obtained in step 2 was clamped with a platinum electrode clamp as the cathode, the platinum electrode as the anode, and silver / silver chloride as the reference electrode. The second electrolyte was added until the FN / Ni(OH)x was submerged 1 cm below the second electrolyte. 2And put in a stirring bar; set the water bath temperature of the second electrolyte in the electrolytic cell to 30°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 600r / min; use cyclic voltammetry (CV) with a voltage range of 0 to -0.5V and a scan rate of 50mV / s. After 20 cycles, remove the FN / Ni(OH)x at the cathode, rinse with pure water and vacuum dry to obtain FN / Pt-Ni(OH)x.

[0109] Embodiment 5:

[0110] Nickel support pretreatment

[0111] Cut the commercial nickel foam (FN) into 1*2cm 2 The size was immersed in a 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 1 min to remove surface oxides and other impurities, and then the FN after ultrasonic cleaning was rinsed with ultrapure water and vacuum dried to obtain the pretreated FN.

[0112] Step 1: Prepare nickel ion electrolyte

[0113] Add a certain proportion of nickel nitrate and citric acid to a 1 mol / L, pH=8.5 Tris buffer, and stir until completely dissolved to obtain a first electrolyte with a nickel nitrate concentration of 0.15 mol / L and a citric acid mass percentage of 15 wt%;

[0114] Step 2: Electrodeposition of Nickel Hydroxide (Ni(OH)x)

[0115] Using the three-electrode system of Chenhua electrochemical workstation, take two pretreated FN sheets and clamp them with platinum electrode clamps as cathode and anode respectively, mercury / mercuric oxide as reference electrode, add the first electrolyte until the pretreated FN is submerged 1 cm below the first electrolyte 2 and put in a stirrer; set the water bath temperature of the first electrolyte in the electrolytic cell to 25°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 600r / min; select multiple current steps (ISTEP), set the current size to 0.01A, that is, the constant current density is 10mA / cm 2 , after deposition for 30 min, the FN after cathode pretreatment was removed, rinsed with pure water and vacuum dried to obtain FN / Ni(OH)x;

[0116] Step 3: Prepare platinum ion electrolyte

[0117] Add a certain proportion of chloroplatinic acid and sodium tartrate to pure water, and stir until completely dissolved to obtain a second electrolyte with a chloroplatinic acid concentration of 0.1 mol / L and a sodium tartrate mass percentage of 15 wt%;

[0118] Step 4: Electrodeposition of Platinum

[0119] Using the three-electrode system of Chenhua electrochemical workstation, the FN / Ni(OH)x obtained in step 2 was clamped with a platinum electrode clamp as the cathode, the platinum electrode as the anode, and silver / silver chloride as the reference electrode. The second electrolyte was added until the FN / Ni(OH)x was submerged 1 cm below the second electrolyte. 2 And put in a stirring bar; set the water bath temperature of the second electrolyte in the electrolytic cell to 50°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 300r / min; select cyclic voltammetry (CV) with a voltage range of 0 to -0.5V and a scan rate of 100mV / s. After 40 cycles, remove the FN / Ni(OH)x at the cathode, rinse with pure water and vacuum dry to obtain FN / Pt-Ni(OH)x.

[0120] Embodiment 6:

[0121] Nickel support pretreatment

[0122] Cut the commercial nickel foam (FN) into 1*2cm 2 The size was immersed in 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 20 min to remove surface oxides and other impurities, and then the FN after ultrasonic cleaning was rinsed with ultrapure water and vacuum dried to obtain the pretreated FN.

[0123] Step 1: Prepare nickel ion electrolyte

[0124] Add a certain proportion of nickel sulfate, nickel nitrate and citric acid to pure water, stir until completely dissolved, and obtain a first electrolyte with a nickel sulfate concentration of 0.05 mol / L, a nickel nitrate concentration of 0.05 mol / L, and a citric acid mass percentage of 15 wt%;

[0125] Step 2: Electrodeposition of Nickel Hydroxide (Ni(OH)x)

[0126] Using the three-electrode system of Chenhua electrochemical workstation, take two pretreated FN sheets and clamp them with platinum electrode clamps as cathode and anode respectively, silver / silver chloride as reference electrode, add the first electrolyte until the pretreated FN is submerged 1cm below the first electrolyte 2 and put in a stirrer; set the water bath temperature of the first electrolyte in the electrolytic cell to 30°C, and stabilize it for 30 minutes after reaching the temperature; adjust the magnetic stirring speed to 300r / min; select multiple current steps (ISTEP), set the current size to 0.01A, that is, the constant current density is 10mA / cm 2 , after deposition for 30 min, the FN after cathode pretreatment was removed, rinsed with pure water and vacuum dried to obtain FN / Ni(OH)x;

[0127] Step 3: Prepare platinum ion electrolyte

[0128] Add a certain proportion of chloroplatinic acid and sodium tartrate to pure water, and stir until completely dissolved to obtain a second electrolyte with a chloroplatinic acid concentration of 0.1 mol / L and a sodium tartrate mass percentage of 10 wt%;

[0129] Step 4: Electrodeposition of Platinum

[0130] Using the three-electrode system of Chenhua electrochemical workstation, the FN / Ni(OH)x obtained in step 2 was clamped with a platinum electrode clamp as the cathode, the platinum electrode as the anode, and silver / silver chloride as the reference electrode. The second electrolyte was added until the FN / Ni(OH)x was submerged 1 cm below the second electrolyte. 2 And put in a stirring bar; set the water bath temperature of the second electrolyte in the electrolytic cell to 20°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 300r / min; select cyclic voltammetry (CV) with a voltage range of 0 to -0.5V and a scan rate of 50mV / s. After 20 cycles, remove the FN / Ni(OH)x at the cathode, rinse with pure water and vacuum dry to obtain FN / Pt-Ni(OH)x.

[0131] Comparative Example 1:

[0132] Comparative Example 1 is pure nickel foam without any Pt-Ni(OH)x deposition layer. Commercial nickel foam (FN) is immersed in a 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 20 min to remove surface oxides and other impurities. The FN after ultrasonic cleaning is then rinsed with ultrapure water and vacuum dried to obtain pretreated FN. The pretreated FN is then used for electrochemical hydrogen evolution performance test.

[0133] The present invention performs the following characterization on Examples 1 to 6 and Comparative Example 1 to demonstrate the beneficial effects of the present invention:

[0134] Figure 1 The microstructure of the prepared jackfruit shell-like nickel-supported nickel hydroxide electrode is shown. Figure 1 It can be clearly seen that the micron-sized granular nickel hydroxide presents a jackfruit shell-like structure, and the structure of the micron-sized granular nickel hydroxide is uniform and continuous.

[0135] Figure 2 The microstructure of the prepared jackfruit shell-like nickel-supported platinum-loaded nickel hydroxide electrode is demonstrated, with stably dispersed platinum atoms in the upper domain based on the surface carrier particle structure and having large roughness and specific surface area.

[0136] Figure 3 The nickel element distribution mapping of the prepared jackfruit shell-textured nickel-supported platinum-loaded nickel hydroxide electrode is shown, which includes all the nickel elements in the nickel support and the surface nickel hydroxide, forming a spatially confined carrier.

[0137] Figure 4 The platinum element distribution mapping of the prepared jackfruit shell-shaped nickel-supported platinum-loaded nickel hydroxide electrode is shown. The surface platinum element is uniform without obvious element segregation, and the platinum content is about 0.45at% (atomic percentage).

[0138] Figure 5 The overlay diagram of the nickel and platinum multi-element distribution of the prepared jackfruit shell-like nickel-supported platinum-loaded nickel hydroxide electrode shows the platinum element evenly distributed on the nickel hydroxide carrier particle structure, that is, the platinum catalyst is in situ grown on the surface of the micron-sized granular nickel hydroxide, indicating that the nickel hydroxide carrier has effective spatial confinement for the platinum catalyst.

[0139] Figure 6 The particle size statistics of the prepared jackfruit shell-like nickel-supported platinum-loaded nickel hydroxide electrode are shown. The surface platinum-loaded nickel hydroxide particles tend to be normally distributed between 0.7-1.4 microns, and the average particle size is about 1 micron. Compared with the nickel support, the surface platinum-loaded nickel hydroxide particles have a larger specific surface area.

[0140] Figure 7 The water contact angle test results of the jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode are shown. Compared with Comparative Example 1, the water contact angle of the platinum-loaded nickel hydroxide supported by the jackfruit shell-shaped nickel is 1.04°, which has an excellent wetting effect, and therefore has better hydrophilicity and air repellency during the electrolysis reaction.

[0141] Figure 8 The catalytic performance of the jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode in the alkaline water electrolysis hydrogen production reaction in 1 mol / L KOH electrolyte was demonstrated. The jackfruit shell-shaped FN / Pt-Ni(OH)x produced 100 mA / cm 2 At a current density of , the overpotential is only 243 mV, which is 211 mV lower than that of Comparative Example 1. The catalytic activity is higher and the energy consumption for hydrogen production is lower.

[0142] Fig. 9 The stability of the prepared jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode in 30% KOH electrolyte was demonstrated. Under industrial conditions of 80°C, the jackfruit shell-shaped FN / Pt-Ni(OH)x alkaline water electrolysis hydrogen production electrode was 3000A / m 2 It runs stably for 10 hours at the current density without obvious attenuation.

[0143] The working principle of the present invention is:

[0144] In the present invention, by selecting the optimal nickel source, the first electrolyte formula formed by the first solvent and citric acid, and accurately controlling the first electrochemical deposition process parameters such as the electrodeposition temperature, the electrolyte stirring speed, the constant current density, and the deposition time, the formation of the jackfruit shell-like surface morphology of nickel hydroxide is precisely controlled, and a uniform and continuous nickel hydroxide confined carrier island is obtained on the nickel support. By selecting the optimal platinum source, the second solvent and the sodium tartrate formed by the second electrolyte formula, and the second electrochemical deposition process parameters such as the scanning rate and the cycle period, the platinum atoms are effectively restricted to be uniformly and stably dispersed on the surface of the nickel hydroxide carrier, and a nickel-supported platinum-loaded nickel hydroxide electrode with jackfruit shell texture is obtained. While the electrode improves the overall conductivity of the catalytic layer in the alkaline water electrolysis hydrogen production reaction, the confined space promotes the orderly migration of adsorbed hydrogen species on different active sites of platinum and nickel hydroxide in the nickel-supported platinum-loaded nickel hydroxide electrode, thereby enhancing the hydrogen overflow effect and thus strengthening the hydrogen evolution reaction process.

Claims

1. A jackfruit shell-shaped alkaline water electrolysis hydrogen production electrode, comprising a nickel support, characterized in that: Micron-sized granular nickel hydroxide is evenly distributed on the surface of the nickel support, and a platinum catalyst is in-situ grown on the surface of the micron-sized granular nickel hydroxide.

2. The alkaline water electrolysis hydrogen production electrode according to claim 1, characterized in that: The particle size of the micron-sized granular nickel hydroxide is in the range of 0.7 to 1.4 microns, and the micron-sized granular nickel hydroxide has a jackfruit shell grain structure.

3. A method for preparing an alkaline water electrolysis hydrogen production electrode as claimed in claim 1 or 2, characterized in that: The following steps are involved: Step 1: Add a nickel source compound and citric acid to a first solvent in sequence, and stir until completely dissolved to form a first electrolyte; Step 2: immersing the nickel support into the first electrolyte in step 1 to perform a first electrochemical deposition to obtain a nickel-supported nickel hydroxide electrode (Ni / Ni(OH)x); Step 3: Add a platinum source compound and sodium tartrate to the second solvent in sequence, and stir until completely dissolved to form a second electrolyte; Step 4: immersing the nickel-supported nickel hydroxide electrode (Ni / Ni(OH)x) in step 2 into the second electrolyte in step 3 for a second electrochemical deposition to obtain a nickel-supported platinum-loaded nickel hydroxide electrode (Ni / Pt-Ni(OH)x); Preferably, in step 1 or step 3, the first solvent or the second solvent is any one or more of pure water, Tris buffer, Tris hydrochloric acid buffer, and isopropanol, and the first solvent or the second solvent may be the same or different; Preferably, the nickel source compound in step 1 is any one or more of nickel chloride, nickel nitrate, nickel sulfate, nickel sulfamate, and nickel acetate; Preferably, the nickel support in step 2 is any one of nickel foam, nickel mesh, and nickel felt; Preferably, the platinum source compound in step 3 is any one of chloroplatinic acid and dinitrosodiammineplatinum.

4. The preparation method according to claim 3, characterized in that: Step 1: The nickel source ion concentration in the first electrolyte is 0.05-0.2 mol / L, and the mass percentage of citric acid is 5-30 wt%; Preferably, the nickel source ion concentration in the first electrolyte is any one of 0.05 mol / L, 0.1 mol / L, 0.15 mol / L or 0.2 mol / L; Preferably, the mass percentage of citric acid in the first electrolyte is any one of 5wt%, 10wt%, 20wt% or 30wt%.

5. The preparation method according to claim 3, characterized in that: Before immersing the nickel support in the first electrolyte, the nickel support is first immersed in a 1 mol / L hydrochloric acid solution for ultrasonic cleaning for 1-20 min to remove surface oxides and other impurities, and then the nickel support after ultrasonic cleaning is rinsed with ultrapure water and vacuum dried.

6. The preparation method according to claim 3, characterized in that: Step 2 The specific process of the first electrochemical deposition is: using a three-electrode system, the nickel support is used as the cathode and anode respectively, silver / silver chloride is used as the reference electrode, the cathode, anode and reference electrode are immersed in the first electrolyte, and the nickel source ions in the first electrolyte are deposited at a constant current by using multiple current steps, and the reaction system temperature in the first electrochemical deposition is controlled to be 20-50°C, the stirring speed in the first electrolyte is 200-600r / min, and the constant current density is 5-30mA / cm 2 The first deposition time is 10 to 90 minutes, and after the first electrochemical deposition is completed, a nickel-supported nickel hydroxide electrode is obtained; Preferably, the temperature of the reaction system is any one of 20°C, 30°C, 40°C, and 50°C; Preferably, the stirring speed in the first electrolyte is any one of 200r / min, 300r / min, 400r / min, 500r / min, and 600r / min; Preferably, the constant current density is 5 mA / cm 2 , 10mA / cm 2 , 20mA / cm 2 、30mA / cm 2 Any value in ; Preferably, the first deposition time is any one of 10 min, 30 min, 60 min and 90 min.

7. The preparation method according to claim 3, characterized in that: Step 3: The concentration of platinum source ions in the second electrolyte is 0.02-0.1 mol / L, and the mass percentage of sodium tartrate is 5%-30wt%; Preferably, the concentration of platinum source ions in the second electrolyte is any one of 0.02 mol / L, 0.04 mol / L, 0.06 mol / L, 0.08 mol / L, and 0.1 mol / L; Preferably, the mass percentage of sodium tartrate in the second electrolyte is any one of 5wt%, 10wt%, 20wt% and 30wt%.

8. The preparation method according to claim 3, characterized in that: Step 4: The specific process of the second electrochemical deposition is: using a three-electrode system, using the nickel-supported nickel hydroxide electrode as a cathode, and a platinum sheet electrode as an anode, the cathode and the anode are immersed in a second electrolyte, and using cyclic voltammetry to perform electroreduction limited deposition on the platinum source ions in the second electrolyte, and controlling the voltage range of the second electrochemical deposition to be 0 to -0.5V, the scanning rate to be 50 to 200mV / s, and the cycle period to be 20 to 100 circles; Preferably, the scanning rate is any one of 50mV / s, 100mV / s, 150mV / s, and 200mV / s; Preferably, the cycle period is any value among 20 circles, 40 circles, 60 circles, 80 circles, and 100 circles.

9. The preparation method according to claim 3, characterized in that: The following steps are involved: Step 9.1: Add nickel sulfate and citric acid to a 1 mol / L, pH=8.5 Tris buffer, and stir until completely dissolved to obtain a first electrolyte with a nickel sulfate concentration of 0.1 mol / L and a citric acid mass percentage of 10 wt%; Step 9.2: Using the three-electrode system of the Chenhua electrochemical workstation, take two pre-treated commercial foam nickel (FN) and clamp them with platinum electrode clamps, respectively as cathode and anode, and silver / silver chloride as reference electrode. Add the first electrolyte in step 9.1 until the pre-treated FN is submerged 1 cm below the first electrolyte. 2 and put in a stirrer; set the water bath temperature of the first electrolyte in the electrolytic cell to 40°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 200r / min; select multiple current steps (ISTEP), set the current size to 0.01A, that is, the constant current density is 10mA / cm 2 After 60 min of deposition, the FN after cathode pretreatment was removed, rinsed with pure water and vacuum dried to obtain a nickel hydroxide electrode supported by nickel foam (FN / Ni(OH)x); Step 9.3: Add chloroplatinic acid and sodium tartrate to pure water, and stir until completely dissolved to obtain a second electrolyte with a chloroplatinic acid concentration of 0.08 mol / L and a sodium tartrate mass percentage of 5 wt%; Step 9.4: Using the three-electrode system of Chenhua electrochemical workstation, the FN / Ni(OH)x obtained in step 9.2 was clamped with a platinum electrode clamp as the cathode, the platinum electrode as the anode, and silver / silver chloride as the reference electrode. The second electrolyte in step 9.3 was added until the FN / Ni(OH)x was submerged 1 cm below the second electrolyte. 2 And put in a stirring bar; set the water bath temperature of the second electrolyte in the electrolytic cell to 30°C, and stabilize it for 30 minutes after reaching temperature; adjust the magnetic stirring speed to 600r / min; use cyclic voltammetry (CV) with a voltage range of 0 to -0.5V and a scan rate of 50mV / s. After 20 cycles, remove the cathode FN / Ni(OH)x, rinse with pure water and vacuum dry to obtain a foam nickel-supported platinum-loaded nickel hydroxide electrode (FN / Pt-Ni(OH)x).

10. Use of the alkaline water electrolysis hydrogen production electrode as claimed in claim 1 or 2 in alkaline water electrolysis hydrogen production.

Citation Information

Patent Citations

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