CN111740139B - Ion exchange-free alkaline polymer electrolyte fuel cell membrane electrode and preparation method thereof - Google Patents

Ion exchange-free alkaline polymer electrolyte fuel cell membrane electrode and preparation method thereof Download PDF

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CN111740139B
CN111740139B CN202010565123.5A CN202010565123A CN111740139B CN 111740139 B CN111740139 B CN 111740139B CN 202010565123 A CN202010565123 A CN 202010565123A CN 111740139 B CN111740139 B CN 111740139B
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polymer electrolyte
alkaline polymer
fuel cell
membrane electrode
catalyst layer
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CN111740139A (en
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庄林
李启浩
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Wuhan University WHU
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
    • 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
    • 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
    • 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
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Sustainable Energy (AREA)
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Abstract

The invention discloses an ion exchange-free alkaline polymer electrolyte fuel cell membrane electrode and a preparation method thereof. The membrane electrode comprises an anode catalyst layer, a membrane and a cathode catalyst layer, and an anionic alkaline polymer electrolyte membrane and solution which can directly participate in the anode reaction of the fuel cell are prepared through pre-ion exchange; then the polymer electrolyte solution and a fuel cell catalyst are used together to prepare catalyst layer precursor ink, and the membrane electrode of the alkaline polymer electrolyte fuel cell free of ion exchange is further prepared. The membrane electrode prepared by the invention is characterized in that the membrane electrode can be assembled and operated without ion exchange, the assembly process is simplified, the size change caused by the ion exchange is eliminated, and the mechanical strength of the membrane electrode is enhanced, so that the stability of the membrane electrode is improved; can promote the scale preparation and application of the alkaline polymer electrolyte fuel cell and the galvanic pile.

Description

Alkaline polymer electrolyte fuel cell membrane electrode free of ion exchange and preparation method thereof
Technical Field
The invention belongs to the field of fuel cells, relates to a preparation method of a membrane electrode, and particularly relates to an ion exchange-free alkaline polymer electrolyte fuel cell membrane electrode and a preparation method thereof. The invention prepares the alkaline polymer electrolyte fuel cell or the electric pile which can be directly assembled without ion exchange by carrying out pre-ion exchange on the alkaline polymer electrolyte.
Background
The Alkaline Polymer Electrolyte Fuel Cell (APEFC) has the advantages of high energy efficiency, quiet, clean and no pollution, and the alkaline working environment thereof makes the use of non-noble catalysts possible, so that the manufacturing cost of the fuel cell can be greatly reduced, thereby drawing extensive attention and research.
In alkaline polymer electrolyte fuel cells, an Alkaline Polyelectrolyte (APE) membrane is required to serve as a barrier to gas transport from the cathode and anode and ion transport, and a catalytic layer is also required to conduct ions.
The synthesis of alkaline polymer electrolyte generally adopts S N2 nucleophilic attack to fix the cation to the polymer chain, the counter ion of the cation fixed to the polymer chain is generally chloride (Cl) in the synthesized basic polymer electrolyte-) Bromine ion (Br)-) Iodide ion (I)-) Plasma halide or Sulfate (SO)4 2-) Hexafluorophosphate radical (PF)6 -) And (3) plasma. All anions can not participate in the anode reaction of the fuel cell, so that the synthesized alkaline polymer electrolyte can not directly operate after being prepared into a membrane electrode, and needs to be addedIon exchange is carried out step by step, and the ions are exchanged into anions (hydroxyl (OH) which can participate in the anode reaction of the fuel cell-) Carbonate (CO)3 2-) Bicarbonate radical (HCO)3 -) ) can only be operated thereafter, which increases the complexity of the battery assembly. Meanwhile, the ion exchange process of the membrane electrode can cause swelling of about 5% to 10%, the assembly of the fuel cell and the electric stack needs to accurately control the size of the membrane electrode, and the size change caused by the ion exchange makes the assembly of the alkaline polymer electrolyte fuel cell and the electric stack difficult, which limits the large-scale preparation and application of the alkaline polymer electrolyte fuel cell. Therefore, the preparation technology of the alkaline polymer electrolyte fuel cell membrane electrode free of ion exchange can simplify the assembly of the alkaline polymer electrolyte fuel cell, eliminate the size change caused by the ion exchange of the membrane electrode and promote the large-scale preparation and application of the alkaline polymer electrolyte fuel cell.
Disclosure of Invention
The invention aims to provide a preparation method of an alkaline polymer electrolyte fuel cell membrane electrode free of ion exchange. The invention prepares the counter ion of hydroxyl (OH) through pre-ion exchange-) Carbonate (CO)3 2-) Bicarbonate radical (HCO)3 -) And the alkaline polymer electrolyte membrane and the solution of anions (the reaction formula is shown in figure 2) which can participate in the anode reaction of the fuel cell, and further the membrane electrode of the alkaline polymer electrolyte fuel cell which can be assembled and operated without ion exchange is prepared.
In order to achieve the purpose, the invention adopts the scheme that:
an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode, characterized in that: comprises an anode catalytic layer, a membrane and a cathode catalytic layer.
The anode catalyst layer and the cathode catalyst layer are both composed of corresponding catalysts and alkaline polymer electrolytes, wherein counter ions of the alkaline polyelectrolytes are anions (hydroxyl (OH) capable of participating in the anode reaction of the fuel cell-) Carbonate (CO)3 2-) Bicarbonate radical (HCO)3 -) One or a different ratio ofA plurality of examples);
the membrane is an alkaline polymer electrolyte membrane with micron-sized thickness, which is anionic (hydroxyl (OH) capable of participating in anode reaction of fuel cell-) Carbonate (CO)3 2-) Bicarbonate radical (HCO)3 -) Any one of them or a plurality of them in different proportions).
The preparation steps of the membrane electrode of the alkaline polymer electrolyte fuel cell free of ion exchange are as follows:
step 1, soaking alkaline polymer electrolyte solid, the counter ions of which are negative ions which cannot participate in the anode reaction, in a salt solution with a certain concentration for a period of time at a certain temperature, exchanging the counter ions of the alkaline polymer electrolyte, separating the alkaline polymer electrolyte solid, washing away redundant salt with purified water, and drying to obtain the alkaline polymer electrolyte solid, the counter ions of which are negative ions which can participate in the anode reaction of the fuel cell; the salt solution is a salt solution containing anions which can participate in the anode reaction of the fuel cell;
step 2, dissolving the alkaline polymer electrolyte solid subjected to ion exchange in the step 1 in a solvent to obtain an alkaline polymer electrolyte solution with known concentration;
step 3, preparing an alkaline polymer electrolyte membrane, namely taking a piece of alkaline polymer electrolyte membrane to perform ion exchange according to the method in the step 1 to obtain the alkaline polymer electrolyte membrane of which the counter ions are anions capable of participating in the anode reaction of the fuel cell;
or adopting the alkaline polymer electrolyte solution obtained in the step 2 to obtain an alkaline polymer electrolyte membrane of which the counter ions are anions capable of participating in the anode reaction of the fuel cell by adopting a membrane forming process; the method comprises the following specific steps:
A. soaking an alkaline polymer electrolyte membrane, the counter ion of which is an anion that cannot participate in the anode reaction of the fuel cell, in a salt solution with a certain concentration, wherein the salt is hydroxide (OH)-) Or Carbonate (CO)3 2-) Or bicarbonate radical (HCO)3 -) The solvent is water. Soaking at a certain temperatureAnd (3) completely exchanging the counter ions of the alkaline polymer electrolyte membrane for a period of time, taking out the membrane, washing off redundant salt by using purified water, and drying to obtain the alkaline polymer electrolyte membrane with the counter ions capable of participating in the reaction of the fuel cell.
And B, taking a certain amount of the alkaline polymer electrolyte solution prepared in the step 2, and preparing the alkaline polymer electrolyte membrane which can participate in the reaction of the fuel cell for ions by using a drying film forming method, a blade coating film forming method or a tape casting film forming method. The thickness of the prepared alkaline polymer electrolyte membrane can be controlled by controlling the concentration of the alkaline polymer electrolyte solution prepared in step 2 or the amount of the alkaline polymer electrolyte solution added.
Step 4, weighing a certain amount of fuel cell catalyst, adding the alkaline polymer electrolyte solution obtained in the step 2, dispersing the alkaline polymer electrolyte solution into a solvent to obtain catalyst layer precursor ink, and respectively preparing cathode catalyst layer precursor ink and anode catalyst layer precursor ink according to the method;
and 5, respectively preparing the precursor ink of the cathode catalyst layer and the precursor ink of the anode catalyst layer on two sides of the alkaline polymer electrolyte membrane obtained in the step 3 by adopting a fuel cell catalyst layer preparation process to form the cathode catalyst layer and the anode catalyst layer, and finishing the preparation of the membrane electrode of the alkaline polymer electrolyte fuel cell.
Preferably, in step 1, the salt of the salt solution is a water-soluble salt with an anion selected from one or a combination of hydroxide, carbonate and bicarbonate.
Preferably, in step 1, the alkaline polymer electrolyte solid is a powder solid.
Preferably, in the step 1, the soaking temperature is 20-100 ℃, and the soaking time is 1-72 hours.
Preferably, in step 2, the concentration of the alkaline polymer electrolyte solution is in the range of 2 to 500 mg/mL.
Preferably, in step 2, the solvent is any one or a mixture of several of dimethyl sulfoxide, dimethylformamide, tetrahydrofuran, 2-pyrrolidone, n-propanol, isopropanol, ethanol and water.
Preferably, in step 3, the film forming process is any one of drying film forming, blade coating film forming and casting film forming.
Preferably, in step 4, the fuel cell catalyst is one or more of Pt, Ru, Pd, Ir, Rh, Os, Ni, Mo, Co, Mn, W, V, or an oxide or nitride thereof.
Preferably, in step 4, the process for preparing the cathode catalytic layer and the anode catalytic layer is any one of spraying, blade coating, brushing and printing.
The prepared membrane electrode of the alkaline polymer electrolyte fuel cell free of ion exchange can be directly added with gas diffusion layers on two sides for cell assembly operation; or adding gas diffusion layers on two sides for hot pressing to form an integrated membrane electrode and then assembling for operation.
Compared with the prior art for preparing the membrane electrode of the alkaline polymer electrolyte fuel cell, the invention has the following advantages:
the invention prepares the alkaline polymer electrolyte fuel cell membrane electrode without ion exchange through pre-ion exchange, simplifies the assembly process of the alkaline polymer electrolyte fuel cell, eliminates the size change caused by the ion exchange of the alkaline polymer electrolyte fuel cell membrane electrode, enhances the mechanical strength of the alkaline polymer electrolyte fuel cell membrane electrode and increases the stability thereof; can promote the scale preparation and application of the alkaline polymer electrolyte fuel cell and the galvanic pile.
Drawings
FIG. 1 is a schematic view of the membrane electrode structure of the present invention;
wherein 1 is an anode catalyst layer, 2 is a polyelectrolyte membrane, and 3 is a cathode catalyst layer.
FIG. 2 is a reaction scheme in which anions that may participate in the anode reaction of a fuel cell participate in the anode reaction;
wherein 1.1 is hydroxyl (OH)-) A reaction formula participating in an anode reaction; 1.2 is Carbonate (CO)3 2-) A reaction formula participating in an anode reaction; 1.3 is bicarbonate radical (HCO)3 -) And (3) reaction formula participating in anode reaction.
FIG. 3 is a graph showing cell performance curves under the membrane electrode assembly manufacturing method and cell operating conditions for an alkaline polymer electrolyte fuel cell according to example 1 of the present invention.
FIG. 4 is a graph showing cell performance curves under the membrane electrode assembly manufacturing method and cell operating conditions for an alkaline polymer electrolyte fuel cell according to example 2 of the present invention.
FIG. 5 is a graph showing cell performance curves under the membrane electrode assembly manufacturing method and cell operating conditions for an alkaline polymer electrolyte fuel cell according to example 3 of the present invention.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The invention is further illustrated by the following specific examples, which are intended to facilitate a better understanding of the contents of the invention, but which are not intended to limit the scope of the invention in any way.
Example 1
The structure of the membrane electrode of the ion exchange-free alkaline polymer electrolyte fuel cell is shown in fig. 1, and the membrane electrode sequentially comprises an anode catalyst layer 1, a polyelectrolyte membrane 2 and a cathode catalyst layer 3 from left to right.
The membrane electrode of the alkaline polymer electrolyte fuel cell free of ion exchange is prepared by adopting the following process:
200mg of alkaline polymer electrolyte powder of quaternized polyarylpiperidine copolymer (QAPT, purchased from Yiwei Co., Ltd.) was weighed, 50mL of 1mol/L KOH solution was added, and the mixture was soaked at 60 ℃ for 5 hours to completely exchange counter ions for hydroxyl (OH)-). Then, QAPT powder was separated by centrifugation, and then washed 5 times with purified water to remove excess alkali. Finally drying to Obtain Hydroxyl (OH) as counter ion-) The alkaline polymer electrolyte powder (QAPT powder) of (1).
The QAPT powder was dissolved in 10mL of dimethyl sulfoxide (DMSO) to obtain a 20mg/mL concentration of hydroxide (OH) as the counter ion-) QAPPT solution of (1).
Taking a piece of QA with the area of 5cm multiplied by 5cm and the thickness of 25 micrometersPPT membrane, adding 50mL of 1mol/L KOH solution, soaking at 60 deg.C for 5 hr to completely exchange counter ions into hydroxide (OH)-). The membrane was removed and washed under flowing purified water for 3 minutes to clean the caustic soda. Drying to Obtain Hydroxyl (OH) ion-) The QAPT film of (1).
6mg of a 60% commercial Pt/C catalyst was weighed and 75. mu.l of 20mg/mL of counter ion as hydroxide (OH)-) 2mL of isopropanol was added to the QAPT solution. Uniformly dispersing the precursor solution by ultrasonic for 1 hour, and uniformly dividing the precursor solution into anode and cathode catalyst precursor ink respectively.
Respectively ultrasonically spraying the anode catalyst precursor ink and the cathode catalyst precursor ink on prepared counter ions of hydroxyl (OH)-) Respectively obtaining an anode catalyst layer 1 and a cathode catalyst layer 3 at two sides of the QAPT membrane, wherein the middle QAPT membrane is a polyelectrolyte membrane 2, the catalysts at the anode and the cathode are Pt/C, and the loading capacity of Pt is 0.4mg/cm2. Obtaining the alkaline polymer electrolyte membrane electrode free from ion exchange.
The ion-exchange-free alkaline polymer electrolyte membrane electrode is clamped between gas diffusion layers and assembled into a single cell for testing, and the cell operating conditions are as follows:
hydrogen with the flow rate of 500mL/min is introduced into the anode, and oxygen with the flow rate of 500mL/min is introduced into the cathode; the back pressures of the cathode and the anode are both 0.2 MPa; the cell operating temperature was 80 ℃. After the battery is activated for 12 hours at a constant voltage of 0.5V, a performance test is carried out, the polarization curve and the power density curve of the battery are shown in figure 3, and the maximum current density of the battery can reach 2A/cm2The maximum power density can reach 0.6W/cm2。
Example 2
The difference from example 1 is that the counter ion is hydroxyl (OH)-) The preparation method of the QAPT film comprises the following steps:
10g of QAPT powder was taken, 500mL of 1mol/L KOH solution was added, and the mixture was soaked at 60 ℃ for 5 hours to completely exchange the counter ion into hydroxide (OH)-). Then, QAPT powder was separated by centrifugation, and then washed 5 times with purified water to remove excess caustic soda. Finally drying to Obtain Hydroxyl (OH) as counter ion-) QAP of (2)PT powder.
Making the counter ion into hydroxyl (OH)-) The QAPT powder of (2) was dissolved in 40mL of dimethyl sulfoxide (DMSO) to obtain a concentration of 250mg/mL of hydroxide (OH) as the counter ion-) The QAPT concentrated solution is prepared into hydroxide (OH) ion by using a casting method-) A QAPT film of thickness 20 microns.
The other preparation and test methods are the same as those of example 1, the polarization curve and power density curve of the cell are shown in FIG. 4, and the maximum current density can reach 2A/cm2The maximum power density can reach 0.7W/cm2。
Example 3
The difference from example 2 is that the anode catalyst used 60% of commercial PtRu/C catalyst, the metal loading was again 0.4mg/cm2The other preparation and test methods are the same as those of example 1, the polarization curve and power density curve of the cell are shown in FIG. 5, and the maximum current density can reach 2.8A/cm2The maximum power density can reach 1.1W/cm2。
The above embodiments are merely illustrative of the present invention and are not to be construed as limiting the invention. Although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that various combinations, modifications or equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, and the technical solution of the present invention is covered by the claims of the present invention.

Claims (9)

1. A preparation method of an ion exchange-free alkaline polymer electrolyte fuel cell membrane electrode is characterized by comprising the following steps:
step 1, soaking an alkaline polymer electrolyte solid, the counter ions of which are anions which cannot participate in an anode reaction, in a salt solution with a certain concentration, soaking for a period of time at a certain temperature, exchanging the counter ions of the alkaline polymer electrolyte, separating the alkaline polymer electrolyte solid, washing off redundant salts with purified water, and drying to obtain the alkaline polymer electrolyte solid, the counter ions of which are anions which can participate in the anode reaction of the fuel cell; the salt solution is a salt solution containing anions which can participate in the anode reaction of the fuel cell;
step 2, dissolving the alkaline polymer electrolyte solid subjected to ion exchange in the step 1 in a solvent to obtain an alkaline polymer electrolyte solution with known concentration;
step 3, preparing an alkaline polymer electrolyte membrane, namely obtaining the alkaline polymer electrolyte membrane with the counter ions which can participate in the anode reaction of the fuel cell by adopting the alkaline polymer electrolyte solution obtained in the step 2 and adopting a membrane forming process;
step 4, weighing a certain amount of fuel cell catalyst, adding the alkaline polymer electrolyte solution obtained in the step 2, dispersing the alkaline polymer electrolyte solution into a solvent to obtain catalyst layer precursor ink, and respectively preparing cathode catalyst layer precursor ink and anode catalyst layer precursor ink;
and 5, respectively preparing the precursor ink of the cathode catalyst layer and the precursor ink of the anode catalyst layer on two sides of the alkaline polymer electrolyte membrane obtained in the step 3 by adopting a fuel cell catalyst layer preparation process to form the cathode catalyst layer and the anode catalyst layer, and finishing the preparation of the membrane electrode of the alkaline polymer electrolyte fuel cell.
2. The method for preparing an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode assembly according to claim 1, wherein: in the step 1, the salt of the salt solution is a water-soluble salt with an anion of any one or a combination of more of hydroxide, carbonate and bicarbonate.
3. The method for preparing an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode assembly according to claim 1, wherein: in step 1, the alkaline polymer electrolyte solid is a powder solid.
4. The method for preparing an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode assembly according to claim 1, wherein: in step 1, the soaking temperature is 20-100 DEG CoC, soaking time is 1-72 hours.
5. The method for preparing an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode assembly according to claim 1, wherein: in step 2, the concentration of the alkaline polymer electrolyte solution is in the range of 2-500 mg/mL.
6. The method for preparing an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode assembly according to claim 1, wherein: in the step 2, the solvent is any one or a mixture of dimethyl sulfoxide, dimethylformamide, tetrahydrofuran, 2-pyrrolidone, n-propanol, isopropanol, ethanol and water.
7. The method for preparing an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode assembly according to claim 1, wherein: in the step 3, the film forming process is any one of drying film forming, blade coating film forming and curtain coating film forming.
8. The method for preparing an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode assembly according to claim 1, wherein: in step 4, the fuel cell catalyst is one or more of Pt, Ru, Pd, Ir, Rh, Os, Ni, Mo, Co, Mn, W, V, or their oxides or nitrides.
9. The method for preparing an ion-exchange-free alkaline polymer electrolyte fuel cell membrane electrode assembly according to claim 1, wherein: in the step 4, the process for preparing the cathode catalyst layer and the anode catalyst layer is any one of spraying, blade coating, brush coating and printing.
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