CN113871633A - Method for high-efficiency in-situ activation of membrane electrode of proton exchange membrane fuel cell - Google Patents
Method for high-efficiency in-situ activation of membrane electrode of proton exchange membrane fuel cell Download PDFInfo
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- CN113871633A CN113871633A CN202111131874.7A CN202111131874A CN113871633A CN 113871633 A CN113871633 A CN 113871633A CN 202111131874 A CN202111131874 A CN 202111131874A CN 113871633 A CN113871633 A CN 113871633A
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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
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- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a method for efficiently activating a membrane electrode of a proton exchange membrane fuel cell in situ. Firstly, adding materials such as carbon, pore-forming agent and the like into catalyst slurry, then ultrasonically spraying the slurry to two sides of a proton exchange membrane, and attaching gas diffusion layers to the two sides to obtain the membrane electrode. Activation is carried out by the following steps: (1) assembling the membrane electrode into a single cell, wherein the temperature of the cell is 20-90 ℃, the relative humidity of a cathode and an anode is 20-100%, and the stoichiometric amounts of hydrogen and air are 1.0-4.0 and 1.0-5.0 respectively; (2) respectively controlling the voltage of the battery at 0.8-0.9V, 0.5-0.8V and 0.3-0.5V, and respectively controlling the duration time at 0.5-3 min, 0.5-5 min and 0.5-5 min; (3) and (3) circulating the step (2) for 2-8 times. The invention optimizes the three-phase interface of the membrane electrode by voltage cycle and adding materials such as carbon, pore-forming agent and the like, improves the diffusion and transmission of water, gas and electrons, and shortens the activation time of the membrane electrode. Compared with the traditional activation method, the in-situ activation method has the advantages of simple process, short time and high efficiency.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to a method for efficiently activating a membrane electrode of a proton exchange membrane fuel cell in situ.
Background
A fuel cell is a device that converts chemical energy into electrical energy and requires activation after the cell assembly is complete to achieve optimal performance. The traditional activation modes mainly comprise constant-current activation and variable-current forced activation, the activation time is several hours, and meanwhile, the consumption of hydrogen is large, so that the commercial development of the fuel cell is hindered. Therefore, how to improve the activation process of the fuel cell, shorten the activation time, and improve the activation efficiency is one of the important influencing factors for promoting the commercial development of the fuel cell.
Disclosure of Invention
The invention aims to provide a method for quickly activating a membrane electrode of a proton exchange membrane fuel cell, which is simple to operate, can reduce the activation time of the cell and improve the activation efficiency.
The invention adopts the following technical scheme:
the in-situ activation method for membrane electrode of proton exchange membrane fuel cell includes assembling the membrane electrode into single cell, detecting its air tightness, introducing hydrogen and air and making high-low circulation on the output voltage of the cell so as to activate the membrane electrode of proton exchange membrane fuel cell in-situ.
Further, the membrane electrode is prepared by spraying, wherein the slurry used for spraying comprises: the catalyst comprises a catalyst, a solvent and a perfluorinated sulfonic acid resin solution, wherein the solvent is deionized water and low-fat alcohol; optionally a hydrophilic material, a hydrophobic material, a carbon material, a pore former, and/or an anti-stiction catalyst.
Preferably, the catalyst is one or more of Pt/C, PtCo/C, PtNi/C, PtCoMn/C.
Preferably, the low fatty alcohol is one or more of ethanol, isopropanol, n-propanol and ethylene glycol.
Preferably, the hydrophilic material comprises SiO2、Al2O3Crosslinked poly (arylene sulfide)One or more of vinyl alcohol and silicon-aluminum fiber.
Preferably, the hydrophobic material is one or more of FEP, PTFE, PFA, PFPE.
Preferably, the pore-forming agent is one or more of oxalic acid, ammonium bicarbonate, ammonium carbonate and ammonium chloride.
Preferably, the anti-reversal catalyst is IrO2、PtRu/C、PtIr/C、RuO2、RuO2-IrO2、RuO2-TiO2One or more of (a).
Preferably, the carbon material is one or more of carbon nanotube, acetylene black, ketjen black, graphene oxide, graphene, carbon nanohorn, graphite, and activated carbon.
Preferably, the perfluorosulfonic acid resin solution isDE2020、IC100、IC154、D79-25BS、One or more of D83-24 BS.
Further, the output voltage is 0.8-0.9V, 0.5-0.8V and 0.3-0.5V, and the duration of each voltage is 0.5-5 min.
The steps adopted by the invention are as follows:
step 3, testing of a single battery: and assembling the membrane electrode into a single cell, detecting the air tightness of the single cell, respectively introducing air and hydrogen into a cathode and an anode, heating the cell to a certain temperature, adjusting the output voltage to be 0.8-0.9V, 0.5-0.8V and 0.3-0.5V, controlling the duration of each voltage to be 0.5-5 min, and circulating for 2-8 times.
Preferably, in step 1; the weight parts of the pore-forming agent and the carbon material are not 0 at the same time.
Further, in the step 1, the mass ratio of the solvent to the catalyst in the catalyst slurry is (10-100): (0.1-10). The mass ratio of the catalyst to the perfluorinated sulfonic acid resin solution is (0.1-10): (0.1-6). The mass ratio of the hydrophilic material to the catalyst is (0.01-5): (0.1-10). The mass ratio of the hydrophobic material to the catalyst is (0.01-1): (0.1-10). The mass ratio of the carbon material to the catalyst is (0.01-3): (0.1-10). The mass ratio of the pore-forming agent to the catalyst is (0.01-1): (0.1-10). The mass ratio of the antipole catalyst to the catalyst is (0.01-3): (0.1-10).
Further, in the step 2, the anode Pt loading capacity of the membrane electrode is 0.1mg/cm2~0.5mg/cm2The Pt loading capacity of the cathode is 0.01mg/cm2~0.3mg/cm2The drying temperature is 30-90 ℃, and the thickness of the gas diffusion layer is 100-350 μm.
Further, in the step 3, the gas leakage rate of the single cell is 0-0.1 ml/min, the relative humidity of the cathode and the anode is 20-100%, the stoichiometric ratio of hydrogen is 1.0-4.0, the stoichiometric ratio of air is 1.2-4.5, the temperature of the cell is 20-90 ℃, and the reduction range of the output voltage is 0.2-0.4V each time.
Further, in the step 1; the weight parts of the pore-forming agent and the carbon material are not 0 at the same time.
The invention has the beneficial effects that:
the invention provides a method for high-efficiency in-situ activation of a membrane electrode of a proton exchange membrane fuel cell, which effectively removes impurities and larger porosity in a catalyst layer by adding materials such as carbon materials, pore-forming agents and the like in the catalyst layer and combining high and low cycles of output voltage, improves the efficiency of reactants reaching active sites of the catalyst layer and enables the fuel cell to reach an optimal working state in a short time. Meanwhile, the invention carries out activation by a voltage-changing mode, and can avoid the phenomenon that the instantaneous hydrogen supply is insufficient in the process of sudden load pulling of the battery, thereby reducing the possibility of the reverse pole of the battery. The invention has simple process and high activation efficiency, can greatly shorten the activation time of the battery and reduce the production cost.
Drawings
Fig. 1, 2 and 3 are sectional profiles of catalytic layers in examples 1, 2 and 3, respectively, according to the present invention.
Fig. 4, 5 and 6 are surface topography diagrams of the catalytic layers in example 1, example 2 and example 3, respectively, of the present invention.
Fig. 7 is a graph showing the change of the output voltage with time in example 1 of the present invention. The output voltage of the battery is continuously cycled between a low potential and a high potential, and the activation time is only 63min, which is shortened by about 74 percent compared with the activation time of the prior fuel cell.
FIG. 8 is a graph showing the variation of the output voltage with time according to example 2 of the present invention. The output voltage of the battery is continuously cycled between 0.85V, 0.75V and 0.45V, and the activation can be completed in only 60min, which shortens the activation time by about 75 percent compared with the activation time of the existing fuel battery.
FIG. 9 is a graph showing the variation of the output voltage with time according to example 3 of the present invention. The output voltage of the battery continuously cycles between a low potential and a high potential, and the activation is completed only within 77min, so that the activation time is shortened by about 68% compared with that of the conventional fuel cell.
Fig. 10 is a graph comparing polarization curves before and after activation of single cells in examples 1, 2 and 3 of the present invention with non-activated curves. It can be seen in the figure that: the voltage of the activated battery under low current density and high current density is obviously improved, which shows that the method for activating the membrane electrode of the proton exchange membrane fuel cell provided by the invention has obvious effect on activating the fuel cell in a short time.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the proton exchange membrane fuel cell membrane electrode in the embodiment is prepared from the following raw materials: 100mg of catalyst, 3mg of carbon material, 140mg of perfluorinated sulfonic acid resin solution, 10g of solvent and 25cm of proton exchange membrane2Gas diffusion layer 25cm2. Wherein the catalyst is Pt/C (Johnson Matthey, HiSPEC 13100, Pt content is 60 wt%), the carbon material is carbon nano tube (Wolk, multi-wall carbon nano tube, tube diameter is 2-10nm, purity is more than or equal to 95%), and the perfluorinated sulfonic acid resin solution isDE2020 (solids content 25 wt%), the solvent is: deionized water, isopropanol and ethanol, wherein the proton exchange membrane is Kemu NC 700. The gas diffusion layer is Kodbao H24CX483 and has the thickness of 250 mu m.
And 3, assembling the membrane electrode into a single cell, detecting the air tightness of the cell by using high-purity nitrogen with 100kPa, and respectively introducing air and hydrogen with the relative humidity of 100% into a cathode and an anode of the cell, wherein the temperature of the cell is 70 ℃, the stoichiometric ratio of the air is 1.8, and the stoichiometric ratio of the hydrogen is 1.5.
And 4, adjusting the output voltage of the battery to be 0.9V for 1min, 0.7V for 4min and 0.5V for 4min in sequence, circulating for 7 times, and finishing the in-situ activation of the membrane electrode of the proton exchange membrane fuel cell after 63 min.
Table 1 activation parameters set for example 1
Fig. 1 and 4 are respectively a profile view of a cross section and a surface of a catalytic layer of the membrane electrode prepared in embodiment 1 of the present invention, the thickness of a cathode of the catalytic layer is 9 μm, the thickness of an anode of the catalytic layer is 3 μm, and the surface of the catalytic layer is flat and has no cracks.
Fig. 7 is a graph showing the change of the output voltage with time in example 1 of the present invention. The output voltage of the battery continuously circulates between a low potential and a high potential, the activation time is only 63min after the activation is completed, and the activation time is shortened by about 74% compared with the activation time of the existing fuel battery (the activation time of the existing fuel battery is the national standard GB/T20042.5-2009, and the activation time in the 6.6 single battery activation is more than or equal to 4 h).
Example 2:
the proton exchange membrane fuel cell membrane electrode in the embodiment is prepared from the following raw materials: 100mg of catalyst, 5mg of carbon material, 160mg of perfluorinated sulfonic acid resin solution, 10g of solvent and 25cm of proton exchange membrane2. Wherein the catalyst is Pt/C (Pt content 60 wt%, Johnson Matthey, HiSPEC 13100), the carbon material is carbon black (Cabot, Vulcan XC-72), and the perfluorinated sulfonic acid resinThe solution isDE2020 (solids content 25 wt%), the solvent is: deionized water, n-propanol and ethanol. The proton exchange membrane is Kemu NC 700. The gas diffusion layer is Kodbao H24CX483 and has the thickness of 250 mu m.
And 3, assembling the membrane electrode into a single cell, detecting the air tightness of the cell by using high-purity nitrogen with 100kPa, and respectively introducing air and hydrogen with the relative humidity of 100% into a cathode and an anode of the cell, wherein the temperature of the cell is 75 ℃, the stoichiometric ratio of the air is 2.5, and the stoichiometric ratio of the hydrogen is 2.0.
And 4, adjusting the output voltage of the battery to be 0.85V for 1min, 0.75V for 4min and 0.45V for 5min in sequence, and circulating for 6 times, wherein the time is 60min, and the in-situ activation of the membrane electrode of the proton exchange membrane fuel cell is completed.
Table 2 activation parameters set for example 2
Fig. 2 and 5 are respectively a profile view of the cross section and the surface of the catalytic layer of the membrane electrode prepared in embodiment 2 of the present invention, the thickness of the cathode of the catalytic layer is 8 μm, the thickness of the anode of the catalytic layer is 3 μm, and the surface of the catalytic layer is flat and has no cracks.
FIG. 8 is a graph showing the variation of the output voltage with time according to example 2 of the present invention. The output voltage of the cell continuously circulates between 0.85V, 0.75V and 0.45V, the activation can be completed only in 60min, and compared with the activation time of the existing fuel cell (the existing activation time is GB/T20042.5-2009, the activation time in 6.6 single cell activation is more than or equal to 4h), the activation time is shortened by about 75%.
Example 3:
the proton exchange membrane fuel cell membrane electrode in the embodiment is prepared from the following raw materials: 100mg of catalyst, 10mg of pore-forming agent, 112mg of perfluorinated sulfonic acid resin solution, 10g of solvent and 25cm of proton exchange membrane2. Wherein the catalyst is Pt/C (Johnson Matthey, HiSPEC 13100, Pt content 60 wt%) and IrO2(Shanghai Jiping), the pore-forming agent is ammonium carbonate, and the perfluorinated sulfonic acid resin solution isD79-25BS (solid content 25 wt%), and the solvent is: deionized water and isopropanol, wherein the proton exchange membrane is Kemu NC 700. The gas diffusion layer is Kodbao H24CX483 and has the thickness of 250 mu m.
And 3, assembling the membrane electrode into a single cell, detecting the air tightness of the cell by using high-purity nitrogen with 100kPa, and respectively introducing air and hydrogen with the relative humidity of 100% into a cathode and an anode of the cell, wherein the temperature of the cell is 80 ℃, the stoichiometric ratio of the air is 2.0, and the stoichiometric ratio of the hydrogen is 1.8.
And 4, adjusting the output voltage of the battery to be 0.85V for 2min, 0.65V for 4min and 0.5V for 5min in sequence, circulating for 7 times, and consuming for 77min to finish the in-situ activation of the membrane electrode of the proton exchange membrane fuel cell.
Table 3 activation parameters set for example 3
Fig. 3 and 6 are respectively a profile view of the cross section and the surface of the catalytic layer of the membrane electrode prepared in embodiment 3 of the present invention, the thickness of the cathode of the catalytic layer is 9 μm, the thickness of the anode of the catalytic layer is 3 μm, and the surface of the catalytic layer is flat and has holes left after the pore-forming agent is volatilized.
FIG. 9 is a graph showing the variation of the output voltage with time according to example 3 of the present invention. The output voltage of the battery continuously cycles between a low potential and a high potential, and the activation is completed only within 77min, so that the activation time is shortened by about 68% compared with that of the conventional fuel cell.
Fig. 10 is a graph comparing polarization curves before and after activation of single cells in examples 1, 2 and 3 of the present invention with non-activated curves. It can be seen in the figure that: the voltage of the activated battery under low current density and high current density is obviously improved, which shows that the method for activating the membrane electrode of the proton exchange membrane fuel cell provided by the invention has obvious effect on activating the fuel cell in a short time.
The invention has not been described in detail and is part of the common general knowledge of a person skilled in the art. The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and the preferred embodiments are not exhaustive and do not limit the invention to the precise embodiments described. Various modifications and improvements of the technical solution of the present invention may be made by those skilled in the art without departing from the spirit of the present invention, and the technical solution of the present invention is to be covered by the protection scope defined by the claims.
Claims (8)
1. A method for high-efficiency in-situ activation of a membrane electrode of a proton exchange membrane fuel cell is characterized by comprising the following steps: the in-situ activation method is to assemble the membrane electrode into a single cell, detect the air tightness of the single cell, then introduce hydrogen and air and carry out high-low circulation on the output voltage of the cell so as to achieve the purpose of in-situ activation of the membrane electrode of the proton exchange membrane fuel cell.
2. The method of in situ activating a pem fuel cell membrane electrode of claim 1 wherein: the membrane electrode is prepared by spraying, and slurry used by spraying comprises:
the catalyst comprises a catalyst, a solvent and a perfluorinated sulfonic acid resin solution, wherein the solvent is deionized water and low-fat alcohol;
optionally a hydrophilic material, a hydrophobic material, a carbon material, a pore former and/or an anti-stiction catalyst;
preferably, the catalyst is one or more of Pt/C, PtCo/C, PtNi/C, PtCoMn/C;
preferably, the low fatty alcohol is one or more of ethanol, isopropanol, n-propanol and ethylene glycol;
preferably, the hydrophilic material comprises SiO2、Al2O3One or more of cross-linked polyvinyl alcohol and silicon-aluminum fiber;
preferably, the hydrophobic material is one or more of FEP, PTFE, PFA, PFPE;
preferably, the pore-forming agent is one or more of oxalic acid, ammonium bicarbonate, ammonium carbonate and ammonium chloride;
preferably, the anti-reversal catalyst is IrO2、PtRu/C、PtIr/C、RuO2、RuO2-IrO2、RuO2-TiO2One or more of;
preferably, the carbon material is one or more of carbon nanotube, acetylene black, ketjen black, graphene oxide, graphene, carbon nanohorn, graphite, and activated carbon;
3. The method of in situ activating a pem fuel cell membrane electrode of claim 1 wherein: the output voltage is 0.8-0.9V, 0.5-0.8V and 0.3-0.5V, and the duration of each voltage is 0.5-5 min.
4. A method for high efficiency in situ activation of a pem fuel cell membrane electrode according to any of claims 1-3 comprising the steps of:
step 1, preparation of catalyst slurry: mixing, dispersing and uniformly dispersing 1-100 parts by weight of a solvent, 0.1-10 parts by weight of a catalyst, 0.1-10 parts by weight of a perfluorosulfonic acid resin solution, 0-3 parts by weight of a hydrophilic material, 0-3 parts by weight of a hydrophobic material, 0-5 parts by weight of a pore-forming agent, 0-1 part by weight of an anti-reversal catalyst and 0-5 parts by weight of a carbon material, wherein the solid content of the obtained dispersion liquid is 0.1-15 wt%;
step 2, preparing a membrane electrode: uniformly spraying the catalyst slurry to two sides of a proton exchange membrane, drying the membrane electrode, and covering a gas diffusion layer to obtain a membrane electrode assembly;
step 3, testing of a single battery: and assembling the membrane electrode into a single cell, detecting the air tightness of the single cell, introducing air and hydrogen into a cathode and an anode respectively, heating the cell, adjusting the output voltage to be 0.8-0.9V, 0.5-0.8V and 0.3-0.5V, keeping the duration of each voltage to be 0.5-5 min, and circulating for 2-8 times.
5. The method for efficient in-situ activation of pem fuel cell membrane electrode of claim 4 wherein: the mass ratio of the solvent to the catalyst in the catalyst slurry is (10-100): (0.1-10), wherein the mass ratio of the catalyst to the perfluorinated sulfonic acid resin solution is (0.1-10): (0.1-6); preferably, the mass ratio of the hydrophilic material to the catalyst is (0.01-5): (0.1 to 10); preferably, the mass ratio of the hydrophobic material to the catalyst is (0.01-1): (0.1 to 10); preferably, the mass ratio of the carbon material to the catalyst is (0.01-3): (0.1 to 10); preferably, the mass ratio of the pore-forming agent to the catalyst is (0.01-1): (0.1 to 10); preferably, the mass ratio of the antipole catalyst to the catalyst is (0.01-3): (0.1-10).
6. The method of in situ activating a pem fuel cell membrane electrode of claim 4 wherein: the anode Pt loading capacity of the membrane electrode is 0.1mg/cm2~0.5mg/cm2The Pt loading capacity of the cathode is 0.01mg/cm2~0.3mg/cm2The drying temperature is 30-90 ℃, and the thickness of the gas diffusion layer is 100-350 μm.
7. The method of in situ activating a pem fuel cell membrane electrode of claim 4 wherein: the gas leakage rate of the single cell is 0-0.1 ml/min, the relative humidity of the cathode and the anode is 20-100%, the stoichiometric ratio of hydrogen is 1.0-4.0, the stoichiometric ratio of air is 1.2-4.5, the temperature of the cell is 20-90 ℃, and the reduction range of the output voltage is 0.1-0.4V each time.
8. The method of in situ activating a pem fuel cell membrane electrode of claim 4 wherein: in the step 1; the weight parts of the pore-forming agent and the carbon material are not 0 at the same time.
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CN114361472A (en) * | 2022-01-10 | 2022-04-15 | 合肥工业大学 | Preparation method of high-activity/anti-reversal-pole catalyst for proton exchange membrane fuel cell |
CN116759590A (en) * | 2023-08-17 | 2023-09-15 | 安徽明天新能源科技有限公司 | Preparation method of composite CCM with high durability and low activation time and different catalytic layers |
CN116759590B (en) * | 2023-08-17 | 2023-10-31 | 安徽明天新能源科技有限公司 | Preparation method of multi-layer catalytic layer structure CCM |
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