CN117039010A - Membrane electrode catalyst layer, preparation method thereof and proton exchange membrane fuel cell - Google Patents
Membrane electrode catalyst layer, preparation method thereof and proton exchange membrane fuel cell Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 263
- 239000012528 membrane Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims description 21
- 239000000446 fuel Substances 0.000 title claims description 16
- 239000002002 slurry Substances 0.000 claims abstract description 211
- 238000005507 spraying Methods 0.000 claims abstract description 157
- 239000007921 spray Substances 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 20
- 229920000557 Nafion® Polymers 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 16
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical group [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 10
- 239000001099 ammonium carbonate Substances 0.000 claims description 10
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 8
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 31
- 229920000642 polymer Polymers 0.000 abstract description 3
- 238000004537 pulping Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 68
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 42
- 238000010008 shearing Methods 0.000 description 34
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 33
- 238000003756 stirring Methods 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 17
- 229910021641 deionized water Inorganic materials 0.000 description 17
- 238000003860 storage Methods 0.000 description 17
- 238000001816 cooling Methods 0.000 description 16
- 239000002184 metal Substances 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 15
- 210000004027 cell Anatomy 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 229910052697 platinum Inorganic materials 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000011068 loading method Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 210000000170 cell membrane Anatomy 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical group OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inert Electrodes (AREA)
Abstract
Compared with the prior art, the application designs two catalyst slurries with different concentrations, designs the raw materials, the dosage ratio and the concentration, and realizes the effective improvement of the performance of the membrane electrode by utilizing the simultaneous spraying of the gradient catalytic layer; the consistency of the spraying thickness is effectively improved by utilizing the combination of different spraying angles of the double nozzles; and the double nozzles are utilized for high-efficiency spraying, so that layering and the like caused by repeated pulping and intermittent spraying are effectively avoided. And the application utilizes double-nozzle spraying, and realizes gradient configuration of porosity by reducing the polymer content in the outer catalyst slurry and increasing the pore-forming agent content. The two spray heads are utilized to set vertical angle spraying, so that the problem of inconsistent spraying thickness of the fan-shaped spraying which is thick in the middle and thin on two sides is effectively avoided.
Description
Technical Field
The application belongs to the technical field of membrane electrodes of hydrogen fuel cells, and particularly relates to a membrane electrode catalyst layer, a preparation method thereof and a proton exchange membrane fuel cell.
Background
The fuel cell is a power generation device for directly converting chemical energy into electric energy, has the characteristics of environmental friendliness, high energy conversion efficiency, long service life and the like, and has been widely applied in various fields. Membrane Electrodes (MEA) are the core sites for multiphase mass transport and electrochemical reactions within a fuel cell, the quality of which directly determines the performance, life and cost of a proton exchange membrane fuel cell.
The Membrane Electrode (MEA) consists of a proton exchange membrane, a catalytic layer and a gas diffusion layer, the proton exchange membrane adopted at present is mainly a perfluorosulfonic acid proton exchange membrane, the proton conductivity of the perfluorosulfonic acid is seriously dependent on the hydration state of the membrane, when the membrane electrode loses water, the proton conductivity of the membrane electrode is obviously reduced, ohmic polarization is increased, the water content is too high, the transmission resistance of reaction gas is increased, and the performance of the cell is influenced. Therefore, whether the membrane electrode of the proton exchange membrane fuel cell can stably operate with high performance and long service life is closely related to the internal water management of the electrode. The graded catalyst layer may have improved proton conductivity and water management of the proton membrane.
According to the current research progress, the CCM structure membrane electrode with the catalyst coated on the surface of the polymer electrolyte membrane is an electrode structure widely adopted by various fuel cells at present because of lower electrode internal resistance, higher catalyst utilization rate and excellent interface compatibility. In the existing catalyst spraying equipment for producing the fuel cell membrane electrode, a single spray head is generally adopted, and an intermittent operation mode is adopted; if the gradient catalytic layer is to be prepared, a slurry is required to be prepared first, the film is placed in a spraying area, a single spray head is adopted to finish the first spraying, the slurry is required to be reconfigured after the first spraying is finished, the second spraying is performed after waiting for a period of time, the spraying work cannot be continuously performed, the production efficiency is reduced, the surface of the coating is partially dried and is easy to delaminate, dust and impurities are easy to adhere, the spraying direction cannot be changed rapidly, the middle of the spraying thickness is thick, the two sides are thin, the thickness is uneven, and the consistency of products is affected. Thus, there is a need for adjustments to existing ultrasonic spray equipment and processes.
An ultrasonic spraying method for preparing a porous catalytic layer of a fuel cell membrane electrode is disclosed in publication No. CN 112259749A, which is published in 1 month of 2021, and the gradient configuration of the porosity of the porous catalytic layer and the component content of a high polymer additive solution along the thickness direction of the catalytic layer is completed by arranging a spraying auxiliary way and a control system for controlling the component content of the catalytic layer along with the spraying time. However, the parameters of the spraying equipment need to be continuously adjusted in the spraying process, the process is not well controlled, and the problem of the difference of the spraying thickness cannot be solved.
The utility model provides a spraying frock of publication number CN 211637051U that 9 days of 2020 published 10 months discloses spraying equipment with high efficiency, including the frame, sets up the spraying case in the frame, the spraying case is provided with material transfer module, material transfer module is including arranging the spraying district of spraying incasement portion in, sets up the carrying area in spraying case outside, the top of spraying district is provided with the coating subassembly, the fixed setting in coating subassembly and spraying case top, material transfer module still includes convertible work piece clamping component, and this technique can improve CCM preparation efficiency, but can not solve the inconsistent problem of spraying thickness.
Disclosure of Invention
The application aims to provide a membrane electrode catalyst layer and a preparation method thereof, wherein the membrane electrode catalyst layer is prepared by using single-sided double nozzles, the spraying of the double nozzles at different spraying angles is controlled, and the components and the concentration of spraying slurry of the catalyst layer are controlled, so that the gradient of the catalyst is realized, the thickness is uniform and the height is consistent. Solves the technical problems of great loss of single catalytic layer spraying catalytic layer pores and inconsistent spraying thickness in the preparation of the membrane electrode by a spraying method in the prior art.
The proton exchange membrane fuel cell provided by the application comprises the membrane electrode catalyst layer.
The specific technical scheme of the application is as follows:
a method for preparing a membrane electrode catalyst layer, comprising the steps of:
1) Preparing a catalyst slurry A and a catalyst slurry B containing pore-forming agents;
2) And (3) spraying catalyst slurry A and catalyst slurry B on the proton exchange membrane by using a double nozzle to obtain a membrane electrode catalyst layer.
In the step 1), the raw materials of the catalyst slurry A comprise a catalyst, a solvent and a Nafion solution;
in the step 1), in the catalyst slurry a, the mass ratio of the catalyst, the solvent and the Nafion solution is: 10:92-96:2.9-3.3; preferably 10:95:3.
In the step 1), the raw materials of the catalyst slurry B comprise a catalyst, a solvent, a Nafion solution and a pore-forming agent;
in the catalyst slurry B, the mass ratio of the catalyst to the solvent to the Nafion solution to the pore-forming agent is 10:92-96:1.0-3.3:1-2;
in the catalyst slurry A and the catalyst slurry B, the catalyst is a catalyst with the weight percentage of metal of 10-70 percent; the catalyst is selected from one or more of Pt/C, ptCo/C, ptRu/C; the solvent is a mixture of water and an alcohol solvent; the mass ratio of the water to the alcohol solvent is 4-6:5-7, preferably 4:5.5; the water is preferably deionized water; the alcohol solvent is selected from one or more of ethanol, isopropanol, n-propanol and ethylene glycol; the mass concentration of the Nafion solution is 20%, and the Nafion solution is a commercial product.
In the catalyst slurry B, the pore-forming agent is selected from ammonium bicarbonate, ammonium carbonate or ammonium nitrate;
in the step 1), the preparation method of the catalyst slurry A comprises the following steps: adding a catalyst into deionized water, adding an alcohol solvent with the formula amount of 65-70%, and finally adding a Nafion solution, and magnetically stirring to form a premix; cooling the premix in a water bath, and dispersing by adopting ultrasonic waves; adding alcohol solvent with the residual amount of the formula into the slurry after ultrasonic dispersion, and dispersing by adopting sealed high-speed shearing, thus obtaining the required catalyst slurry A after the dispersion is completed.
In the preparation method of the catalyst slurry A, the magnetic stirring rotating speed is 400-600rpm, and the stirring time is 3-8min; the ultrasonic dispersion time is 10-20min, and the ultrasonic power is 500-700W; the water bath temperature is 25-30 ℃; the sealed high-speed shearing dispersion is carried out for 2-3min, the shearing line speed is 20-30m/s, and the temperature is kept at 25-30 ℃.
In the step 1), the preparation method of the catalyst slurry B comprises the following steps: adding a catalyst into deionized water, adding an alcohol solvent with the formula amount of 65-70%, and finally adding a Nafion solution and a pore-forming agent, and magnetically stirring to form a premix; cooling the premix in a water bath, and dispersing by adopting ultrasonic waves; adding alcohol solvent with the residual amount of the formula into the slurry after ultrasonic dispersion, and dispersing by adopting sealed high-speed shearing, thus obtaining the required catalyst slurry B after the dispersion is completed.
In the preparation method of the catalyst slurry B, the magnetic stirring rotation speed is 400-600rpm, and the stirring time is 3-8min; the ultrasonic dispersion time is 10-20min, and the ultrasonic power is 500-700W; the water bath temperature is 25-30 ℃; the sealed high-speed shearing dispersion is carried out for 2-3min, the shearing line speed is 20-30m/s, and the temperature is kept at 25-30 ℃.
In the application, the preparation method of the catalyst slurry B is the same as the preparation method of the catalyst slurry A, except that the pore-forming agent is added into the catalyst slurry B.
In step 2), two nozzles, one for spraying catalyst slurry A and the other for catalyst slurry B;
in the step 2), the mass ratio of the catalyst slurry A to the catalyst slurry B sprayed is as follows: 1:0.9-1.1, preferably 1:1;
in the step 2), an included angle of 0-90 degrees is formed between the spraying angle of the spraying catalyst slurry A and the spraying angle of the spraying catalyst slurry B.
In the step 2), a spray head for spraying the catalyst slurry A is arranged above the proton exchange membrane, the flow rate of a catalyst slurry flow path is set to be constant 0.3-0.6mL/min, and the spraying time is 8-15min; the spray head for the catalyst slurry B is arranged above the proton exchange membrane, and the flow is initially set to be 0.3-1mL/min; the spraying time is 8-15min. Spray catalysisThe spray angle of the catalyst slurry A and the spray angle of the spray catalyst slurry B form an included angle of 0-90 degrees, and the included angle is not 0 degrees, and is preferably 90 degrees. The whole catalytic layer is sprayed, and the anode catalyst layer is controlled to be 0.05-0.07mg/cm 2 The cathode catalyst layer is controlled to be 0.25-0.33mg/cm 2 CCM controls platinum loading to 0.3-0.4mg/cm 2 。
The application realizes gradient configuration of porosity by spraying different catalyst slurries by double nozzles by using a preparation method of a single-sided fixed double-nozzle hydrogen fuel cell membrane electrode, and reduces uneven spraying thickness by using complementation of different spraying angles of a spray head.
The membrane electrode catalyst layer provided by the application is prepared by adopting the method.
The proton exchange membrane fuel cell provided by the application comprises the membrane electrode catalyst layer.
Compared with the prior art, the application designs two catalyst slurries with different concentrations, designs the raw materials, the dosage ratio and the concentration, and realizes the simultaneous spraying of the gradient catalytic layers so as to effectively improve the performance of the membrane electrode; the consistency of the spraying thickness is effectively improved by utilizing the combination of different spraying angles of the double nozzles; and the double nozzles are utilized for high-efficiency spraying, so that layering and the like caused by repeated pulping and intermittent spraying are effectively avoided. And the application utilizes double-nozzle spraying, and realizes gradient configuration of porosity by reducing the polymer content in the outer catalyst slurry and increasing the pore-forming agent content. The two spray heads are used for setting the spray direction to have an included angle for spraying, so that the problem that the spray thickness of the fan-shaped spray is inconsistent in the middle and the two sides are thin is effectively avoided.
Drawings
FIG. 1 is a schematic view of an ultrasonic spray apparatus of the present application;
FIG. 2 is a comparison of polarization curves of membrane electrode samples obtained in example 1 of the present application and comparative examples 1, 2, and 3;
the figure indicates: 5-a catalyst slurry a nozzle; 1-a catalyst slurry A spray cavity; 7-a main pipe of catalyst slurry A; 9-a catalyst slurry a holding tank; 15-catalyst slurry B nozzle; 11-a catalyst slurry B spray cavity; 17-a main pipe of catalyst slurry B; 19-a catalyst slurry B holding tank; 13-proton exchange membrane.
Detailed Description
The present technical scheme is further described in detail below with reference to the accompanying drawings.
Example 1
A method for preparing a membrane electrode catalyst layer, comprising the steps of:
1) Catalyst slurry a: taking 10g of a Pt/C catalyst with the metal weight percentage of 50%wt, adding 40mL of deionized water, adding 47mL of isopropanol, adding 3mL of 20%wt Nafion solution, and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
2) Catalyst slurry B: taking 10g of a Pt/C catalyst with the metal weight percentage of 50%wt, adding 40mL of deionized water, adding 47mL of isopropanol, adding 1.5mL of LNafion (20%), and adding 1.5g of ammonium carbonate, and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
3) CCM spraying: and (3) attaching the proton exchange membrane to a spraying base station of ultrasonic spraying equipment in an adsorption manner, and heating the spraying base station to 100 ℃, wherein the ultrasonic spraying equipment comprises spraying equipment for catalyst slurry A and catalyst slurry B. The spraying of the catalyst slurry A comprises a catalyst slurry A storage tank 9 for storing the catalyst slurry A, the catalyst slurry A is connected with a catalyst slurry A main pipe 7, the catalyst slurry A main pipe 7 is connected with a catalyst slurry A spraying cavity 1, and the catalyst slurry A spraying cavity 1 is connected with a catalyst slurry A nozzle 5. The catalyst slurry A is stored in a catalyst slurry A storage tank 9, when spraying is needed, the catalyst slurry A flows into a catalyst slurry A main pipe 7 and a catalyst slurry A spray 1 in sequence through the catalyst slurry A storage tank 9, the flow rate of a flow path is set to be constant 0.5mL/min, and finally the catalyst is catalyzedAnd a catalyst slurry A nozzle 5, wherein the catalyst slurry A is sprayed on the surface of the proton exchange membrane for 10min. The spraying of the catalyst slurry B includes a catalyst slurry B storage tank 19 for storing the catalyst slurry B, which is connected to the catalyst slurry B main pipe 17, the catalyst slurry B main pipe 17 is connected to the catalyst slurry B spraying chamber 11, and the catalyst slurry B spraying chamber 11 is connected to the catalyst slurry B nozzle 15. When spraying is needed, the catalyst slurry B flows into a catalyst slurry B main pipe 17 and a catalyst slurry B spray 11 sequentially through the catalyst slurry B storage tank 19, finally reaches a catalyst slurry B spray nozzle 15, a catalyst slurry A spray nozzle 5 is perpendicular to proton membrane spraying, the catalyst slurry B spray nozzle 15 rotates 90 degrees relative to the catalyst slurry A spray nozzle 5, namely, a 90-degree included angle is formed between the spraying angle of the catalyst slurry A and the spraying angle of the catalyst slurry B, the catalyst slurry B is sprayed on the surface of the proton exchange membrane, the flow is initially set to 0.5mL/min, and the spraying time is 10min; platinum loading of 0.05-0.4mg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The mass ratio of the catalyst slurry A to the catalyst slurry B is 1:1; and (3) finishing the spraying of the anode catalytic layer, spraying the cathode catalytic layer, and controlling the anode catalytic layer to be 0.06mg/cm after all spraying is finished 2 The cathode catalyst layer was controlled to 0.30mg/cm 2 CCM controls platinum loading to 0.3-0.4mg/cm 2 ；
A proton exchange membrane fuel cell comprises the membrane electrode catalyst layer, and the specific preparation method comprises the following steps:
1) A membrane electrode catalyst layer was prepared in the same manner as in example 1;
2) MEA preparation:
feeding CCM, a frame and a diffusion layer GDL, cutting the size outline of an active area, cutting the active area into pieces, and discharging and collecting the pieces; placing the cut frame and CCM, and attaching the sheet material in alignment to form MEA-5; placing a sheet GDL and dispensing a cathode GDL; performing MEA-5/MEA-7 assembly, and placing into a heat curing device; placing the MEA-7 into a finished product cutting machine, and die-cutting to obtain an MEA-7 product; and the MEA-7 product sequentially performs air tightness detection and electrical property detection.
Comparative example 1
A method for preparing a membrane electrode catalyst layer, comprising the steps of:
1) Catalyst slurry a: taking 10g of a Pt/C catalyst with the metal weight percentage of 50% and adding 40mL of deionized water, 47mL of isopropanol and 3mL of 20% Naf ion solution, and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
2) Catalyst slurry B: taking 10g of a Pt/C catalyst with the metal weight percentage of 50% and adding 40mL of deionized water, 47mL of isopropanol and 3mL of 20% Naf ion solution, and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
3) The CCM spraying comprises the steps of adsorbing and attaching a proton exchange membrane to a spraying base of ultrasonic spraying equipment, heating the spraying base to 100 ℃, transferring catalyst slurry A to a catalyst slurry A storage tank 9, setting the flow of a catalyst slurry A flow path to be constant 0.5mL/min, spraying for 10min, transferring catalyst slurry B to a catalyst slurry B storage tank, setting a catalyst slurry B nozzle 15 above the proton exchange membrane, spraying the catalyst slurry A nozzle 5 perpendicular to the proton membrane, rotating the catalyst slurry B nozzle 15 by 90 degrees relative to the catalyst slurry A nozzle 5, namely forming a 90-degree included angle between the spraying angle of the catalyst slurry A and the spraying angle of the catalyst slurry B, and initially setting the flow to be 0.5mL/min, wherein the spraying time is 10min; the mass ratio of the catalyst slurry A to the catalyst slurry B is 1:1; and (3) finishing the spraying of the anode catalytic layer, spraying the cathode catalytic layer, and controlling the anode catalytic layer to be 0.06mg/cm after all spraying is finished 2 The cathode catalyst layer was controlled to 0.30mg/cm 2 CCM controls platinum loading to 0.3-0.4mg/cm 2 ；
Example 2
A method for preparing a membrane electrode catalyst layer, comprising the steps of:
1) Catalyst slurry a: : taking 10g of a Pt/C catalyst with the metal weight percentage of 50%wt, adding 40mL of deionized water, adding 47mL of isopropanol, adding 3mL of Nafion (20 wt%) and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
2) Catalyst slurry B: taking 10g of a Pt/C catalyst with the metal weight percentage of 50% and adding 40mL of deionized water, then adding 47mL of isopropanol, finally adding 1mL of Nafion (20%), 2g of ammonium carbonate, and magnetically stirring for 5min at a rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
3) The CCM spraying comprises the steps of adsorbing and attaching a proton exchange membrane to a spraying base of ultrasonic spraying equipment, heating the spraying base to 100 ℃, transferring catalyst slurry A to a catalyst slurry A storage tank 9, setting the flow of a catalyst slurry A flow path to be constant 0.5mL/min, spraying for 10min, transferring catalyst slurry B to a catalyst slurry B storage tank, setting a catalyst slurry B nozzle 15 above the proton exchange membrane, spraying the catalyst slurry A nozzle 5 perpendicular to the proton membrane, rotating the catalyst slurry B nozzle 15 by 90 degrees relative to the catalyst slurry A nozzle 5, namely forming a 90-degree included angle between the spraying angle of the catalyst slurry A and the spraying angle of the catalyst slurry B, and initially setting the flow to be 0.5mL/min, wherein the spraying time is 10min; the mass ratio of the catalyst slurry A to the catalyst slurry B is 1:1; and (3) finishing the spraying of the anode catalytic layer, spraying the cathode catalytic layer, and controlling the anode catalytic layer to be 0.06mg/cm after all spraying is finished 2 The cathode catalyst layer was controlled to 0.30mg/cm 2 CCM control of platinum loading0.3-0.4mg/cm 2 ；
Example 3
A method for preparing a membrane electrode catalyst layer, comprising the steps of:
1) Catalyst slurry a: taking 10g of a Pt/C catalyst with the metal weight percentage of 50% and adding 40mL of deionized water, adding 47mL of isopropanol, adding 3mL of LNafi on (20 wt%) and magnetically stirring at 500rpm for 5min to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
2) Catalyst slurry B: taking 10g of Pt/C catalyst with the metal weight percentage of 50% and adding 40mL of deionized water, then adding 47mL of isopropanol, finally adding 2mL of LNafi on (20% by weight), and 1g of ammonium carbonate, and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
3) CCM spraying: attaching the proton exchange membrane to a spraying base of ultrasonic spraying equipment in an adsorption manner, heating the spraying base to 100 ℃, transferring catalyst slurry A into a catalyst slurry A storage tank 9, enabling a catalyst slurry A nozzle 5 to be positioned above the proton exchange membrane, setting the flow of a catalyst slurry A flow path to be constant 0.5mL/min, enabling the spraying time to be 10min, transferring catalyst slurry B into a catalyst slurry B storage tank, enabling a catalyst slurry B nozzle 15 to be positioned above the proton exchange membrane, enabling the catalyst slurry A nozzle 5 to be perpendicular to proton membrane spraying, enabling the catalyst slurry B nozzle 15 to rotate 90 degrees relative to the catalyst slurry A nozzle 5, namely enabling a 90-degree included angle to be formed between the catalyst slurry A spraying angle and the spraying catalyst slurry B spraying angle, enabling the flow to be initially set to be 0.5mL/min, and enabling the spraying time to be 10min; the mass ratio of the catalyst slurry A to the catalyst slurry B is 1:1; the anode catalytic layer spraying is finished, the cathode catalytic layer spraying is carried out, all spraying is finished, and the anode catalytic layer is controlled at 0.06mg/cm 2 The cathode catalyst layer was controlled to 0.30mg/cm 2 CCM controls platinum loading to 0.3-0.4mg/cm 2 ；
Example 4
A method for preparing a membrane electrode catalyst layer, comprising the steps of:
1) Catalyst slurry a: taking 10g of a Pt/C catalyst with the metal weight percentage of 50%wt, adding 40mL of deionized water, adding 47mL of isopropanol, adding 3mLNaf (20%), and magnetically stirring at 500rpm for 5min to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
2) Catalyst slurry B: taking 10g of a Pt/C catalyst with the metal weight percentage of 50% and adding 40mL of deionized water, adding 47mL of isopropanol, adding 1.5mL of LNaf ion (20%), and 1.5g of ammonium carbonate, and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
3) CCM spraying: attaching the proton exchange membrane to a spraying base of ultrasonic spraying equipment in an adsorption manner, heating the spraying base to 100 ℃, transferring catalyst slurry A into a catalyst slurry A storage tank 9, enabling a catalyst slurry A nozzle 5 to be positioned above the proton exchange membrane, setting the flow of a catalyst slurry A flow path to be constant 0.5mL/min, enabling the spraying time to be 10min, transferring catalyst slurry B into a catalyst slurry B storage tank, enabling a catalyst slurry B nozzle 15 to be positioned above the proton exchange membrane, enabling the catalyst slurry A nozzle 5 to be perpendicular to proton membrane spraying, enabling the catalyst slurry B nozzle 15 to rotate by 30 degrees relative to the catalyst slurry A nozzle 5, namely enabling a 30-degree included angle to be formed between the catalyst slurry A spraying angle and the spraying catalyst slurry B spraying angle, enabling the flow to be initially set to be 0.5mL/min, and enabling the spraying time to be 10min; the mass ratio of the catalyst slurry A to the catalyst slurry B is 1:1; the anode catalytic layer spraying is finished,spraying the cathode catalyst layer, and controlling the anode catalyst layer to be 0.06mg/cm after all spraying is finished 2 The cathode catalyst layer was controlled to 0.30mg/cm 2 CCM controls platinum loading to 0.3-0.4mg/cm 2 ；
Example 5
A method for preparing a membrane electrode catalyst layer, comprising the steps of:
1) Catalyst slurry a: taking 10g of a Pt/C catalyst with the metal weight percentage of 50%wt, adding 40mL of deionized water, adding 47mL of isopropanol, adding 3mL of LNafion (20 wt%) and magnetically stirring for 5min at a rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
21 Catalyst slurry B): taking 10g of a Pt/C catalyst with the metal weight percentage of 50% and adding 40mL of deionized water, adding 47mL of isopropanol, adding 1.5mL of LNafion (20 wt%) and 1.5g of ammonium carbonate, and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
3) CCM spraying: attaching the proton exchange membrane to a spraying base of ultrasonic spraying equipment in an adsorption manner, heating the spraying base to 100 ℃, transferring catalyst slurry A into a catalyst slurry A storage tank 9, setting the flow of a catalyst slurry A flow path to be constant 0.5mL/min, spraying for 10min, transferring catalyst slurry B into a catalyst slurry B storage tank, setting a catalyst slurry B nozzle 15 above the proton exchange membrane, spraying the catalyst slurry A nozzle 5 perpendicular to the proton membrane, and rotating the catalyst slurry B nozzle 15 by 60 degrees relative to the catalyst slurry A nozzle 5, wherein a 60-degree included angle is formed between the spraying angle of the catalyst slurry A and the spraying angle of the catalyst slurry B, the flow is initially set to be 0.5mL/min, and the spraying time is 10min; sprayingCatalyst slurry A and catalyst slurry B are coated in a mass ratio of 1:1; and (3) finishing the spraying of the anode catalytic layer, spraying the cathode catalytic layer, and controlling the anode catalytic layer to be 0.06mg/cm after all spraying is finished 2 The cathode catalyst layer was controlled to 0.30mg/cm 2 CCM controls platinum loading to 0.3-0.4mg/cm 2 ；
Comparative example 2
A method for preparing a membrane electrode catalyst layer, comprising the steps of:
1) Catalyst slurry a: taking 10g of a Pt/C catalyst with the metal weight percentage of 50%wt, adding 40mL of deionized water, adding 47mL of isopropanol, adding 3mL of LNafion (20 wt%) and magnetically stirring for 5min at a rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
2) Catalyst slurry B: taking 10g of a Pt/C catalyst with the metal weight percentage of 50% and adding 40mL of deionized water, adding 47mL of isopropanol, adding 1.5mL of LNafion (20 wt%) and 1.5g of ammonium carbonate, and magnetically stirring for 5min at the rotating speed of 500rpm to form a premix; cooling the premix in a 29 ℃ water bath, dispersing for 15min by adopting 500W ultrasonic waves, adding 23ml of isopropanol, and carrying out sealed high-speed shearing and dispersing for 3min, wherein the shearing line speed is 30m/s, the temperature is kept at 25-30 ℃, and the required slurry is prepared after the dispersing is completed;
3) CCM spraying: attaching the proton exchange membrane to a spraying base station of ultrasonic spraying equipment in an adsorption manner, heating the spraying base station to 100 ℃, transferring catalyst slurry A into a catalyst slurry A storage tank 9, setting the flow of a catalyst slurry A flow path to be constant 0.5mL/min, setting the spraying time to be 10min, transferring catalyst slurry B into a catalyst slurry B storage tank, setting a catalyst slurry B nozzle 15 above the proton exchange membrane, spraying the catalyst slurry A nozzle 5 perpendicular to the proton membrane, and forming a 0-degree clamp between the catalyst slurry A spraying angle and the spraying catalyst slurry B spraying angle, wherein the spraying angle is the same as that of the catalyst slurry B nozzle 15Angle, flow is initially set to 0.5mL/min, and spraying time is 10min; the mass ratio of the catalyst slurry A to the catalyst slurry B is 1:1; and (3) finishing the spraying of the anode catalytic layer, spraying the cathode catalytic layer, and controlling the anode catalytic layer to be 0.06mg/cm after all spraying is finished 2 The cathode catalyst layer was controlled to 0.30mg/cm 2 CCM controls platinum loading to 0.3-0.4mg/cm 2 ；
The main parameters for the preparation of the membrane electrode of the examples and comparative examples are shown in Table 1.
TABLE 1 Main parameters in the preparation of Membrane electrodes of examples and comparative examples
By comparing the polarization curves of the membrane electrode in the embodiment 1 with those in the comparative embodiment 1 and the embodiment 2 and the embodiment 3, as can be obtained by comparing the graph in fig. 2, the catalyst outer layer increases the content of the pore-forming agent, thereby effectively improving the power density of the membrane electrode; this is because the pore-forming agent increases the porosity of the catalyst layer, facilitating the passage of reactant gases into the catalyst layer through the proton exchange membrane, while the Nafion (r) adhesive layer, while being effective in reducing the ohmic polarization resistance, reduces the gas diffusion rate of the catalyst layer.
As can be seen from table 2, the difference in catalyst layer thickness between comparative example 1 and examples 4 and 5, and comparative example 2, the spray head corresponding to slurry B was rotated by a certain angle, so that the superposition of the middle dense area of the fan-shaped spray surface was reduced, and the dispersion was more uniform.
Table 2 difference in thickness of the cathode catalytic layer of the membrane electrode in example 1 and examples 4, 5 and 6
The foregoing descriptions of specific exemplary embodiments of the present application are presented for purposes of illustration and description. It is not intended to limit the application to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the application and its practical application to thereby enable others skilled in the art to make and utilize the application in various embodiments. Embodiments, and various alternatives and modifications. It is intended that the scope of the application be defined by the claims and their equivalents.
Claims (10)
1. A method of preparing a membrane electrode catalyst layer, the method comprising the steps of:
1) Preparing a catalyst slurry A and a catalyst slurry B containing pore-forming agents;
2) And (3) spraying catalyst slurry A and catalyst slurry B on the proton exchange membrane by using a double nozzle to obtain a membrane electrode catalyst layer.
2. The method of claim 1, wherein in step 1), the catalyst slurry a feedstock comprises a catalyst, a solvent, and a Nafion solution.
3. The preparation method according to claim 2, wherein in the step 1), the mass ratio of the catalyst, the solvent and the Nafion solution in the catalyst slurry a is: 10:92-96:2.9-3.3.
4. The preparation method according to claim 1, wherein the raw materials of the catalyst slurry B include a catalyst, a solvent, a Nafion solution and a pore-forming agent.
5. The preparation method according to claim 4, wherein the mass ratio of the catalyst, the solvent, the Nafion solution and the pore-forming agent in the catalyst slurry B is 10:92-96:1.0-3.3:0-2.
6. The method according to claim 4 or 5, wherein in step 1), the pore-forming agent is selected from ammonium bicarbonate, ammonium carbonate or ammonium nitrate.
7. The preparation method according to claim 1, wherein in the step 2), the mass ratio of the sprayed catalyst slurry a to the sprayed catalyst slurry B is: 1:0.9-1.1.
8. The method of claim 2, wherein in step 2), the twin nozzles, one for spraying catalyst slurry a and the other for catalyst slurry B; the spray angle of the spray catalyst slurry A and the spray angle of the spray catalyst slurry B form an included angle of 0-90 degrees.
9. A membrane electrode catalyst layer prepared by the method of any one of claims 1 to 8.
10. A proton exchange membrane fuel cell comprising the membrane electrode catalyst layer of claim 9.
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