Method for preparing high-performance AEM water electrolysis hydrogen production membrane electrode

By employing a hydrophobically modified diffusion layer and anion exchange resin solution in the AEM water electrolysis hydrogen production membrane electrode, the problems of catalyst layer shedding and aggregation were solved, the stability and catalytic activity of the membrane electrode were improved, and efficient water electrolysis hydrogen production performance was achieved.

CN121496433APending Publication Date: 2026-02-10JIANGSU LONGPAN HYDROGEN ENERGY TECH CO LTD +1

Patent Information

Application Number
CN202511552718.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-10-28
Publication Date
2026-02-10

AI Technical Summary

Technical Problem

In existing AEM water electrolysis hydrogen production membrane electrodes, the catalyst layer is prone to detachment and catalyst particle agglomeration, resulting in reduced catalytic capacity. Existing modified gas diffusion layers have failed to effectively solve the problems of oxygen bubble retention and catalyst layer stability.

Method used

A hydrophobically modified diffusion layer is combined with anion exchange resin solution. By adding the anion exchange resin solution and hydrophobic binder stepwise, a continuous hydrophilic channel is formed, which avoids catalyst aggregation and shedding, and improves the stability and activity of the membrane electrode.

Benefits of technology

This reduces oxygen bubble retention while improving the stability and catalytic activity of the membrane electrode, thus enhancing the electrode's transport efficiency and lifespan.

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Abstract

The invention discloses a method for preparing a high-performance AEM water-electrolyzed hydrogen production membrane electrode, which comprises the following steps: respectively preparing an AEM water-electrolyzed hydrogen production anode and an AEM water-electrolyzed hydrogen production membrane cathode, then placing the AEM water-electrolyzed hydrogen production anode and the AEM water-electrolyzed hydrogen production cathode on two sides of an anion exchange membrane, and sealing edges to prepare the AEM water-electrolyzed hydrogen production membrane electrode, the preparation method comprises the following steps: mixing catalyst powder with a solvent to prepare catalyst prefabricated slurry, adding an anion exchange resin solution in batches, adding a hydrophobic binder to prepare catalyst slurry, coating the surface of a hydrophobic modified diffusion layer with the slurry, and finally coating the surface of the diffusion layer with the anion exchange resin solution to prepare the hydrophobic modified diffusion layer. And soaking in an organic solvent, and washing. According to the prepared AEM water electrolysis hydrogen production membrane electrode, on the basis that oxygen bubble retention can be reduced, the stability is improved, and meanwhile the activity of the membrane electrode is improved.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of preparation of AEM electrolytic water hydrogen membrane electrode. BACKGROUND

[0002] Electrolytic water hydrogen production technology mainly includes alkaline electrolytic water hydrogen production technology (ALK), proton exchange membrane (PEM) electrolytic water hydrogen production technology, anion exchange membrane (AEM) electrolytic water hydrogen production technology and solid oxide electrolytic water hydrogen production technology (SOEC). Among them, AEM electrolytic water combines the advantages of low cost of ALK and high efficiency and high convenience of PEM electrolytic water, and becomes the latest developed electrolytic water hydrogen production technology. AEM electrolysis tank, as a device for converting electrical energy into chemical energy, is the core component of AEM electrolytic water hydrogen production system. AEM electrolysis tank is mainly composed of end plate, bipolar plate, gas diffusion layer, AEM, membrane electrode and the like.

[0003] Among them, the membrane electrode is the core component of the anion exchange membrane electrolysis tank, and the AEM electrolytic water hydrogen membrane electrode (Membrane Electrode Assembly, MEA) adopts a sandwich type hierarchical structure, which is composed of a gas diffusion layer (Gas Diffusion Layer, GDL), a catalyst layer (Catalyst Layer, CL) and an anion exchange membrane.

[0004] The prior art, application number 202510477674.9, named "AEM electrolytic water hydrogen anode gas diffusion layer, preparation method and application" discloses that the gas diffusion layer body substrate is modified by using a modified reagent, thereby solving the problems of low mechanical strength, easy corrosion and difficult oxygen bubble discharge of the gas diffusion layer.

[0005] Based on this, the modified gas diffusion layer is used to prepare the membrane electrode in the test process. The membrane electrode preparation method is divided into CCS method and CCM method. Due to the swelling problem of AEM membrane, there are few reports on the membrane electrode made by CCM method on the AEM membrane. The CCS method is obtained by directly spraying or coating the catalyst active component on the diffusion layer. Since the catalyst layer is in a bare state, with the progress of electrolytic water hydrogen production, the catalyst layer is easy to fall off, and the catalyst particles in the catalyst layer will gradually agglomerate, so that the effective active area of the catalyst layer is continuously reduced, and the catalytic ability is gradually reduced.

[0006] Based on this, the present research is to study a preparation process of AEM electrolytic water hydrogen membrane electrode which can effectively avoid catalyst agglomeration and falling off. SUMMARY

[0007] Technical problems solved by the application: The technical problems to be solved by the application are to provide a preparation method of an AEM water electrolysis hydrogen production membrane electrode, which is based on the use of a modified diffusion layer to reduce the retention of oxygen bubbles, and can effectively avoid catalyst particle agglomeration and falling, and further improve the activity of the catalyst layer.

[0008] Technical scheme: The method for preparing a high-performance AEM water electrolysis hydrogen production membrane electrode comprises the following steps:

[0009] (1) Preparation of an AEM water electrolysis hydrogen production anode:

[0010] 1) Mix the anode catalyst powder with the solvent and ball mill to form anode catalyst pre-slurry;

[0011] 2) Add anion exchange resin solution to the anode catalyst pre-slurry in portions, mix into slurry under ultrasonic, then add a hydrophobic binder, shear mix, and prepare anode catalyst slurry;

[0012] 3) Apply the anode catalyst slurry prepared in step 2) to the surface of the hydrophobically modified diffusion layer, dry to prepare a diffusion layer A coated with anode catalyst;

[0013] 4) Coat the surface of the diffusion layer A prepared in step 3) with anion exchange resin solution to obtain a diffusion layer B with anion exchange membrane resin coating, and immerse it in an organic solvent to prepare an AEM water electrolysis hydrogen production anode;

[0014] (2) Preparation of an AEM water electrolysis hydrogen production membrane electrode:

[0015] Place the AEM water electrolysis hydrogen production anode prepared in step 4) and the AEM water electrolysis hydrogen production cathode on both sides of the anion exchange membrane and edge seal to prepare an AEM water electrolysis hydrogen production membrane electrode.

[0016] Further, the cathode of the AEM water electrolysis hydrogen production membrane electrode can also be prepared by the following steps:

[0017] 1) Mix the cathode catalyst powder with the solvent and ball mill to form cathode catalyst pre-slurry;

[0018] 2) Add anion exchange resin solution to the cathode catalyst pre-slurry in portions, mix into slurry under ultrasonic, then add a hydrophobic binder, shear mix, and prepare cathode catalyst slurry;

[0019] 3) Apply the cathode catalyst slurry prepared in step 2) to the surface of the hydrophobically modified diffusion layer, dry to prepare a diffusion layer C coated with cathode catalyst;

[0020] 4) coating the surface of the diffusion layer C prepared in step 3) with an anion exchange resin solution to obtain a diffusion layer D with an anion exchange membrane resin coating, and soaking in an organic solvent to obtain an AEM electrolytic water hydrogen production cathode.

[0021] In the anode preparation step 1) or the cathode preparation step 1) of the AEM electrolytic water hydrogen production membrane electrode of the present application, the solvent is deionized water and an organic solvent in a volume ratio of 1: (1-10), wherein the organic solvent is selected from ethanol, isopropanol, propylene glycol or acetone; and the amount of the solvent added is 1-5 times the mass of the anode catalyst powder or the cathode catalyst powder.

[0022] In the anode preparation step 4) or the cathode preparation step 4) of the AEM electrolytic water hydrogen production membrane electrode of the present application, the organic solvent is selected from ethanol, isopropanol, propylene glycol or acetone, and is consistent with the organic solvent used in step 1).

[0023] In the anode preparation step 2) or the cathode preparation step 2) of the AEM electrolytic water hydrogen production membrane electrode of the present application, the amount of the anion exchange resin solution added is 5-20% of the weight of the anode catalyst powder or the cathode catalyst powder, the time interval for adding in several times is 5-20 min, and the amount of each addition is 1 / 8-1 / 2 of the total amount of the anion exchange resin solution.

[0024] In the anode preparation step 2) or the cathode preparation step 2) of the AEM electrolytic water hydrogen production membrane electrode of the present application, the hydrophobic binder is selected from polytetrafluoroethylene, polyperfluoroethylene propylene or polyvinylidene fluoride, and the amount of the hydrophobic binder added is 0.1-2.5% of the total solid matter in the anode catalyst slurry or the cathode catalyst slurry.

[0025] In the anode preparation step 3) or the cathode preparation step 3) of the AEM electrolytic water hydrogen production membrane electrode of the present application, the hydrophobically modified diffusion layer is prepared by the following steps:

[0026] a. pretreating a diffusion layer with a porosity of 50-80%, then immersing in a modification reagent, reacting at 55-65 ℃ for 8-12 min, adding sodium dodecyl sulfate, continuing to immerse at 35-45 ℃ for 15-25 min and air drying to obtain a preliminarily modified gas diffusion layer;

[0027] b. reacting the preliminarily modified gas diffusion layer in an inert atmosphere at 600-800 ℃ for 1.5-2 h to obtain a hydrophobically modified diffusion layer.

[0028] Furthermore, in step a of preparing the hydrophobically modified diffusion layer, the modifying reagents include HCl solution, HNO3 solution and FeCl3 solution in a volume ratio of (40-55):(20-35):(10-25); the amount of sodium dodecyl sulfate added is such that its mass concentration in the modifying reagents reaches 0.4-0.6 wt%.

[0029] In step 4) of the anode preparation or cathode preparation of the AEM water electrolysis hydrogen production membrane electrode of the present invention, the coating thickness of the anion exchange resin solution on the surface of the diffusion layer A is 5-20 μm; the coating thickness of the anion exchange resin solution on the surface of the diffusion layer C is 5-20 μm.

[0030] In step 4) of the AEM water electrolysis hydrogen production membrane electrode of the present invention, the immersion time in the organic solvent is 20-90 s.

[0031] Beneficial Effects: Compared with the prior art, the significant advantage of this invention is that the AEM water electrolysis hydrogen production membrane electrode can improve stability and enhance the activity of the membrane electrode while reducing oxygen bubble retention. Specifically, the AEM water electrolysis hydrogen production membrane electrode employs a hydrophobic modified diffusion layer combined with an anion exchange resin solution coated on the surface of a catalyst-containing diffusion layer. The hydrophobic modified diffusion layer reduces oxygen bubble retention, while the anion exchange resin coating on the catalyst-containing diffusion layer improves stability (the anion exchange resin coating can interpenetrate with the organic solvent to form interconnected cross-linked channels, effectively increasing OH- ion exchange capacity). - To improve ion transport efficiency and minimize electrode material shedding under high electrical density conditions during activation and hydrogen evolution via water electrolysis, the hydrophilicity of the membrane electrode is increased to compensate for the low membrane electrode activity caused by hydrophobic modification of the diffusion layer.

[0032] On the other hand, based on the hydrophobic modified gas diffusion layer, anion exchange resin solution is added in stages, along with a hydrophobic binder. This allows the solution to be added in stages and uniformly dispersed in the slurry to form continuous hydrophilic channels. This avoids the problems of "local over-hydrophilicity (clogging pores) or under-hydrophilicity (disruption of ion conduction)" caused by the aggregation of anion exchange resin solution. At the same time, the introduction of a hydrophobic binder reduces the interfacial tension between the slurry and the hydrophobic modified diffusion layer substrate, preventing the slurry from shrinking and agglomerating on the hydrophobic substrate due to excessive hydrophilicity during coating. This ensures uniform spreading of the coating, effectively promotes uniform dispersion of the catalyst, avoids agglomeration, and further improves its activity. Attached Figure Description

[0033] Figure 1 These are AEM cell activity test diagrams for Embodiment 1 and Comparative Examples 1-4 of the present invention;

[0034] Figure 2 These are AEM cell activity test diagrams for Embodiment 2 and Comparative Example 5 of the present invention. Detailed Implementation

[0035] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

[0036] It should be noted that the anode catalyst powder used in this invention is any one or more of the known NiCoFe-LDH, NiFeB, NiFeS, and NiFeO. Preferably, the anode catalyst powder used in the following examples and comparative examples is NiCoFe-LDH, a known material, such as the anode material disclosed in application number 202510164054X. The cathode catalyst powder is a Pt / C powder with a platinum mass concentration of 20-60%. The anion exchange resin solution includes any one of the following: FAA-3-SOLUT-10, FAA-3-shredded film, I-250, and FAB-PK-130; I-250 is used in the examples and comparative examples. The CAS numbers or manufacturers of the raw materials are shown in Table 1 below.

[0037] Table 1. Sources of raw materials used in this invention

[0038]

[0039] The hydrophobically modified diffusion layer used in the following embodiments of the present invention is prepared by the following steps:

[0040] (1) Place the nickel felt substrate diffusion layer with a porosity of 50-80% and a thickness of 250 μm in acetone and ethanol in sequence, and ultrasonically clean it for 30 min respectively; rinse the ultrasonically cleaned gas diffusion layer with water and dry it to complete the pretreatment.

[0041] (2) Prepare a modifying agent by mixing a 10% HCl solution, a 1.0M HNO3 solution and a 1.2M FeCl3 solution. The volume ratio of the HCl solution, HNO3 solution and FeCl3 solution in the modifying agent is 50:30:20.

[0042] (3) The nickel felt substrate diffusion layer is immersed in the modifying agent and reacted at 60 °C for 10 min. Then sodium dodecyl sulfate is added to the modifying agent. The amount of sodium dodecyl sulfate added is such that its mass concentration in the modifying agent reaches about 0.5 wt%. The substrate is then immersed at 40 °C for 15 min.

[0043] (4) After the impregnation is completed, the nickel felt substrate diffusion layer is dried and placed in a mixture of CH4 and Ar gas. It is then treated at 700 °C for 2 h to obtain the modified nickel felt substrate diffusion layer. The flow ratio of CH4 to Ar in the mixture of CH4 and Ar gas is (1:5)-(1:20).

[0044] Furthermore, when preparing diffusion layer A or diffusion layer C in this invention, a layer with an area of ​​5 cm² is used. 2 The gas diffusion layer is placed on a ceramic heating plate and heated to 80°C. Then, using an ultrasonic spraying machine, the anode catalyst slurry or cathode catalyst slurry is uniformly sprayed onto the hydrophobic modified diffusion layer at a discharge rate of 10 μL / s. This spraying process is a common practice in the art, and therefore will not be described in detail in the following embodiments and comparative examples.

[0045] The preparation of the AEM electrolysis water-to-hydrogen cathode in the following embodiments and comparative examples of the present invention is the same as the preparation method of the AEM electrolysis water-to-hydrogen anode in the respective embodiments or comparative examples, except that the anode catalyst material is replaced with the cathode catalyst material.

[0046] Example 1

[0047] The method for preparing a high-performance AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis in Example 1 includes the following steps:

[0048] (1) Preparation of AEM anode for hydrogen production via water electrolysis:

[0049] 1) Deionized water and ethanol were ultrasonically mixed at a volume ratio of 1:1 to obtain a solvent; the anode NiCoFe-LDH catalyst powder and the solvent were mixed at a mass ratio of 1:3 and ball-milled at 600 rpm for 60 min to obtain the anode NiCoFe-LDH catalyst pre-slurry.

[0050] 2) Add 1 / 4 of I-250 to the anode NiCoFe-LDH catalyst pre-slurry every 10 min. The weight of I-250 is 5% of the weight of NiCoFe-LDH catalyst powder. After ultrasonic mixing for 30 min, add polytetrafluoroethylene (PTFE). The weight of PTFE is 0.5% of the total solid matter in the slurry. Shear and mix for 40 min to obtain the anode NiCoFe-LDH catalyst slurry.

[0051] 3) In an area of ​​5 cm 2 Anode NiCoFe-LDH catalyst slurry was coated on the surface of the modified nickel felt substrate diffusion layer and dried to obtain the anode nickel felt substrate diffusion layer NiCoFe-LDH-NFF (A).

[0052] 4) A 10 μm thick layer of I-250 was coated on the surface of NiCoFe-LDH-NFF (A) to obtain a diffusion layer (B) coated with I-250 resin; the diffusion layer (B) coated with I-250 resin was immersed in ethanol for 30 s, and the surface was rinsed with deionized water several times to obtain the AEM water electrolysis hydrogen production anode NiCoFe-LDH-NFF;

[0053] (2) Preparation of AEM water electrolysis hydrogen production membrane electrode:

[0054] The NiCoFe-LDH-NFF and AEM electrolysis hydrogen production cathodes were placed on both sides of the anion exchange membrane and sealed to obtain the AEM electrolysis hydrogen production membrane electrode.

[0055] Comparative Example 1

[0056] Comparative Example 1 is basically the same as Example 1, except that the preparation process of the anode NiCoFe-LDH catalyst slurry is different. The specific steps are as follows:

[0057] (1) Preparation of AEM anode for hydrogen production via water electrolysis:

[0058] 1) Deionized water and ethanol were ultrasonically mixed at a volume ratio of 1:1 to obtain a solvent; the anode NiCoFe-LDH catalyst powder and the solvent were mixed at a mass ratio of 1:3, and I-250 and polytetrafluoroethylene were added. The weight of I-250 was 5% of the weight of the NiCoFe-LDH catalyst powder, and the weight of polytetrafluoroethylene was 0.5% of the total solid matter in the slurry. After ultrasonic mixing for 30 min, the anode NiCoFe-LDH catalyst slurry was obtained.

[0059] 2) In an area of ​​5cm 2 Anode NiCoFe-LDH catalyst slurry was coated onto the surface of the modified nickel felt substrate diffusion layer and dried to obtain the anode nickel felt substrate diffusion layer NiCoFe-LDH-NFF.

[0060] 3) Coat the surface of NiCoFe-LDH-NFF with I-250 with a thickness of 10 μm to obtain a diffusion layer coated with I-250 resin; immerse the diffusion layer coated with I-250 resin in ethanol for 30s, and rinse the surface with deionized water several times to obtain the AEM water electrolysis hydrogen production anode NiCoFe-LDH-NFF.

[0061] (2) Preparation of AEM water electrolysis hydrogen production membrane electrode:

[0062] The NiCoFe-LDH-NFF and AEM water electrolysis hydrogen production membrane cathodes were placed on both sides of the anion exchange membrane and sealed to obtain the AEM water electrolysis hydrogen production membrane electrode.

[0063] Comparative Example 2

[0064] Comparative Example 2 is basically the same as Example 1, except that the nickel felt substrate diffusion layer is not pre-modified for hydrophobicity.

[0065] Comparative Example 3

[0066] The process is essentially the same as in Example 1, except that an additional layer of anion exchange resin coating is not applied. Specifically, the steps include the following:

[0067] (1) Preparation of AEM anode for hydrogen production via water electrolysis:

[0068] 1) Deionized water and ethanol were ultrasonically mixed at a volume ratio of 1:1 to obtain a solvent; the anode NiCoFe-LDH catalyst powder and the solvent were mixed at a mass ratio of 1:3 and ball-milled at 600 rpm for 60 min to obtain the anode NiCoFe-LDH catalyst pre-slurry.

[0069] 2) Add 1 / 4 of I-250 to the anode NiCoFe-LDH catalyst pre-slurry every 10 min. The weight of I-250 is 5% of the weight of NiCoFe-LDH catalyst powder. After ultrasonic mixing for 30 min, add polytetrafluoroethylene (PTFE). The weight of PTFE is 0.5% of the total solid matter in the slurry. Shear and mix for 40 min to obtain the anode NiCoFe-LDH catalyst slurry.

[0070] 3) In an area of ​​5cm 2 Anode NiCoFe-LDH catalyst slurry was coated onto the surface of the modified nickel felt substrate diffusion layer and dried to obtain the anode nickel felt substrate diffusion layer NiCoFe-LDH-NFF.

[0071] (2) Preparation of AEM water electrolysis hydrogen production membrane electrode:

[0072] The NiCoFe-LDH-NFF and AEM water electrolysis hydrogen production membrane cathodes were placed on both sides of the anion exchange membrane and sealed to obtain the AEM water electrolysis hydrogen production membrane electrode.

[0073] Comparative Example 4

[0074] The basic steps are the same as in Example 1, except that epoxy resin is used as the adhesive.

[0075] Performance testing

[0076] The performance of the AEM water electrolysis membrane electrodes used in Example 1, Comparative Examples 1 to 4 was tested, and the results are as follows: Figure 1 As shown. Figure 1 As can be seen from Example 1 and Comparative Example 1, the current density in Example 1 reaches 29000 A / m. 2@2V, while the current density of Comparative Example 1 is 26000A / m. 2 @2V, therefore, adding each component of the catalyst slurry in batches can solve problems such as agglomeration and phase separation caused by polarity differences, as well as performance loss caused by competitive adsorption of functional components, thereby achieving uniform slurry dispersion and improving electrode performance.

[0077] Combining Example 1 with Comparative Examples 2 and 3, it can be seen that the current density of Comparative Examples 2 and 3 is only 24000 A / m. 2 @2V. Further analysis reveals that by hydrophobically modifying the nickel felt substrate and simultaneously coating the catalyst layer surface with an anion exchange membrane solution to prevent excessive hydrophobicity, OH⁻ migrates in the AEM network as hydrated ions. Therefore, the synergistic effect between the nickel felt modification and the additional anion exchange membrane solution coating essentially allows the substrate to shift from passively adapting to the gas-liquid environment to actively optimizing the three-phase interface through surface characteristic control. This solves problems such as water flooding, corrosion, and poor adhesion caused by hydrophilicity, while retaining the core advantages of high conductivity and porosity of the nickel felt. Furthermore, to avoid further hydrophobicity, the ultimate goal of achieving "highly efficient mass transfer, structurally stable, and long-lasting" AEM electrodes is achieved.

[0078] Furthermore, the addition of a hydrophobic binder can reduce the interfacial tension between the slurry and the hydrophobically modified diffusion layer substrate, preventing the slurry from shrinking and agglomerating on the hydrophobic substrate due to excessive hydrophilicity during coating. This further adjusts the uniformity of the catalyst layer on the electrode surface, thereby improving activity. Combining Example 1 and Comparative Example 4, it can be seen that Comparative Example 4, despite the addition of hydrophilic epoxy resin, only achieved a current density of 22000 A / m. 2 @2V.

[0079] Based on the above Comparative Examples 2, 3 and 4, it can be seen that by using a hydrophobic modified diffusion layer substrate, and by combining the addition of a hydrophobic binder and the coating of anion exchange membrane solution, the electrode performance can be effectively improved.

[0080] Example 2

[0081] The method for preparing a high-performance AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis in Example 2 includes the following steps:

[0082] (1) Preparation of AEM anode for hydrogen production via water electrolysis:

[0083] 1) Deionized water and isopropanol were ultrasonically mixed at a volume ratio of 1:1 to obtain a solvent; the anode NiCoFe-LDH catalyst powder and the solvent were mixed at a mass ratio of 1:3 and ball-milled at 600 rpm for 60 min to obtain the anode NiCoFe-LDH catalyst pre-slurry.

[0084] 2) Add 1 / 2 of I-250 to the anode NiCoFe-LDH catalyst pre-slurry every 20 min. The weight of I-250 is 15% of the weight of NiCoFe-LDH catalyst powder. After ultrasonic mixing for 30 min, add polytetrafluoroethylene (PTFE). The weight of PTFE is 1% of the total solid matter weight in the slurry. Shear and mix for 40 min to obtain the anode NiCoFe-LDH catalyst slurry.

[0085] 3) In an area of ​​5cm 2 Anode NiCoFe-LDH catalyst slurry was coated on the surface of the modified nickel felt substrate diffusion layer and dried to obtain the anode nickel felt substrate diffusion layer NiCoFe-LDH-NFF (A).

[0086] 4) A 5 μm thick layer of I-250 was coated on the surface (A) of NiCoFe-LDH-NFF to obtain a diffusion layer (B) coated with I-250 resin.

[0087] 5) Immerse the diffusion layer (B) coated with I-250 resin in isopropanol for 60s, and rinse the surface with deionized water several times to remove excess isopropanol, thus obtaining the AEM water electrolysis hydrogen production anode NiCoFe-LDH-NFF.

[0088] (2) Preparation of AEM water electrolysis hydrogen production membrane electrode:

[0089] The NiCoFe-LDH-NFF and AEM water electrolysis hydrogen production membrane cathodes were placed on both sides of the anion exchange membrane and sealed to obtain the AEM water electrolysis hydrogen production membrane electrode.

[0090] Comparative Example 5

[0091] The basic steps are the same as in Example 2, except that polyacrylonitrile is used as the binder.

[0092] Performance testing

[0093] The performance of the AEM water electrolysis hydrogen production membrane electrodes prepared in Example 2 and Comparative Example 5 was tested, and the results are as follows: Figure 2 As shown. Figure 2 In Example 2, the current density reached 27000 A / m. 2 @2V. In Comparative Example 5, after changing to a more hydrophilic polyacrylonitrile, the current density decreased to 19000 A / m. 2 @2V further verified the synergistic relationship between the hydrophobic binder, the hydrophilic slurry, and the hydrophobic modified diffusion layer matrix.

[0094] In addition to the above embodiments, the process conditions and parameters defined by the preparation method of the present invention can achieve both reduced oxygen bubble retention and improved stability, while further enhancing the activity of the membrane electrode. Therefore, further experimental verification is not required for each instance.

Claims

1. A method for preparing a high-performance AEM (Alternating Electrode Electrolysis) membrane electrode for hydrogen production via water electrolysis, characterized in that, Includes the following steps: (1) Preparation of AEM anode for hydrogen production via water electrolysis: 1) The anode catalyst powder is mixed with a solvent and ball-milled to form an anode catalyst pre-slurry; 2) Anion exchange resin solution is added to the anode catalyst pre-slurry in portions, and the mixture is ultrasonically mixed into a slurry. Then, a hydrophobic binder is added, and the mixture is sheared and mixed to obtain the anode catalyst slurry. 3) The anode catalyst slurry obtained in step 2) is coated onto the surface of the hydrophobically modified diffusion layer and dried to obtain diffusion layer A coated with anode catalyst; 4) Coat the surface of the diffusion layer A obtained in step 3) with anion exchange resin solution to obtain diffusion layer B with anion exchange membrane resin coating, and immerse it in an organic solvent to obtain AEM water electrolysis hydrogen production anode. (2) Preparation of AEM water electrolysis hydrogen production membrane electrode: The AEM electrolysis water-to-hydrogen anode and the AEM electrolysis water-to-hydrogen cathode prepared in step 4) are placed on both sides of the anion exchange membrane and sealed to obtain the AEM electrolysis water-to-hydrogen membrane electrode.

2. The method for preparing an AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis according to claim 1, characterized in that, The AEM electrolysis water production hydrogen cathode is prepared by the following steps: 1) The cathode catalyst powder is mixed with a solvent and ball-milled to form a cathode catalyst pre-slurry; 2) Add anion exchange resin solution to the cathode catalyst pre-slurry in portions, mix ultrasonically to form a slurry, add a hydrophobic binder, and shear mix to obtain the cathode catalyst slurry. 3) The cathode catalyst slurry obtained in step 2) is coated onto the surface of the hydrophobic modified diffusion layer and dried to obtain the diffusion layer C coated with the cathode catalyst. 4) Coat the surface of the diffusion layer C obtained in step 3) with anion exchange resin solution to obtain a diffusion layer D with anion exchange membrane resin coating, and immerse it in an organic solvent to obtain an AEM water electrolysis hydrogen production cathode.

3. The method for preparing an AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis according to claim 1 or 2, characterized in that, In step 1), the solvent is deionized water and an organic solvent in a volume ratio of 1:(1-10), wherein the organic solvent is selected from ethanol, isopropanol, propylene glycol or acetone; the amount of solvent added is 1-5 times the mass of the catalyst powder.

4. The method for preparing an AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis according to claim 3, characterized in that, In step 4), the organic solvent is selected from ethanol, isopropanol, propylene glycol or acetone, and is consistent with the organic solvent used in step 1).

5. The method for preparing an AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis according to claim 1 or 2, characterized in that, In step 2), the amount of anion exchange resin solution added is 5-20% of the weight of the catalyst powder, the time interval between additions is 5-20 min, and the amount added each time is 1 / 8-1 / 2 of the total amount of anion exchange resin solution.

6. The method for preparing an AEM (Alternating Electrode Electrolyte) membrane electrode for hydrogen production via water electrolysis according to claim 1 or 2, characterized in that, In step 2), the hydrophobic binder is selected from polytetrafluoroethylene, perfluoroethylene propylene, or polyvinylidene fluoride, and its addition amount accounts for 0.1-2.5% of the total solid matter weight in the catalyst slurry.

7. The method for preparing an AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis according to claim 1 or 2, characterized in that, In step 4), the coating thickness of the anion exchange resin solution on the surface of diffusion layer A or diffusion layer C is 5-20 μm.

8. The method for preparing an AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis according to claim 1 or 2, characterized in that, In step 4), the soaking time in the organic solvent is 20-90 s.

9. The method for preparing an AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production via water electrolysis according to claim 1 or 2, characterized in that, In step 3), the hydrophobically modified diffusion layer is prepared by the following steps: a. Pre-treat the diffusion layer with a porosity of 50-80%, then immerse it in the modifying agent and react at 55-65 ℃ for 8-12 min. Add sodium dodecyl sulfate, continue immersion at 35-45 ℃ for 15-25 min, and then air dry to obtain the gas diffusion layer after preliminary modification. b. The preliminarily modified gas diffusion layer is reacted in an inert atmosphere at 600-800 ℃ for 1.5-2 h to obtain a hydrophobically modified diffusion layer.

10. The method for preparing an AEM (Aqueous Electrolytic Metallization) membrane electrode for hydrogen production by water electrolysis according to claim 9, characterized in that, In step a, the modifying reagent includes an HCl solution, an HNO3 solution, and a FeCl3 solution in a volume ratio of (40-55):(20-35):(10-25); the amount of sodium dodecyl sulfate added is such that its mass concentration in the modifying reagent reaches 0.4-0.6 wt%.

Citation Information

Patent Citations

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