A preparation method for the anode oxygen plate of PEM water electrolysis

Abstract

The present invention provides a method for preparing a PEM water electrolysis anode oxygen plate, which relates to the field of proton exchange membrane water electrolysis. First, the cleaned nickel foam is immersed in a noble metal solution, taken out and calcined after the immersion ends. Then, the treated nickel foam is immersed in a hydrochloric acid solution, washed and dried for standby. Next, the nickel foam is placed on a heating platform, and the noble metal solution is sprayed. A mixed slurry prepared by mixing the titanium powder after heating and pickling with a solvent and a binder is applied to the nickel foam in multiple times and fixed into shape. Finally, it is hot-pressed and calcined with a mold to obtain a PEM water electrolysis anode oxygen plate with low cost, high mechanical strength, oxidation resistance, corrosion resistance and excellent electrical conductivity, which is suitable for a strongly oxidizing environment.

Description

Technical Field

[0001] The present invention belongs to the field of proton exchange membrane water electrolysis, and particularly relates to a method for preparing a PEM water electrolysis anode oxygen plate. Background Art

[0002] Hydrogen has a wide range of sources, high calorific value, is clean and carbon-free, can be used for energy storage, power generation, and heating, is flexible and efficient, and has rich application scenarios. Hydrogen production by water electrolysis is considered the future development direction of hydrogen production, especially the use of renewable energy for water electrolysis to produce hydrogen. PEM water electrolysis for hydrogen production selects a perfluorosulfonic acid proton exchange membrane with good chemical stability, proton conductivity, and gas separation as a solid electrolyte to replace the asbestos membrane, which can effectively prevent electron transfer and improve the safety of the electrolytic cell. The main components of PEM water electrolysis for hydrogen production include a membrane electrode and a bipolar plate. The membrane electrode generally uses a PE membrane or an ion exchange membrane material as the separator material, and a conductive and corrosion-resistant material is used for the bipolar plate.

[0003] The bipolar plate is one of the key technologies in PEM water electrolysis technology. It plays roles such as support, gas separation, conduction, and heat dissipation in the water electrolysis cell. Therefore, the bipolar plate becomes the most important part among the components of the PEM stack. The research on bipolar plates with low cost, high chemical stability, and high electrical and thermal conductivity is crucial. Currently, the commonly used bipolar plate materials are divided into three categories: graphite materials, composite materials, and metal materials. Graphite materials are inexpensive and have a simple processing technology, but the mechanical properties of graphite are poor, and it is prone to phenomena such as fracture and breakage under high pressure. Composite materials have excellent chemical stability, but their electrical and thermal conductivity and mechanical properties are poor. Metal materials have excellent properties in terms of electrical conductivity, thermal conductivity, and mechanical properties. Due to the requirement for stability, the price of metal materials becomes the main limiting condition. In addition, the working environment of the anode of the PEM water electrolysis cell is harsh, and metals are easily corroded, resulting in the leaching of metal ions, which in turn pollutes the PEM water electrolysis cell. The current solution is to use high-purity materials as the bipolar plate matrix structure and perform an anti-corrosion coating treatment on the surface of the bipolar plate to reduce the anode oxidation problem. However, generally, the better the conductivity of the coating, the worse the corrosion resistance. This is the biggest bottleneck restricting the development of the surface coating of metal bipolar plates.

[0004] Currently, the bipolar plates of PEM water electrolysis cells are mainly integral metal plates, which have a large amount of metal used, complex processing, large weight, and high cost. The most basic materials are austenitic stainless steel and titanium. Coating treatments are carried out on the metal bipolar plates, and the commonly used coatings include Ti-Ag films, (Ti, Zr)N, ruthenium oxide, platinum, and gold, etc. However, the corrosion resistance and durability of the coatings still need to be further improved. In addition, the bipolar plates of the existing water electrolysis cell technology are severely corroded under the conditions of the acidity of the PEM water electrolysis stack and the applied voltage, which severely limits the use of metal bipolar plates and results in the high cost of current PEM water electrolysis for hydrogen production. Summary of the Invention

[0005] Aiming at the deficiencies existing in the prior art, the technical problem to be solved by the present invention is how to prepare an anode oxygen plate with low cost, high mechanical strength, oxidation resistance, corrosion resistance and excellent electrical conductivity, which is suitable for a strong oxidizing environment.

[0006] To solve the above technical problem, the present invention provides a method for preparing a PEM water electrolysis anode oxygen plate, comprising the following steps:

[0007] Step 1: Clean the nickel foam and set it aside;

[0008] Step 2: Immerse the nickel foam cleaned in Step 1 in a noble metal solution, take it out after the immersion ends and conduct calcination, and set it aside;

[0009] Step 3: Immerse the nickel foam treated in Step 2 in a hydrochloric acid solution, then clean it with deionized water and dry it;

[0010] Step 4: Select spherical dehydrogenated titanium powder for heating and pickling, then conduct cleaning and vacuum drying, and set it aside;

[0011] Step 5: Mix the spherical dehydrogenated titanium powder treated in Step 4, a binder and an alcohol solvent, and disperse to obtain a mixed slurry;

[0012] Step 6: Place the nickel foam treated in Step 3 on a heating platform, and simultaneously spray a noble metal solution to make the nickel foam in an atomized noble metal solution atmosphere. At the same time, brush the mixed slurry prepared in Step 5 multiple times and heat it to be fixed into a flat plate;

[0013] Step 7: Take out the flat plate fixed and formed in Step 6, lay the fixed and formed flat plate on a mold with a parallel flow field, and then put the whole into a hot press for hot pressing;

[0014] Step 8: Place the plate with a parallel flow field hot-pressed in Step 7 in a nitrogen-filling furnace for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0015] Further, in Step 1, the pore diameter of the nickel foam is 200 - 400 nm; the solution for cleaning the nickel foam is an acetone solution, the cleaning method is ultrasonic cleaning, the number of cleaning times is 3 - 5 times, and the ultrasonic cleaning time for each time is 3 - 5 min.

[0016] Further, in Step 2, the noble metal solution is any one of iridium chloride hexahydrate solution, ruthenium chloride trihydrate, and palladium chloride solution. The content of noble metal ions in the noble metal solution is 20 - 50 mmol / L, the soaking time is 4 - 8 h, the calcination time is 20 - 40 min, and the calcination temperature is 495 - 580 °C. If the soaking time is too short, too little noble metal adheres to the nickel foam, reducing the anti-corrosion effect. If the soaking time is too long, the noble metal layer thickens, increasing the cost.

[0017] Further, in Step 3, the concentration of the hydrochloric acid solution is 1 - 3 mol / L, the soaking time is 5 - 10 min, the number of times of washing with deionized water is 6 - 9 times, and the drying temperature is 60 - 80 °C.

[0018] Further, in Step 4, the particle size of the spherical dehydrogenated titanium powder is 10 - 30 nm;

[0019] The method of heating and pickling the spherical dehydrogenated titanium powder is as follows: Place the spherical dehydrogenated titanium powder in an acid solution and use a stirrer with a heating function to heat and stir the spherical dehydrogenated titanium powder. The pickling time of the spherical dehydrogenated titanium powder is 20 - 40 min, the heating temperature is 40 - 60 °C, the acid solution is any one of hydrochloric acid solution, oxalic acid solution, and formic acid solution, and the concentration of the acid solution is 0.1 - 0.5 mol / L;

[0020] Cleaning is carried out using an alcohol solvent, and the alcohol solvent is any one of methanol, ethanol, and n-propanol. The number of times of cleaning with the alcohol solvent is 4 - 7 times; the drying temperature is 60 - 80 °C.

[0021] Further, in Step 5, the binder is a PTFE emulsion with a concentration of 25 wt%; the alcohol solvents are any one of methanol, ethanol, and n-propanol; the mass ratio of the spherical dehydrogenated titanium powder, the binder, and the alcohol solvent is 1∶0.5 - 0.8∶20 - 35; the dispersion method is any one of ultrasonic dispersion and high-speed stirring dispersion; the viscosity of the mixed slurry is 50 - 120 cp.

[0022] Further, in Step 6, the temperature of the heating platform is 120 - 150 °C; the noble metal solution sprayed is the same as the noble metal solution used in Step 2; the atomized noble metal solution is achieved by spraying with an atomizing nozzle, the spraying flow rate of the noble metal solution is 3 - 5 L / min, and the noble metal suspension concentration in the atomized noble metal solution atmosphere is 10000 - 25000 μg / m 3 ; the number of brushing times is 5 - 8 times; the heating and fixing forming time is 4 - 8 min.

[0023] Further, in Step 7, the temperature for hot pressing is 80 - 110 °C; the pressure is 0.6 - 0.9 MPa; the hot pressing time is 1.5 - 3 min.

[0024] Further, in step seven, the mold with a parallel flow field is made of stainless steel material. The mold includes a base plate, and two or more raised structures are installed on the base plate at intervals and placed in parallel.

[0025] After the mold is pressed on the nickel foam, the concave flow channel pattern formed by the raised structure on the surface of the nickel foam is a parallel flow field structure.

[0026] Further, in step eight, the calcination temperature in the nitrogen charging furnace is 350 - 450 °C.

[0027] Beneficial effects:

[0028] 1. The present invention uses nickel foam as the matrix material. Since nickel foam has a very rich pore structure, it can fully fill the functional material, realizing the effective combination of the pore structure and the functional material. Therefore, it has a uniform and high mass transfer capacity. Secondly, the present invention uses spherical dehydrogenated titanium powder with ultra-fine particle size as the brush coating material, further ensuring that the spherical dehydrogenated titanium powder is fully filled in the pore structure of the nickel foam to form a conductive path. On the other hand, due to the ultra-high conductivity of the spherical dehydrogenated titanium powder, it promotes the electron conduction of the anode oxygen plate, reduces the ohmic resistance, and improves the electrolysis efficiency. Nickel foam has excellent electron conduction ability, and is corrosion-resistant and oxidation-resistant. Filling titanium powder with high stability inside the nickel foam wrapped with precious metal further improves the conductivity of the overall oxygen plate.

[0029] 2. The present invention uses nickel foam as the matrix material. Since nickel foam is soft and malleable, it can be directly hot-pressed into shape to form a flow field structure in one step. Due to the special functionality of the oxygen plate (such as high conductivity, anti-oxidation function, etc.), in the conventional preparation methods, steps such as coating precious metal on the oxygen plate, forming the oxygen plate, compounding the flow field structure, and anti-oxidation treatment are included, with complex processes and high costs. However, the present invention reasonably utilizes the material characteristics of cheap nickel foam to integrally prepare the oxygen plate and the flow field structure on the surface of the oxygen plate, greatly reducing the preparation process of the oxygen plate and saving costs on the premise of ensuring the performance of the oxygen plate.

[0030] 3. In the preparation method of the present invention, first, nickel foam is immersed in a noble metal solution so that noble metal ions adhere to the inner wall and surface of the pores of the nickel foam. The metal ions and the nickel foam undergo a chemical reaction at high temperature. On the one hand, the stability and corrosion resistance are improved. On the other hand, a high-speed conductive grid channel can be formed inside the entire anode oxygen plate, improving the ultra-high conductivity of the oxygen plate. Since the pickling process will cause certain corrosion to the nickel foam, in order to minimize the damage to the structural strength of the nickel foam as much as possible, the present invention is designed to perform pickling after soaking in the noble metal solution. On the one hand, it is to remove the residues on the surface after the front-end process treatment. On the other hand, it etches the parts that did not adhere to the noble metal ions in the front-end process, preparing for the subsequent spraying and adhesion of noble metal ions, so that the noble metal ions adhere to the inner wall and surface of the pores of the nickel foam, effectively improving the overall structural strength. The pickling carried out after the nickel foam is calcined after being immersed in the noble metal solution, combined with the control of pickling concentration, time, temperature, etc., has a mild etching degree, thus greatly reducing the corrosiveness and not affecting the overall structural strength.

[0031] 4. When the present invention applies spherical dehydrogenated titanium powder to the surface of nickel foam, it adopts the method of multiple brush coatings to allow the spherical dehydrogenated titanium powder to fully fill the pores of the nickel foam. Moreover, when the present invention applies the titanium slurry multiple times, it is carried out in a noble metal atmosphere. Multiple brush coatings enable the noble metal to have sufficient contact with the applied spherical dehydrogenated titanium powder, and the noble metal can adhere to the surface of the spherical dehydrogenated titanium powder, achieving the effect of noble metal coverage and filling the interior of the prepared oxygen plate, improving the overall conductivity while preventing the spherical dehydrogenated titanium powder from being oxidized at high potentials. In addition, the brush coating of the titanium slurry and the noble metal atmosphere are both carried out simultaneously under a heating state. The high-temperature volatilization of the solvent under the heating state generates stress concentration, enabling the noble metal and the slurry to enter the pores of the nickel foam together. During the forming process of the nickel foam, the noble metal and the titanium powder quickly combine and solidify with the nickel foam and are "locked" inside it, promoting and accelerating the combination process and facilitating the formation of a strongly solidified structure with stable structure.

[0032] 5. After the present invention is formed, it is placed on a mold with a flow field. Since the nickel foam and the solidified slurry are relatively soft, and because the nickel foam has a certain supporting property, using a parallel flow field mold, an oxygen plate flow field can be directly formed on the flat surface under a certain pressure, and at the same time, the anode oxygen plate is compacted to improve the firmness.

[0033] 6. Through high-temperature calcination, the binder in the brush-coated spherical dehydrogenated titanium powder slurry is sintered and vaporized to form an ultra-fine pore structure, which can better promote the discharge of gas adhering to the surface of the bipolar plate during the electrolysis of water, reduce the surface impedance, and improve the electrolysis efficiency. In addition, high-temperature calcination further enables the noble metal on the surface of the nickel foam to undergo metal interdiffusion with nickel to form a metal intermetallic compound. On the one hand, the metal intermetallic compound has an ordered structure, high strength, and strong oxidation resistance, protecting the anode oxygen plate from oxidation and increasing the service life. On the other hand, the ordered structure further makes the conductive channels grid-like, improving the conductivity.

[0034] The concept, specific structure, and technical effects of the present invention will be further described below in conjunction with the accompanying drawings to fully understand the purpose, features, and effects of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 is a cross-sectional view of a mold with a parallel flow field;

[0036] Figure 2 is a top view of a mold with a parallel flow field;

[0037] In the figure:

[0038] 1. Base plate; 2. Protruding structure. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0039] The present invention will be further elaborated below in conjunction with the specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and not to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of this application.

[0040] In the accompanying drawings, components with the same structure are denoted by the same numeral labels, and components with similar structures or functions are denoted by similar numeral labels. The size and thickness of each component shown in the drawings are arbitrarily shown, and the present invention does not limit the size and thickness of each component. In order to make the illustration clearer, the thickness of some components in the drawings is appropriately exaggerated.

[0041] As Figures 1-2 shown, a mold with a parallel flow field applicable to the following examples and comparative examples is made of stainless steel. The mold includes a base plate 1, and two or more spaced and parallelly placed protruding structures 2 are installed on the base plate 1;

[0042] After the mold is pressed on the nickel foam, the concave flow channel pattern formed by the protruding structure 2 on the surface of the nickel foam is a parallel flow field structure.

[0043] Example 1:

[0044] 1. Select nickel foam with a pore size of 200 nm and place it in acetone. Ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for later use.

[0045] 2. Measure 50 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 1 mol / L dilute hydrochloric acid solution. Set it aside for later use.

[0046] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L. Set it aside for later use.

[0047] 4. Immerse the nickel foam cleaned with acetone in step 1 in the precious metal solution prepared in step 3 for 8 h, then take it out and calcine it at a high temperature of 495 °C for 40 min. Set it aside for later use.

[0048] 5. Immerse the nickel foam treated in step 4 in the dilute hydrochloric acid solution prepared in step 2 for 10 min, then take it out and wash it 9 times with deionized water, and dry it at 80 °C. Set it aside for later use.

[0049] 6. Measure 10 mL of 36.5 wt.% hydrochloric acid and add it to 1190 mL of deionized water to prepare a dilute hydrochloric acid solution with a concentration of 0.1 mol / L. Weigh spherical dehydrogenated titanium powder with a particle size of 10 nm and add it to the dilute hydrochloric acid solution. Heat it to 60 °C and stir for 40 min, then take it out, wash it 4 times with ethanol, and dry it at 60 °C. Set it aside for later use.

[0050] 7. Weigh 100 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder treated in step 6, and 1750 g of ethanol, and mix and disperse them to form a mixed slurry with a viscosity of 50 cp. Set it aside for later use.

[0051] 8. Place the nickel foam treated in step 5 on a heating platform at a temperature of 150 °C, and place the precious metal ion solution prepared in step 3 in a spraying device. Open the spraying device and set the spraying flow rate to 3 L / min, so that the nickel foam is in an atmosphere with a precious metal ion content of 10000 μg / m 3 . Then brush the mixed slurry prepared in step 7 on the surface of the nickel foam in 8 times, and keep heating for 8 min to make it take shape into a flat plate.

[0052] 9. Take out the flat plate fixed and formed in step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press. Hot press it at 110 °C and 0.6 MPa for 1.5 min; then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filling furnace at 350 °C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0053] Example 2:

[0054] 1. Select nickel foam with a pore size of 400 nm and place it in acetone. Ultrasonically clean it 5 times, with each ultrasonic cleaning time being 3 min. After cleaning, set it aside for later use.

[0055] 2. Measure 150 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 450 mL of deionized water to prepare a 3 mol / L dilute hydrochloric acid solution. Set it aside for later use.

[0056] 3. Weigh 11.27 g of ruthenium chloride trihydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 50 mmol / L. Set it aside for later use.

[0057] 4. Immerse the nickel foam cleaned with acetone in step 1 in the precious metal solution prepared in step 3 for 4 h, then take it out and calcine it at 580 °C for 20 min. Set it aside for later use.

[0058] 5. Immerse the nickel foam treated in step 4 in the dilute hydrochloric acid solution prepared in step 2 for 5 min, then take it out and wash it 6 times with deionized water, and dry it at 60 °C. Set it aside for later use.

[0059] 6. Measure 45 g of oxalic acid and add it to 1000 mL of deionized water to prepare a 0.5 mol / L dilute oxalic acid solution; weigh spherical dehydrogenated titanium powder with a particle size of 30 nm and add it to the dilute oxalic acid solution. Heat it to 40 °C and stir for 20 min, then take it out and wash it 7 times with methanol, and dry it at 80 °C. Set it aside for later use.

[0060] 7. Weigh 128 g of 25 wt.% PTFE, 40 g of the spherical dehydrogenated titanium powder treated in step 6, and 800 g of methanol, and mix and disperse them to form a mixed slurry with a viscosity of 120 cp. Set it aside for later use.

[0061] 8. Place the nickel foam treated in step 5 on a heating platform at a temperature of 120 °C, and load the precious metal ion solution prepared in step 3 into a spraying device. Open the spraying device and set the spraying flow rate to 5 L / min so that the nickel foam is in an atmosphere with a precious metal ion content of 25000 μg / m3. Then brush the mixed slurry prepared in step 7 on the surface of the nickel foam in 5 times, and keep heating for 4 min to make it take shape into a flat plate.

[0062] 9. Take out the flat plate fixed and formed in step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press, and hot press at 80 °C and 0.9 MPa for 3 min; then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filling furnace at 450 °C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0063] Example 3:

[0064] 1. Select nickel foam with a pore size of 300 nm, place it in acetone, and ultrasonically clean it 4 times, with each ultrasonic cleaning time being 4 min. After cleaning, set it aside for use.

[0065] 2. Measure 100 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 2 mol / L dilute hydrochloric acid solution, and set it aside for use.

[0066] 3. Weigh 8.5 g of palladium chloride and dissolve it in 1370 mL of deionized water to prepare a precious metal solution with a concentration of 35 mmol / L, and set it aside for use.

[0067] 4. Immerse the nickel foam cleaned with acetone in step 1 in the precious metal solution prepared in step 3 for 6 h, then take it out and calcine it at 550 °C for 30 min, and set it aside for use.

[0068] 5. Immerse the nickel foam treated in step 4 in the dilute hydrochloric acid solution prepared in step 2 for 7 min, then take it out and wash it 8 times with deionized water, and dry it at 70 °C, and set it aside for use.

[0069] 6. Weigh 20 g of 50 wt.% formic acid and add it to 705 mL of deionized water to prepare a dilute formic acid solution with a concentration of 0.3 mol / L; weigh spherical dehydrogenated titanium powder with a particle size of 20 nm and add it to the dilute formic acid solution, heat it to 50 °C, stir for 30 min, then take it out, wash it 5 times with n-propanol, and dry it at 70 °C, and set it aside for use.

[0070] 7. Weigh 140 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder treated in step 6, and 1500 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 90 cp, and set it aside for use.

[0071] 8. Place the nickel foam treated in step 5 on a heating platform at a temperature of 130 °C, and put the precious metal ion solution prepared in step 3 in a spraying device. Open the spraying device, set the spraying flow rate to 4 L / min, so that the nickel foam is in an atmosphere with a precious metal ion content of 18000 μg / m3, and then brush the mixed slurry prepared in step 7 on the surface of the nickel foam 6 times, and keep heating for 6 min to make it take shape to form a flat plate.

[0072] 9. Take out the flat plate fixed and formed in step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press, and hot press it at 100 °C and 0.7 MPa for 2.5 min; then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filling furnace at 400 °C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0073] Comparative Example 1: (There is no noble metal ion atmosphere during the slurry coating)

[0074] 1. Select nickel foam with a pore size of 200 nm, place it in acetone, and ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for later use.

[0075] 2. Measure 50 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 1 mol / L dilute hydrochloric acid solution, and set it aside for later use.

[0076] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L, and set it aside for later use.

[0077] 4. Immerse the nickel foam cleaned with acetone in step 1 in the precious metal solution prepared in step 3 for 8 h, then take it out and calcine it at a high temperature of 495 °C for 40 min, and set it aside for later use.

[0078] 5. Immerse the nickel foam treated in step 4 in the dilute hydrochloric acid solution prepared in step 2 for 10 min, then take it out, wash it 9 times with deionized water, and dry it at 80 °C, and set it aside for later use.

[0079] 6. Measure 10 mL of 36.5 wt.% hydrochloric acid (12 mol / L) and add it to 1190 mL of deionized water to prepare a dilute hydrochloric acid solution with a concentration of 0.1 mol / L; weigh spherical dehydrogenated titanium powder with a particle size of 10 nm and add it to the dilute hydrochloric acid solution, heat it to 60 °C, stir for 40 min, then take it out, wash it 4 times with ethanol, and dry it at 60 °C, and set it aside for later use.

[0080] 7. Weigh 100 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder treated in step 6, and 1750 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 50 cp, and set it aside for later use.

[0081] 8. Place the nickel foam treated in step 5 on a heating platform at a temperature of 150 °C, then brush the mixed slurry prepared in step 7 on the surface of the nickel foam in 8 times, and keep heating for 8 min to make it take shape to form a flat plate.

[0082] 9. Take out the flat plate fixed and formed in step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press. Hot press it at 110°C and 0.6 MPa for 1.5 min. Then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filling furnace at 350°C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0083] Comparative Example 2: (The nickel foam is not treated with acid)

[0084] 1. Select nickel foam with a pore size of 200 nm and place it in acetone. Ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for use.

[0085] 2. Dry the nickel foam cleaned with acetone in step 1 at 80°C for later use.

[0086] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L for later use.

[0087] 4. Immerse the dried nickel foam in step 2 in the precious metal solution prepared in step 3 for 8 h, then take it out and calcine it at a high temperature of 495°C for 40 min for later use.

[0088] 5. Measure 10 mL of 36.5 wt.% hydrochloric acid and add it to 1190 mL of deionized water to prepare a dilute hydrochloric acid solution with a concentration of 0.1 mol / L. Weigh spherical dehydrogenated titanium powder with a particle size of 10 nm and add it to the dilute hydrochloric acid solution. Heat it to 60°C, stir for 40 min, then take it out, wash it 4 times with ethanol, and dry it at 60°C for later use.

[0089] 6. Weigh 100 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder treated in step 6, and 1750 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 50 cp for later use.

[0090] 7. Place the nickel foam treated in step 4 on a heating platform at a temperature of 150°C, and load the precious metal ion solution prepared in step 3 into a spraying device. Open the spraying device and set the spraying flow rate to 3 L / min so that the nickel foam is in an atmosphere with a precious metal ion content of 10000 μg / m3. Then brush the mixed slurry prepared in step 7 on the surface of the nickel foam in 8 times and keep heating for 8 min to make it take shape into a flat plate.

[0091] 8. Take out the flat plate fixed and formed in step 7, lay it on a mold with a parallel flow field, and then put the whole into a hot press, and hot press it at 110°C and 0.6 MPa for 1.5 min; then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filling furnace at 350°C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0092] Comparative Example 3: (Spherical dehydrogenated titanium powder without acid treatment)

[0093] 1. Select nickel foam with a pore size of 200 nm, place it in acetone, and ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for use.

[0094] 2. Measure 50 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 1 mol / L dilute hydrochloric acid solution, and set it aside for use.

[0095] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L, and set it aside for use.

[0096] 4. Immerse the nickel foam cleaned with acetone in step 1 in the precious metal solution prepared in step 3 for 8 h, then take it out and calcine it at 495°C for 40 min, and set it aside for use.

[0097] 5. Immerse the nickel foam treated in step 4 in the dilute hydrochloric acid solution prepared in step 2 for 10 min, then take it out, wash it 9 times with deionized water, and dry it at 80°C, and set it aside for use.

[0098] 6. Weigh 100 g of 25 wt.% PTFE, 50 g of spherical dehydrogenated titanium powder, and 1750 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 50 cp, and set it aside for use.

[0099] 7. Place the nickel foam treated in step 5 on a heating platform at a temperature of 150°C, and put the precious metal ion solution prepared in step 3 in a spraying device. Open the spraying device and set the spraying flow rate to 3 L / min so that the nickel foam is in an atmosphere with a precious metal ion content of 10000 μg / m 3 Then brush the mixed slurry prepared in step 6 on the surface of the nickel foam in 8 times and keep heating for 8 min to make it take shape and form a flat plate.

[0100] 8. Take out the flat plate fixed and formed in step 7, lay it on a mold with a parallel flow field, and then put the whole into a hot press, and hot press it at 110 °C and 0.6 MPa for 1.5 min; then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filling furnace at 350 °C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0101] Comparative Example 4: (The nickel foam has not been calcined at high temperature)

[0102] 1. Select nickel foam with a pore size of 200 nm and place it in acetone, and ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for later use.

[0103] 2. Measure 50 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 1 mol / L dilute hydrochloric acid solution, and set it aside for later use.

[0104] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L, and set it aside for later use.

[0105] 4. Immerse the nickel foam cleaned with acetone in step 1 in the precious metal solution prepared in step 3 for 8 h, then take it out and dry it at room temperature for later use.

[0106] 5. Immerse the nickel foam processed in step 4 in the dilute hydrochloric acid solution prepared in step 2 for 10 min, then take it out and wash it 9 times with deionized water, and dry it at 80 °C for later use.

[0107] 6. Measure 10 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 1190 mL of deionized water to prepare a dilute hydrochloric acid solution with a concentration of 0.1 mol / L; weigh spherical dehydrogenated titanium powder with a particle size of 10 nm and add it to the dilute hydrochloric acid solution, heat it to 60 °C, stir for 40 min, then take it out, wash it 4 times with ethanol, and dry it at 60 °C for later use.

[0108] 7. Weigh 100 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder processed in step 6, and 1750 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 50 cp, and set it aside for later use.

[0109] 8. Place the nickel foam after being treated in Step 5 on a heating platform at 150°C. Load the precious metal ion solution prepared in Step 3 into a spraying device. Turn on the spraying device and set the spraying flow rate to 3 L / min, so that the nickel foam is in an atmosphere with a precious metal ion content of 10,000 μg / m3. Then, brush the mixed slurry prepared in Step 7 onto the surface of the nickel foam in 8 portions, and keep heating for 8 min to make it take shape and form a flat plate.

[0110] 9. Take out the flat plate fixed and formed in Step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press. Hot press at 110°C and 0.6 MPa for 1.5 min. Then, place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filling furnace at 350°C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0111] Comparative Example 5: (The plate with a flow field is not subjected to high-temperature treatment)

[0112] 1. Select nickel foam with a pore size of 200 nm and place it in acetone. Ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for use.

[0113] 2. Measure 50 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 1 mol / L dilute hydrochloric acid solution. Set it aside for use.

[0114] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L. Set it aside for use.

[0115] 4. Immerse the nickel foam cleaned with acetone in Step 1 in the precious metal solution prepared in Step 3 for 8 h, then take it out and calcine it at 495°C for 40 min. Set it aside for use.

[0116] 5. Immerse the nickel foam treated in Step 4 in the dilute hydrochloric acid solution prepared in Step 2 for 10 min, then take it out and wash it 9 times with deionized water, and dry it at 80°C. Set it aside for use.

[0117] 6. Measure 10 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 1190 mL of deionized water to prepare a dilute hydrochloric acid solution with a concentration of 0.1 mol / L. Weigh spherical dehydrogenated titanium powder with a particle size of 10 nm and add it to the dilute hydrochloric acid solution. Heat it to 60°C and stir for 40 min, then take it out and wash it 4 times with ethanol, and dry it at 60°C. Set it aside for use.

[0118] 7. Weigh 100 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder treated in step 6, and 1750 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 50 cp, and set it aside for later use.

[0119] 8. Place the nickel foam treated in step 5 on a heating platform at a temperature of 150 °C, and put the precious metal ion solution prepared in step 3 into a spraying device. Open the spraying device and set the spraying flow rate to 3 L / min, so that the nickel foam is in an atmosphere with a precious metal ion content of 10000 μg / m³. Then, brush the mixed slurry prepared in step 7 on the surface of the nickel foam in 8 portions, and keep heating for 8 min to make it take shape and form a flat plate.

[0120] 9. Take out the flat plate fixed and formed in step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press. Hot press it at 110 °C and 0.6 MPa for 1.5 min; then take out the hot-pressed plate with a parallel flow field to form a water electrolysis anode oxygen plate with a parallel flow field.

[0121] Comparative Example 6: (The pore size of the nickel foam becomes larger, and the particle size of the titanium powder becomes larger)

[0122] 1. Select nickel foam with a pore size of 1000 nm and place it in acetone, and ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for later use.

[0123] 2. Measure 50 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 1 mol / L dilute hydrochloric acid solution, and set it aside for later use.

[0124] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L, and set it aside for later use.

[0125] 4. Immerse the nickel foam cleaned with acetone in step 1 in the precious metal solution prepared in step 3 for 8 h, then take it out and calcine it at a high temperature of 495 °C for 40 min, and set it aside for later use.

[0126] 5. Immerse the nickel foam treated in step 4 in the dilute hydrochloric acid solution prepared in step 2 for 10 min, then take it out and wash it 9 times with deionized water, and dry it at 80 °C, and set it aside for later use.

[0127] 6. Measure 10 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 1190 mL of deionized water to prepare a dilute hydrochloric acid solution with a concentration of 0.1 mol / L; weigh spherical dehydrogenated titanium powder with a particle size of 100 nm and add it to the dilute hydrochloric acid solution, heat it to 60 °C, stir for 40 min, then take it out, wash it 4 times with ethanol, and dry it at 60 °C, and set it aside for later use.

[0128] 7. Weigh 100 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder treated in step 6, and 1750 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 50 cp, and set it aside for later use.

[0129] 8. Place the nickel foam treated in step 5 on a heating platform at a temperature of 150 °C, and put the precious metal ion solution prepared in step 3 into a spraying device. Open the spraying device and set the spraying flow rate to 3 L / min so that the nickel foam is in an atmosphere with a precious metal ion content of 10000 μg / m 3 . Then brush the mixed slurry prepared in step 7 on the surface of the nickel foam in 8 times and keep heating for 8 min to make it take shape and form a flat plate.

[0130] 9. Take out the flat plate fixed and formed in step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press. Hot press it at 110 °C and 0.6 MPa for 1.5 min; then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filling furnace at 350 °C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0131] Comparative Example 7: (The nickel foam is first pickled in a dilute hydrochloric acid solution and then soaked in the precious metal solution)

[0132] 1. Select nickel foam with a pore size of 200 nm and place it in acetone, and ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for later use.

[0133] 2. Measure 50 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 1 mol / L dilute hydrochloric acid solution, and set it aside for later use.

[0134] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L, and set it aside for later use.

[0135] 4. Immerse the nickel foam cleaned with acetone in step 1 in the dilute hydrochloric acid solution prepared in step 2 for 10 min, then take it out and wash it 9 times with deionized water, and dry it at 80 °C for later use.

[0136] 5. Immerse the nickel foam treated in step 4 in the precious metal solution prepared in step 3 for 8 h, then take it out and calcine it at a high temperature of 495 °C for 40 min for later use.

[0137] 6. Measure 10 mL of 36.5 wt.% hydrochloric acid and add it to 1190 mL of deionized water to prepare a dilute hydrochloric acid solution with a concentration of 0.1 mol / L; weigh spherical dehydrogenated titanium powder with a particle size of 10 nm and add it to the dilute hydrochloric acid solution, heat to 60 °C, stir for 40 min, then take it out, wash it 4 times with ethanol, and dry it at 60 °C for standby;

[0138] 7. Weigh 100 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder treated in step 6, and 1750 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 50 cp for standby;

[0139] 8. Place the nickel foam treated in step 5 on a heating platform at a temperature of 150 °C, and place the precious metal ion solution prepared in step 3 in a spraying device. Open the spraying device and set the spraying flow rate to 3 L / min so that the nickel foam is in an atmosphere with a precious metal ion content of 10000 μg / m 3 Then brush the mixed slurry prepared in step 7 on the surface of the nickel foam in 8 times and keep heating for 8 min to form a flat plate;

[0140] 9. Take out the flat plate fixed and formed in step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press and hot press it at 110 °C and 0.6 MPa for 1.5 min; then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filled furnace at 350 °C for calcination to form a water electrolysis anode oxygen plate with a parallel flow field.

[0141] Comparative Example 8: (The slurry is brushed on the surface of the nickel foam all at once)

[0142] 1. Select nickel foam with a pore size of 200 nm and place it in acetone, ultrasonically clean it 3 times, with each ultrasonic cleaning time being 5 min. After cleaning, set it aside for standby;

[0143] 2. Measure 50 mL of 36.5 wt.% (12 mol / L) hydrochloric acid and add it to 550 mL of deionized water to prepare a 1 mol / L dilute hydrochloric acid solution for standby;

[0144] 3. Weigh 10.3 g of iridium chloride hexahydrate and dissolve it in 1000 mL of deionized water to prepare a precious metal solution with a concentration of 20 mmol / L for standby;

[0145] 4. Immerse the nickel foam cleaned with acetone in step 1 in the precious metal solution prepared in step 3 for 8 h, then take it out and calcine it at 495 °C for 40 min for standby;

[0146] 5. Immerse the nickel foam treated in Step 4 in the dilute hydrochloric acid solution prepared in Step 2 for 10 min, then take it out and wash it 9 times with deionized water, and dry it at 80 °C for standby.

[0147] 6. Measure 10 mL of 36.5 wt.% hydrochloric acid and add it to 1190 mL of deionized water to prepare a dilute hydrochloric acid solution with a concentration of 0.1 mol / L. Weigh spherical dehydrogenated titanium powder with a particle size of 10 nm and add it to the dilute hydrochloric acid solution, heat it to 60 °C, stir for 40 min, then take it out, wash it 4 times with ethanol, and dry it at 60 °C for standby.

[0148] 7. Weigh 100 g of 25 wt.% PTFE, 50 g of the spherical dehydrogenated titanium powder treated in Step 6, and 1750 g of ethanol, mix and disperse them to form a mixed slurry with a viscosity of 50 cp for standby.

[0149] 8. Place the nickel foam treated in Step 5 on a heating platform at a temperature of 150 °C, and put the precious metal ion solution prepared in Step 3 in a spraying device. Open the spraying device and set the spraying flow rate to 3 L / min, so that the nickel foam is in an atmosphere with a precious metal ion content of 10000 μg / m 3 . Then brush all the mixed slurry prepared in Step 7 onto the surface of the nickel foam at one time, and keep heating for 8 min to make it shaped into a flat plate.

[0150] 9. Take out the flat plate fixed and shaped in Step 8, lay it on a mold with a parallel flow field, and then put the whole into a hot press. Hot press it at 110 °C and 0.6 MPa for 1.5 min; then place the hot-pressed plate with a parallel flow field in a high-temperature nitrogen-filled furnace at 350 °C for calcination to form a parallel-flow-field water electrolysis anode oxygen plate.

[0151] Test conditions: The anode catalyst is 2 mg / cm 2 Ir, the cathode catalyst is 0.4 mg Pt / cm 2 70% Pt / C, the proton exchange membrane is Nafion 115 membrane, and the test temperature is 80 °C.

[0152] The electrochemical performance results of the membrane electrodes prepared with the anode oxygen plates in the examples and comparative examples are shown in Table 1.

[0153] As can be seen from Table 1, for the anode oxygen plate for water electrolysis prepared by the present invention, the membrane electrode prepared with the prepared anode oxygen plate has excellent electrochemical activity. At an electrolysis voltage of 1.8 V, its current density is all above 1900 mA / cm 2 .

[0154] In addition, use a four-probe resistance tester to directly read the measured conductivity, and the detailed data are shown in Table 1.

[0155] Table 1

[0156]

[0157] In the comparative examples, in Comparative Example 1, when applying the slurry, it was not carried out in a noble metal atmosphere, and the spherical dehydrogenated titanium powder in the prepared slurry layer was not attached by noble metal ions, resulting in low conductivity and weak antioxidant ability; the nickel foam in Comparative Example 2 was not treated with acid and its rough surface was not formed by acid etching, so the attachment rate of noble metals on its surface was low, resulting in poor conductivity of the prepared anode oxygen plate, and there was a risk of noble metal shedding on the surface of the nickel foam as the operation time increased; the spherical dehydrogenated titanium powder in Comparative Example 3 was also not treated with acid, and fewer noble metal ions adhered to the surface of the spherical dehydrogenated titanium powder during brushing in a noble metal atmosphere, and the conductive network structure of the performance was incomplete, affecting its electrical conductivity; the nickel foam soaked in the noble metal solution in Comparative Example 4 was not treated by high-temperature calcination, and noble metal ions could not form noble metal compounds (metal compounds are compounds with a lattice cross structure prepared from different metals, and their strength and stability are both good), resulting in only simple physical attachment of metal ions, and the noble metal ions were easily shed and carried away during operation, resulting in performance degradation; the plate with a flow field prepared in Comparative Example 5 was not treated at high temperature. On the one hand, the noble metal ions on the surface of the spherical dehydrogenated titanium powder were easily shed, and on the other hand, the binder could not form a uniform void network, affecting the transmission of gas and liquid, and the electrochemical performance was low; Comparative Example 6 used nickel foam with a larger pore diameter and spherical dehydrogenated titanium powder with a larger particle size. Due to the larger pore diameter of the substrate and the influence of the size of the spherical dehydrogenated titanium powder on the fineness of the material, the combined effect of the two was less than satisfactory. As can be seen from Table 1, its electrochemical performance was poor; in Comparative Example 7, the nickel foam was first soaked in an acid solution and then in a noble metal solution. Since the acid solution had a certain corrosiveness to the nickel foam, as can be seen from Table 1, soaking in the acid solution first caused the nickel wire of the nickel foam to break due to acid corrosion, and its water electrolysis performance was affected; in Comparative Example 8, the slurry was all brushed onto the surface of the nickel foam at one time, and the combined effect of the spherical dehydrogenated titanium powder inside the nickel foam was poor and the distribution was uneven. As can be seen from Table 1, its water electrolysis performance was poor.

[0158] In addition, the conductivity of the metal bipolar plate for PEM water electrolysis prepared in the prior art is between 110 - 130 S / cm. Compared with the anode oxygen plate prepared by this invention patent, the conductivity is greater than 110 S / cm, meeting the usage requirements of the bipolar plate for PEM water electrolysis hydrogen production.

[0159] This specific embodiment is only an explanation of the present invention and is not a limitation of the present invention. Those skilled in the art can make modifications without creative contributions to this embodiment according to needs after reading this specification, but as long as it is within the scope of the claims of the present invention, it is protected by the patent law.

Claims

1. A method for preparing a PEM water electrolysis anode oxygen plate, characterized in that, It includes the following steps: Step 1: Clean the nickel foam and set it aside for later use; Step 2: Immerse the nickel foam cleaned in Step 1 in a noble metal solution, take it out after the immersion ends and conduct calcination, and set it aside for later use; Step 3: Immerse the nickel foam processed in Step 2 in a hydrochloric acid solution, then wash it clean with deionized water and dry it; Step 4: Select spherical dehydrogenated titanium powder for heating and pickling, then conduct cleaning and vacuum drying, and set it aside for later use; Step 5: Mix the spherical dehydrogenated titanium powder processed in Step 4, a binder and an alcohol solvent, and disperse them to obtain a mixed slurry; Step 6: Place the nickel foam processed in Step 3 on a heating platform, and simultaneously spray the noble metal solution so that the nickel foam is in an atmosphere of atomized noble metal solution. At the same time, brush the mixed slurry prepared in Step 5 multiple times and heat it to be fixed into a shape to form a flat plate; Step 7: Take out the flat plate fixed into a shape in Step 6, lay the flat plate fixed into a shape on a mold with a parallel flow field, and then put the whole into a hot press for hot pressing; Step 8: Place the plate with a parallel flow field hot-pressed in Step 7 in a nitrogen-filling furnace for calcination to form a water electrolysis anode oxygen plate with a parallel flow field; In Step 2, the noble metal solution is any one of iridium chlorate hexahydrate solution, ruthenium chloride trihydrate, and palladium chloride solution. The content of noble metal ions in the noble metal solution is 20 - 50 mmol / L, the immersion time is 4 - 8 h, the calcination time is 20 - 40 min, and the calcination temperature is 495 - 580 °C; In Step 6, the sprayed noble metal solution is the same as the noble metal solution used in Step 2; Among them, the pore diameter of the nickel foam is 200 - 400 nm; the particle size of the spherical dehydrogenated titanium powder is 10 - 30 nm.

2. The preparation method of the PEM water electrolysis anode oxygen plate according to claim 1, characterized in that, In Step 1, the solution for cleaning the nickel foam is an acetone solution, the cleaning method is ultrasonic cleaning, the number of cleaning times is 3 - 5 times, and the ultrasonic cleaning time each time is 3 - 5 min.

3. The preparation method of the PEM water electrolysis anode oxygen plate according to claim 1, characterized in that, In Step 3, the concentration of the hydrochloric acid solution is 1 - 3 mol / L, the immersion time is 5 - 10 min, the number of times of washing with deionized water is 6 - 9 times, and the drying temperature is 60 - 80 °C.

4. The method for preparing the PEM water electrolysis anode oxygen plate according to claim 1, characterized in that In Step 4, the method for heating and pickling the spherical dehydrogenated titanium powder is: place the spherical dehydrogenated titanium powder in an acid solution, and use a stirrer with a heating function to achieve heating and stirring of the spherical dehydrogenated titanium powder; the pickling time of the spherical dehydrogenated titanium powder is 20 - 40 min, the heating temperature is 40 - 60 °C, the acid solution is any one of hydrochloric acid solution, oxalic acid solution, and formic acid solution, and the concentration of the acid solution is 0.1 - 0.5 mol / L; Use an alcohol solvent for cleaning. The alcohol solvent is any one of methanol, ethanol, and n-propanol; the number of times of cleaning with the alcohol solvent is 4 - 7 times; the drying temperature is 60 - 80 °C.

5. The preparation method of the PEM water electrolysis anode oxygen plate according to claim 1, characterized in that, In Step 5, the binder is a PTFE emulsion with a concentration of 25 wt%; the alcohol solvent is any one of methanol, ethanol, and n-propanol; the mass ratio of the spherical dehydrogenated titanium powder, the binder and the alcohol solvent is 1:0.5 - 0.8:20 - 35; the dispersion method is any one of ultrasonic dispersion and high-speed stirring dispersion; the viscosity of the mixed slurry is 50 - 120 cp.

6. The preparation method of the PEM water electrolysis anode oxygen plate according to claim 1, characterized in that, In Step 6, the temperature of the heating platform is 120-150 °C; the atomized precious metal solution is sprayed by an atomizing nozzle, the spraying flow rate of the precious metal solution is 3-5 L / min, and the precious metal suspension concentration in the atomized state atmosphere of the precious metal solution is 10,000-25,000 μg / m 3 ; the brushing times are 5-8 times; the heating and fixing forming time is 4-8 min.

7. The method for preparing the PEM water electrolysis anode oxygen plate according to claim 1, wherein, In Step 7, the temperature for hot pressing is 80 - 110 °C; the pressure is 0.6 - 0.9 MPa; and the hot pressing time is 1.5 - 3 min.

8. The method for preparing the PEM water electrolysis anode oxygen plate according to claim 1, wherein, In Step 7, the mold with a parallel flow field is made of stainless steel material. The mold includes a base plate (1), and two or more raised structures (2) are installed on the base plate (1) at intervals and placed in parallel; After the mold is pressed on the nickel foam, the concave channel pattern formed by the raised structure (2) on the surface of the nickel foam is a parallel flow field structure.

9. The preparation method of the PEM water electrolysis anode oxygen plate according to claim 1, characterized in that, In Step 8, the temperature for calcination in the nitrogen-filling furnace is 350 - 450 °C.

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