CN113823803B - Proton exchange membrane fuel cell gas diffusion layer-rGO @ Ni/Ni foam Preparation method and application of - Google Patents
Proton exchange membrane fuel cell gas diffusion layer-rGO @ Ni/Ni foam Preparation method and application of Download PDFInfo
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- CN113823803B CN113823803B CN202110991332.0A CN202110991332A CN113823803B CN 113823803 B CN113823803 B CN 113823803B CN 202110991332 A CN202110991332 A CN 202110991332A CN 113823803 B CN113823803 B CN 113823803B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8807—Gas diffusion layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0234—Carbonaceous material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0241—Composites
- H01M8/0245—Composites in the form of layered or coated products
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a preparation method and application of a gas diffusion layer-rGO @ Ni/Nifoam of a proton exchange membrane fuel cell. In a three-electrode electrochemical cell, hydrogen bubbles are used as a template, and three-dimensional nickel nano particles are electrodeposited on foamed nickel by an electrodeposition method; soaking foamed nickel with nickel nanoparticles into graphene oxide aqueous solution for reaction, and reducing graphene oxide in situ by using three-dimensional nickel particles to form rGO @ Ni/Ni foam And (3) obtaining the product. According to the invention, nickel nanoparticles can be deposited on the surface of the foamed nickel, the reduction degree of the graphene oxide is high, and the contact resistance between the gas diffusion layer and the collector plate can be effectively reduced. Compared with the method of directly reducing the graphene oxide by using the foam nickel (skeleton), the method does not corrode the foam nickel substrate. Compared with a reducing agent method for reducing graphene oxide, the method does not involve intervention of a toxic reducing agent, and is high in safety and strong in operability.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to a gas diffusion layer-rGO @ Ni/Ni of a proton exchange membrane fuel cell foam The preparation method and the application thereof.
Background
Proton Exchange Membrane Fuel Cells (PEMFC) use polymeric membranes as solid electrolytes, have the characteristics of high energy conversion rate, low-temperature starting, no electrolyte leakage and the like, and are widely applied to the fields of heavy trucks, aerospace, military and the like. Due to the many advantages of pem fuel cells, the interest is increasing. The gas diffusion layer of the proton exchange membrane fuel cell mostly uses carbon paper and carbon cloth, and plays roles of gas diffusion and electron conduction in the proton exchange membrane fuel cell. The traditional gas diffusion layer has the defects of easy corrosion, large substance transmission resistance and the like. Meanwhile, the physical support effect of the gas diffusion layer with high porosity and high conductivity on the catalyst can improve the utilization rate of the noble metal platinum catalyst and reduce the reactant transmission resistance, thereby improving the performance of the fuel cell. Therefore, a novel gas diffusion layer-rGO @ Ni/Ni of proton exchange membrane fuel cell is provided foam The preparation method has important significance for replacing the traditional gas diffusion layer at present.
Graphene is a novel carbon material formed by tightly stacking single-layer carbon atoms and has a two-dimensional hexagonal honeycomb crystal structure. Graphene is widely used in the technical field of fuel cells due to its excellent chemical and thermodynamic stability, as well as physical and mechanical properties. Graphene has an ultra-large specific surface area due to its unique two-dimensional structure. Also, single-layer graphene is an excellent thermal conductor under room temperature conditions, exhibits high electron mobility, and the like. Thus, graphene is a potentially desirable species.
In the prior art, the ultra-light material and the majordomo and the like in a surface technology key laboratory utilize iron powder to directly reduce graphene oxide at room temperature, and successfully synthesize graphene nanosheets on the surface. The method creates conditions for efficient, environment-friendly and large-scale production of the graphene nanosheets, and simultaneously provides a certain foundation for direct reduction of graphene oxide by other metal nanoparticles such as nickel nanoparticles.
In addition, the invention patents CN103680974A, CN103545121A and CN103258656A propose different methods for reducing graphene oxide by foamed nickel: firstly, obtaining the foamed nickel deposited with the graphene oxide by a soaking mode, and then performing a reduction reaction by adopting an electrode method, ascorbic acid or a high-temperature heating method so as to reduce the graphene oxide into graphene and deposit the graphene on the surface of the foamed nickel. However, the above-mentioned experimental scheme requires additional complicated steps for the reduction reaction, requires expensive experimental equipment (tube furnace) or creates special experimental environment during the experimental reaction, and thus greatly limits the implementation of the experimental scheme. The preparation method of the direct soaking reaction type foam nickel-graphene three-dimensional porous electrode provided in CN106803461A can quickly complete the reduction reaction of graphene oxide through a simple and conveniently controlled soaking process, but the reaction interface is in a smooth nickel skeleton. And nickel nanoparticles are obtained on the framework through foam nickel electrodeposition, and compared with the foam nickel framework, the nickel nanoparticles have larger specific surface area, so that the reduced graphene oxide product has higher quality.
Disclosure of Invention
In order to overcome the defects of the prior art and to overcome the needs of improvement, the invention aims to provide a gas diffusion layer-rGO @ Ni/Ni of a proton exchange membrane fuel cell foam The preparation method and the application thereof. Compared with the prior experimental scheme that various reduction reactions are performed after the graphene oxide-foamed nickel composite material is obtained and the reduction reaction is completed by directly soaking foamed nickel in graphene oxide. The invention electrodeposits three-dimensional nickel nano particles by three electrodes formed by placing a foamed nickel working electrode, a platinum foil counter electrode and a saturated silver/silver chloride reference electrode in a deposition solution of ammonium chloride and nickel chloride, completes reduction reaction by a simple and easily controlled soaking process, and finally forms rGO @ Ni/Ni foam And (4) obtaining a product. In the process of reaction between the nickel nanoparticles and the graphene oxide, the overall reaction rate is greatly improved, the reduction of the adhesion of the graphene oxide is facilitated, and the method has the advantages of simplicity, easy control and safety.
Proton exchange membrane fuel cell gas diffusion layer-rGO @ Ni/Ni foam The preparation method and the application are characterized in that: the preparation process mainly comprises the steps of foam nickel pretreatment, three-electrode electrodeposition and in-situ reductionAnd (3) graphene protoxide.
The foam nickel pretreatment method comprises the following steps: degreasing the foamed nickel by using acetone, etching the foamed nickel for 15 minutes by using dilute hydrochloric acid, washing by using deionized water and drying; after being fully soaked in nickel chloride for 4 hours, the mixture is fully washed by deionized water and dried.
The three-electrode electrodeposition method comprises the following steps: and placing the foamed nickel working electrode, the platinum foil counter electrode and the silver/silver chloride reference electrode in a deposition solution of 1.0-3.0 mol/L ammonium chloride and 0.05-0.2 mol/L nickel chloride to form the three-electrode electrochemical cell. Electrochemical workstation (electrochemical workstation PGSTAT 302) application of 0.5A/cm 2 ~3.0A/cm 2 The constant current is 50-200 seconds, and three-dimensional nickel nano particles are electrodeposited on the foamed nickel to obtain Ni/Ni foam And (3) obtaining the product.
The in-situ graphene oxide reduction method comprises the following steps: ni/Ni foam Directly soaking the graphene oxide in an oxidized graphene aqueous solution with the mass concentration of 0.5 mg/mL-10 mg/mL and the pH value of 1-8. Control of Ni/Ni foam The reaction temperature for reducing the graphene oxide is 30-100 ℃, and the reaction time is 2-12 hours. In this way, graphene oxide is Ni/Ni soaked in the soaking process foam In-situ reduction, namely, the reduced graphene oxide is adsorbed on the surface of the three-dimensional nickel nanoparticle to finally form rGO @ Ni/Ni foam And (3) obtaining the product.
Through the steps, the foam nickel treated by electrodeposition directly reacts with the graphene oxide in the soaking process, so that the reduction reaction can be completed through a simple, easily-controlled and safe soaking process, and the overall reaction efficiency is greatly improved. Obtained rGO @ Ni/Ni foam The product has good reaction gas diffusion performance, so the product is particularly suitable for the material of the gas diffusion layer of the proton exchange membrane fuel cell.
More preferably, the concentration of ammonium chloride is most preferably 2mol/L, the concentration of nickel chloride is most preferably 0.1mol/L, and the current density is most preferably 1.0A/cm 2 The electrodeposition time is most preferably 100 seconds.
Further preferably, in the step (c), the graphene oxide solution is prepared by preferentially oxidizing exfoliated graphene by a modified Hummers method, and the mass concentration of the prepared graphene oxide solution is set to be 1mgmL-1 to 2.5mg mL-1.
As a further preference, the in situ reduction of graphene oxide: ni/Ni foam Directly soaking the graphene oxide in an oxidized graphene aqueous solution with the mass concentration of 0.5 mg/mL-10 mg/mL and the pH value of 1-8. Control of Ni/Ni foam The reaction temperature for reducing the graphene oxide is 30-100 ℃, and the reaction time is 2-12 hours.
More preferably, the graphene oxide is prepared by an improved Hummers oxidation method, the mass concentration is more preferably 0.5 mg/mL-2 mg/mL, and the pH value of the solution is further optimized to be 1-3.
More preferably, the reaction temperature is preferably 70 ℃ to 90 ℃, and the soaking time is preferably 6 hours to 8 hours.
More preferably, the reaction temperature is most preferably 80 ℃ and the soaking time is most preferably 7 hours.
As a further preference, the rgo @ ni/nickel foam product described above is preferred as a gas diffusion layer for a proton exchange membrane fuel cell.
Compared with the prior art, the invention has the following advantages and beneficial effects:
hydrogen bubbles are taken as a template, three-dimensional porous nickel nano particles are electrodeposited on the foamed nickel, and the three-dimensional porous nickel nano particles play a role in reduction in the process of reacting with the graphene oxide. Ni/Ni foam The product has larger specific surface area compared with the foam nickel. Because the nickel particles protrude to form gaps, the graphene oxide can easily obtain the surfaces of the nickel particles, and has a larger reaction interface, so that the reduction reaction can be completed through a simple, easily controlled and safe soaking process.
rGO @ Ni/Ni obtainable according to the invention foam The product has good performance. The reaction process is simple and easy to control, so that rGO @ Ni/Ni foam The material is especially suitable for gas diffusion layers of proton exchange membrane fuel cells.
Drawings
FIG. 1 is rGO @ Ni/Ni provided in embodiment 1 of the present invention foam The preparation method of (1).
Fig. 2 is a schematic structural diagram of a pem fuel cell.
FIG. 3 is the product rGO @ Ni/Ni obtained in example 1 foam The proton exchange membrane fuel cell which is taken as a proton exchange membrane fuel cathode gas diffusion layer as an experimental group and takes carbon cloth as the gas diffusion layer is compared, namely a single cell polarization curve and a power density curve are compared.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following description is given with reference to the accompanying drawings and examples, but the present invention is not limited thereto. It is noted that the processes described below, if not specifically detailed, are all those that can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
Firstly, a foamed nickel substrate (length × width × thickness =20 × 20 × 0.5 mm, 110ppi,320g m) is selected -2 (ii) a China changsha lei ru materials ltd), firstly, acetone is used for degreasing the foamed nickel, then 0.006mol/mL dilute hydrochloric acid is used for etching the foamed nickel for 15 minutes, deionized water is used for fully washing and drying, and then 0.0001mmol/mL nickel chloride is used for fully washing after being soaked for 4 hours.
Next, electrodeposition was performed in a three-electrode electrochemical cell with a platinum foil counter electrode and a saturated silver/silver chloride reference electrode using foamed nickel as the working electrode, 2.0mol/L ammonium chloride, and 0.1mol/L nickel chloride as the deposition solutions. Three-dimensional nickel nanoparticles were electrodeposited on the nickel foam by applying a constant current of 1.0A/cm through an electrochemical workstation (electrochemical workstation PGSTAT 302) for 100 seconds.
Then, obtaining graphene oxide by adopting an improved Hummers oxidation method, wherein the specific process is as follows: taking 1g of natural flake graphite powder, stirring and mixing the natural flake graphite powder with concentrated sulfuric acid and phosphoric acid under an ice bath condition, wherein the volume ratio of the concentrated sulfuric acid to the phosphoric acid is 9.
And then, washing the nickel foam subjected to electrodeposition treatment with deionized water, drying, and soaking into the graphene oxide aqueous solution, wherein nickel nanoparticles electrodeposited on the nickel foam reduce graphene oxide in the solution, and the graphene oxide undergoes a reduction reaction. As another key reaction condition of the invention, the reaction temperature of the foam nickel reduction graphene oxide subjected to the electrodeposition treatment is controlled to be 80 ℃, and the soaking time is 7 hours. In the process, nickel nanoparticles electrically deposited on the foamed nickel react with the graphene oxide solution to gradually deposit and grow graphene on the nickel nanoparticles of the foamed nickel, the foamed nickel is taken out after the reaction is finished, and the surface is cleaned by deionized water to form rGO @ Ni/Ni foam And (3) obtaining the product.
Example 2
Firstly, a foam nickel substrate (length multiplied by width multiplied by thickness =20 multiplied by 0.5 mm, 110PPI,320g m-2; changsha lei Run materials Co., ltd., china) is selected, firstly, acetone is used for degreasing the foam nickel, then 0.006mol/mL diluted hydrochloric acid is used for etching the foam nickel for 15 minutes, deionized water is used for fully washing and drying the foam nickel, and then 0.0001mmol/mL nickel chloride is used for fully washing with deionized water after being soaked for 4 hours.
Next, electrodeposition was performed in a three-electrode electrochemical cell with a platinum foil counter electrode and a saturated silver/silver chloride reference electrode using foamed nickel as the working electrode, 2.0mol/L ammonium chloride, and 0.1mol/L nickel chloride as the deposition solutions. Three-dimensional nickel nanoparticles were electrodeposited on the nickel foam by applying a constant current of 1.0A/cm through an electrochemical workstation (electrochemical workstation PGSTAT 302) for 100 seconds.
Then, obtaining graphene oxide by adopting an improved Hummers oxidation method, wherein the specific process is as follows: taking 1g of natural flake graphite powder, stirring and mixing the natural flake graphite powder with concentrated sulfuric acid and phosphoric acid under an ice bath condition, wherein the volume ratio of the concentrated sulfuric acid to the phosphoric acid is 9.
And then, washing the nickel foam subjected to electrodeposition treatment with deionized water, drying, and soaking in the graphene oxide aqueous solution, wherein nickel nanoparticles electrodeposited on the nickel foam reduce graphene oxide in the solution, and the graphene oxide undergoes a reduction reaction. As another key reaction condition of the method, the reaction temperature of the nickel foam for reduction of the graphene oxide by the electrodeposition treatment is controlled to be 100 ℃, and the soaking time is controlled to be 6 hours. In the process, nickel nanoparticles electrically deposited on the foamed nickel react with the graphene oxide solution, the nickel nanoparticles are gradually deposited on the nickel nanoparticles of the foamed nickel to grow into graphene, the foamed nickel is taken out after the reaction is finished, and the surface is cleaned by deionized water, so that an rGO @ Ni/Nifoam product is formed.
Example 3
Firstly, a foamed nickel substrate (length multiplied by width multiplied by thickness =20 multiplied by 0.5 mm, 110PPI,320g m) is selected -2 (ii) a China changsha lei ru materials ltd), firstly, acetone is used for degreasing the foamed nickel, then 0.006mol/mL dilute hydrochloric acid is used for etching the foamed nickel for 15 minutes, deionized water is used for fully washing and drying, and then 0.0001mmol/mL nickel chloride is used for fully washing after being soaked for 4 hours.
Next, electrodeposition was performed in a three-electrode electrochemical cell with a platinum foil counter electrode and a saturated silver/silver chloride reference electrode using foamed nickel as the working electrode, 2.0mol/L ammonium chloride, and 0.1mol/L nickel chloride as the deposition solutions. Three-dimensional nickel nanoparticles were electrodeposited on the nickel foam by applying a constant current of 0.5A/cm through an electrochemical workstation (electrochemical workstation PGSTAT 302) for 200 seconds.
Then, obtaining graphene oxide by adopting an improved Hummers oxidation method, wherein the specific process is as follows: taking 1g of natural crystalline flake graphite powder, stirring and mixing the natural crystalline flake graphite powder with concentrated sulfuric acid and phosphoric acid under an ice bath condition, wherein the volume ratio of the concentrated sulfuric acid to the phosphoric acid is 9.
And then, washing the nickel foam subjected to electrodeposition treatment with deionized water, drying, and soaking in the graphene oxide aqueous solution, wherein nickel nanoparticles electrodeposited on the nickel foam reduce graphene oxide in the solution, and the graphene oxide undergoes a reduction reaction. As another key reaction condition of the invention, the reaction temperature of the foam nickel reduction graphene oxide subjected to the electrodeposition treatment is controlled to be 80 ℃, and the soaking time is 7 hours. In the process, nickel nanoparticles electrically deposited on the foamed nickel react with the graphene oxide solution to gradually deposit and grow graphene on the nickel nanoparticles of the foamed nickel, the foamed nickel is taken out after the reaction is finished, and the surface is cleaned by deionized water to form rGO @ Ni/Ni foam And (4) obtaining a product.
Example 4
Firstly, a foamed nickel substrate (length multiplied by width multiplied by thickness =20 multiplied by 0.5 mm, 110PPI,320g m) is selected -2 (ii) a China changsha rei material ltd), firstly, acetone is used for degreasing the foamed nickel, then the foamed nickel is etched by using 0.006mol/mL dilute hydrochloric acid for 15 minutes, then deionized water is used for fully washing and drying, and then 0.0001mmol/mL nickel chloride is used for fully washing after being soaked for 4 hours.
Next, electrodeposition was performed in a three-electrode electrochemical cell with a platinum foil counter electrode and a saturated silver/silver chloride reference electrode using foamed nickel as the working electrode, 2.0mol/L ammonium chloride, and 0.1mol/L nickel chloride as the deposition solutions. Three-dimensional nickel nanoparticles were electrodeposited on the nickel foam by applying a constant current of 3.0A/cm through an electrochemical workstation (electrochemical workstation PGSTAT 302) for 50 seconds.
Then, obtaining graphene oxide by adopting an improved Hummers oxidation method, wherein the specific process is as follows: taking 1g of natural crystalline flake graphite powder, stirring and mixing the natural crystalline flake graphite powder with concentrated sulfuric acid and phosphoric acid under an ice bath condition, wherein the volume ratio of the concentrated sulfuric acid to the phosphoric acid is 9.
And then, washing the nickel foam subjected to electrodeposition treatment with deionized water, drying, and soaking in the graphene oxide aqueous solution, wherein nickel nanoparticles electrodeposited on the nickel foam reduce graphene oxide in the solution, and the graphene oxide undergoes a reduction reaction. As another key reaction condition of the invention, the reaction temperature of the foam nickel reduction graphene oxide subjected to the electrodeposition treatment is controlled to be 80 ℃, and the soaking time is 7 hours. In the process, nickel nano particles electrodeposited on the foamed nickel react with the graphene oxide solution, the graphene is gradually deposited and grown on the nickel nano particles of the foamed nickel, the foamed nickel is taken out after the reaction is finished, and the surface is cleaned by deionized water, so that rGO @ Ni/Ni is formed foam And (3) obtaining the product.
Example 5
Taking a Nafion117 proton exchange membrane of 4cm multiplied by 4cm, the size of the active area is 4cm 2 The platinum-carbon catalyst of the anode and the cathode is 0.5mg/cm 2 The loading amount of the proton exchange membrane is respectively sprayed on the two sides of the proton exchange membrane. 2cm x 2cm of carbon cloth with a microporous layer was used as gas diffusion layers for the anode and cathode of the proton exchange membrane fuel cell. Respectively hot-pressing an anode gas diffusion layer, an anode catalyst layer, a proton exchange membrane, a cathode catalyst layer and a cathode gas diffusion layer together in a sandwich manner, wherein the hot-pressing conditions are as follows: hot pressing pressure is 1MPa, hot pressing time is 90 seconds, and a product membrane electrode is obtained. The obtained membrane electrode, collector plate and end plate were assembled together to obtain a hydrogen fuel cell.
The battery temperature is operated at room temperature, the battery performance test conditions are as follows under the conditions that the anode is completely humidified and the cathode is self-breathing: the fuel gas is hydrogen, the oxidant is air, the anode backpressure is 0.16MPa, and the anode relative humidity is 100%. The cell polarization curve and the power density curve are shown in FIG. 3, and the current density can reach 45mA/cm respectively at a voltage of 0.347V 2 Maximum power density of 15.6mW/cm 2 。
Example 6
rGO @ Ni/Ni obtained in example 1 for cathode gas diffusion layer removal foam The procedure was the same as in example 2 except that a carbon black microporous layer was sprayed instead.
The battery temperature is operated at room temperature, the battery performance test conditions are as follows under the conditions that the anode is completely humidified and the cathode is self-breathing: the fuel gas is hydrogen, the oxidant is air, the anode backpressure is 0.16MPa, and the anode relative humidity is 100%. The polarization curve and the power density curve of the battery are shown in FIG. 3, and the current density can reach 115.1mA/cm respectively at a voltage of 0.5V 2 Maximum power density of 58.18mW/cm 2 。
The rGO @ Ni/Ni obtained in example 1 foam The product is used for a cathode gas diffusion layer and an anode gas diffusion layer of the proton exchange membrane fuel cell after being processed, carbon cloth is still used as an experimental group, and the anode gas diffusion layer and the cathode gas diffusion layer both adopt the carbon cloth as a control group. The anode and cathode catalyst (platinum carbon) loading of the experimental group and the control group are both 0.5mg/cm 2 。
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (3)
1. Proton exchange membrane fuel cell gas diffusion layer-rGO @ Ni/Ni foam The preparation method is characterized by comprising the following steps: the preparation process comprises the steps of nickel foam pretreatment, three-electrode electrodeposition and in-situ reduction of graphene oxide;
three electrode electro-depositionThe deposition method comprises the steps of placing a foamed nickel working electrode, a platinum foil counter electrode and a silver/silver chloride reference electrode in a deposition solution of 1.0-3.0 mol/L ammonium chloride and 0.05-0.2 mol/L nickel chloride to form a three-electrode electrochemical cell; electrochemical workstation application of 0.5A/cm 2 ~3.0A/cm 2 The constant current is 50-200 seconds, and three-dimensional nickel nano particles are electrodeposited on the foamed nickel to obtain Ni/Ni foam A product;
the method for reducing the graphene oxide in situ comprises the following steps: ni/Ni foam Directly soaking in graphene oxide aqueous solution for Ni/Ni foam Reducing and oxidizing graphene to obtain rGO @ Ni/Ni foam A product;
the mass concentration of the graphene oxide aqueous solution is 0.5 mg/mL-2 mg/mL;
the pH value of the graphene oxide aqueous solution is 1-3;
the temperature of the Ni/Nifoam reduction-oxidation graphene reaction is 70-90 ℃, and the time of the Ni/Nifoam reduction-oxidation graphene reaction is 6-8 hours.
2. The proton exchange membrane fuel cell as claimed in claim 1, wherein the gas diffusion layer is rgo @ Ni/Ni foam The preparation method is characterized in that the foam nickel pretreatment method comprises the steps of degreasing the foam nickel by using acetone, etching the foam nickel for 10-15 minutes by using dilute hydrochloric acid, washing by using deionized water and drying; soaking in nickel chloride for 3-5 hr, washing with deionized water, and oven drying.
3. The proton exchange membrane fuel cell gas diffusion layer-rGO @ Ni/Ni prepared by the method of claim 1 or 2 foam The application of (2), which is characterized in that: rGO @ Ni/Ni foam The product is used as cathode gas diffusion layer of proton exchange membrane fuel cell.
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| CN107904570A (en) * | 2017-11-07 | 2018-04-13 | 东南大学 | A kind of method for preparing nickel nano particle grapheme foam nickel material |
| CN110767879A (en) * | 2019-10-08 | 2020-02-07 | 天津大学 | Preparation method of nickel-zinc battery based on high-activity nickel anode |
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| CN104291324A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene foams |
| CN104600238B (en) * | 2014-12-22 | 2017-01-25 | 华中科技大学 | Method for preparing directly soaking reaction type foamed nickel-graphene three-dimensional porous electrode |
| CN105836735A (en) * | 2016-03-25 | 2016-08-10 | 西安电子科技大学 | Preparation method for ultra-three-dimension graphene |
| CN105742625B (en) * | 2016-04-15 | 2018-03-02 | 深圳赛骄阳能源科技股份有限公司 | Nano-electrode material with sandwich and its preparation method and application |
| WO2018165396A1 (en) * | 2017-03-08 | 2018-09-13 | Board Of Regents, The University Of Texas System | Dendritic materials with hierarchical porosity |
| US10815580B2 (en) * | 2017-08-10 | 2020-10-27 | Board Of Trustees Of The University Of Arkansas | 3D reduced graphene oxide foams embedded with nanocatalysts, synthesizing methods and applications of same |
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| CN107904570A (en) * | 2017-11-07 | 2018-04-13 | 东南大学 | A kind of method for preparing nickel nano particle grapheme foam nickel material |
| CN110767879A (en) * | 2019-10-08 | 2020-02-07 | 天津大学 | Preparation method of nickel-zinc battery based on high-activity nickel anode |
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