CN105024084A - High-temperature proton exchange membrane fuel cell membrane electrode and preparation method thereof - Google Patents
High-temperature proton exchange membrane fuel cell membrane electrode and preparation method thereof Download PDFInfo
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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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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
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- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8673—Electrically conductive fillers
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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
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
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Abstract
The invention discloses a high-temperature proton exchange membrane fuel cell membrane electrode and a preparation method thereof. The membrane electrode is composed of an anode diffusion layer, an anode catalysis layer, a proton exchange membrane, a cathode catalysis layer and a cathode diffusion layer, wherein the anode catalysis layer and the cathode catalysis layer are each formed by mixing graphene aerogel, PTFE and catalyst. The graphene aerogel is a low-density solid material and has high specific surface area, rich nano-porous structure, high conductivity and hydrophobic property. Due to the catalysis layers with the graphene aerogel phosphoric acid molecules in the proton exchange membrane can be effectively restrained from being adsorbed by the surfaces of the catalysis layers, phosphoric acid is prevented from loss, and the service life of the proton exchange membrane is prolonged; meanwhile, due to the high conductivity of the graphene aerogel, the ohmic resistance of the membrane electrode can be reduced, and therefore the output power of a high-temperature proton exchange membrane fuel cell is improved.
Description
Technical field
The invention belongs to Proton Exchange Membrane Fuel Cells field, relate to a kind of structure and preparation method of high-temperature fuel cell membrane electrode.
Background technology
The energy is the power of economic development, is the material base that the mankind depend on for existence.Fuel cell has become one of most potential technology of following clean energy resource industry due to advantages such as the high and low discharges of its energy conversion rate, will be widely used in the fields such as space flight, military affairs, communication and traffic.
High temperature proton exchange film fuel cell is the new proton exchange film fuel battery technology of development in recent years, and its working temperature is more than 100 DEG C.Current modal high temperature proton exchange film fuel cell adopts PBI/H
3pO
4film, PBI/H
3pO
4film, using phosphoric acid as carrier conduction proton, so do not need hydration reaction not need humidification, simplifies the gas handling system of fuel cell.Its working temperature is at 120 DEG C-180 DEG C, and reaction generates vaporous water, can discharge easily, simplify fuel cell water management system with cathode flame.The raising of working temperature can improve the tolerance of high-temperature fuel cell to CO and S.Widely different due to working temperature and ambient temperature, reaction liberated heat can be more effectively utilized, and heat management system is simplified; Simultaneously along with the raising of reaction temperature, the speed of electrochemical reaction also improves thereupon.But the useful life of high temperature proton exchange film fuel cell is not long, on the one hand in the use procedure of battery because the cohesion of catalyst, the loss of phosphoric acid cause the decay of proton exchange film properties, may occur that in the course of work of charged pool the phenomenon of local overheating causes membrane damage on the other hand.
Summary of the invention
The object of this invention is to provide membrane electrode of a kind of high temperature proton exchange film fuel cell and preparation method thereof, wherein Catalytic Layer is by graphene aerogel and PTFE and Pt is catalyst based is mixed.Graphene aerogel is a kind of low density solid material, has high-specific surface area, abundant nano-pore structure, good conductivity and hydrophobic character.Catalytic Layer containing graphene aerogel can effectively to suppress in proton exchange membrane phosphoric acid molecules in the absorption on Catalytic Layer surface, avoid the loss of phosphoric acid, improve the life-span of proton exchange membrane, its good conductivity can reduce the Ohmic resistance of membrane electrode simultaneously, thus improves the power output of high temperature proton exchange film fuel cell.
Described object is realized by following scheme:
A kind of high temperature proton exchange film fuel cell membrane electrode, is made up of anode diffusion layer, anode catalyst layer, proton exchange membrane, cathode catalysis layer, cathode diffusion layer.Wherein said anode and cathode catalysis layer be by graphene aerogel, PTFE and Pt is catalyst based is mixed.
A preparation method for above-mentioned high temperature proton exchange film fuel cell membrane electrode, with carbon paper or carbon cloth for supporting layer, the then diffusion layer of carbon coating material and PTFE composition, more repeatedly coated cathode, Anode inks, then heat treatment is pressed into membrane electrode.Concrete steps are as follows:
1, the preparation process of negative electrode and anode diffusion layer:
Material with carbon element, PTFE emulsion and isopropanol water solution are mixed, supersonic oscillations, magnetic agitation, form uniform slurry, and wherein PTFE accounts for the 40-60% of solid gross mass.By the mode brushed or spray, slurry is coated onto on carbon paper or carbon cloth, dries roasting, can diffusion layer be obtained.Wherein, the carrying capacity of diffusion layer is 2-7mg. cm
-2.
2, the preparation process of anode catalyst layer:
Directly obtain graphene aerogel by graphite oxide aqueous dispersions by hydro thermal method, then obtained graphene aerogel is ground to form nano particle.
Get a certain amount of PtRu/C catalyst, wherein Pt, Ru atomic ratio is 1:1-1:2, PtRu accounts for the 60-90% of total catalyst weight, mix with pure water, sonic oscillation, then appropriate graphene aerogel nano particle and a small amount of PTFE solution is added, add appropriate aqueous isopropanol again, controlling graphene aerogel and the total weight of PTFE and the mass ratio of PtRu/C catalyst is 1/4-1/10, the mass ratio of graphene aerogel and PTFE is 2:1-10:1, and supersonic oscillations, magnetic agitation are to forming uniform Anode inks;
The mode of being brushed by Anode inks or spray evenly is coated onto on anode diffusion layer, and just obtain anode catalyst layer after oven dry, anode catalyst layer Pt carrying capacity is 1-4mg/ cm
2.
3, the preparation process of cathode catalysis layer:
Weigh a certain amount of Pt/C catalyst, wherein Pt accounts for the 35%-85% of total catalyst weight, add the mixing of appropriate ultra-pure water, sonic oscillation, then graphene aerogel, PTFE solution and appropriate isopropyl alcohol is added, wherein the mass ratio of graphene aerogel and PTFE gross mass and Pt/C mixture is 1/4-1/10, and the mass ratio of graphene aerogel and PTFE is 2:1-10:1, and supersonic oscillations, magnetic agitation are to forming uniform cathode inks;
Brushed by cathode inks or spray to cathode diffusion layer on the surface, oven dry can obtain cathode catalysis layer, and cathode catalysis layer Pt carrying capacity is 3-6mg/ cm
2.
4, the processing procedure of proton exchange membrane:
Cut out the PBI film of suitable size, be immersed under room temperature concentration be in the phosphoric acid solution of 85% continue three days, period repeatedly agitating solution PBI film is fully contacted with phosphoric acid solution.Then taken out, blotted fast with the phosphoric acid solution of filter paper by film surface, then to be put it in vacuum drying chamber dry 10h at 110 DEG C.
5, membrane electrode hot pressing:
According to the order of anode diffusion layer, anode catalyst layer, proton exchange membrane, cathode catalysis layer, cathode diffusion layer, it is put, with hot press at 100-200 kg.cm
-2pressure under, hot pressing 3-8min, the i.e. membrane electrode of obtained high temperature proton exchange film fuel cell at the temperature of 135 DEG C.
The present invention mainly considers the problem that the conductivity of high temperature proton exchange film fuel cell membrane electrode and the PBI proton exchange membrane phosphoric acid of phosphorylation run off.Because H
+be transported by phosphate radical anion moving in film, the loss of phosphoric acid can cause the decline of film properties, thus affects the performance of battery.In order to avoid the loss of phosphoric acid, in the slurry preparation process of cathode and anode catalyst, add graphene aerogel, because it has hydrophobicity, the loss of phosphoric acid molecules with moisture content can be reduced, prevent phosphate radical anion from adsorbing at catalyst surface.Graphene aerogel has good conductivity in addition, and its Conductivity Ratio tradition is only added, and membrane electrode that PTFE makees Catalytic Layer binding agent obtains effective raising.The porosity of graphene aerogel can change by controlling manufacture craft in addition, can be found by the porosity changing graphene aerogel and make the optimal value that electrode effective surface area becomes large, phosphoric acid runs off reduction, also have positive role to the performance improving battery.
Accompanying drawing explanation
fig. 1 is the structural representation that Catalytic Layer contains the high temperature proton exchange film fuel cell membrane electrode of graphene aerogel.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is described further; but be not limited to this; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
As shown in Figure 1, high temperature proton exchange film fuel cell membrane electrode provided by the invention is made up of anode diffusion layer 1, anode catalyst layer 2, proton exchange membrane 3, cathode catalysis layer 4, cathode diffusion layer 5.Wherein anode catalyst layer 2 and cathode catalysis layer 4 be by graphene aerogel, PTFE and Pt is catalyst based is mixed.
The preparation process of high temperature proton exchange film fuel cell membrane electrode comprises negative electrode and anode diffusion layer preparation, negative electrode and anode catalyst layer preparation, the phosphorylation of PBI film, and hot pressing becomes membrane electrode, and concrete steps are as follows:
The preparation of step one, cathode diffusion layer and anode diffusion layer:
Take PTFE (polytetrafluoroethylene) emulsion that 10mg carbon dust XC-72R and 60mg mass percent concentration are 15%, be scattered in 2ml isopropanol water solution (the volume ratio 1:1 of isopropyl alcohol and water), sonic oscillation 30min, then magnetic agitation 30min the slurry that mixes.
Adopt the mode of brushing through being repeatedly coated on the carbon paper of 1cm × 1cm in slurry, until weightening finish reaches 4mg.Then at the temperature of 120 DEG C, dry 30min, the surfactant in isopropyl alcohol and water and PTFE emulsion is volatilized completely, under the high temperature of 350 DEG C, process 30min afterwards, make PTFE be melt into network configuration, obtain cathode diffusion layer and anode diffusion layer.
The preparation of step 2, anode catalyst layer:
Graphene oxide powder and deionized water being made into concentration is the 1-10mg/ml aqueous solution, and ultrasonic vibration 1-5 is little of obtaining finely disseminated graphene oxide water solution; The graphene oxide water solution configured is got 10-500ml to add in water heating kettle, add L-AA again, wherein the mass ratio of L-AA and graphene oxide is 2:1,12 hours are processed at 100-200 DEG C of temperature, obtain Graphene hydrogel, then put it in freeze dryer and obtain graphene aerogel after freeze drying, be then ground into nano particle.
Take 16mg catalyst 40%Pt20%Ru/40%C(mass ratio) and the mixing of 1.5ml pure water, sonic oscillation 10min, then PTFE solution and 2ml isopropyl alcohol that 2mg graphene aerogel and 10mg mass percent concentration are 5% is added, sonic oscillation 30min, then magnetic agitation 30min, obtains Anode inks.
Adopting the mode of brushing through being repeatedly coated on anode diffusion layer in anode catalyst slurries, until weightening finish reaches 5mg, under the condition of 120 DEG C, processing 1h afterwards, can anode gas diffusion electrode be obtained.
The preparation of step 3, cathode catalysis layer:
Take 16mg catalyst 60%Pt/40%C(mass ratio) and the mixing of 1.5ml pure water, sonic oscillation 10min, then PTFE solution and 2ml isopropyl alcohol that 3.5mg graphene aerogel and 10mg mass percent concentration are 5% is added, sonic oscillation 30min, then magnetic agitation 30min, obtains cathode inks;
Adopting the mode of brushing through being repeatedly coated on cathode diffusion layer in cathod catalyst slurries, until weightening finish reaches 5mg, under the condition of 120 DEG C, processing 1h afterwards, can cathode gas diffusion electrode be obtained.
The processing procedure of step 4, proton exchange membrane:
Cut out the PBI film of 1.5cm × 1.5cm, be immersed under room temperature concentration be in the phosphoric acid solution of 85% continue three days, period repeatedly agitating solution PBI film is fully contacted with phosphoric acid solution.Then taken out, blotted fast with the phosphoric acid solution of filter paper by film surface, then to be put it in vacuum drying chamber dry 10h at 110 DEG C.
Step 5, hot pressing become membrane electrode:
Proton exchange membrane is placed in the centre of anode gas diffusion electrode and cathode gas diffusion electrode, three puts neatly, is combined and is placed on hot press, at 180kg.cm
-2pressure under, hot pressing 5min, i.e. obtained high temperature proton exchange film fuel cell membrane electrode at the temperature of 135 DEG C.
Claims (7)
1. a high temperature proton exchange film fuel cell membrane electrode, be made up of anode diffusion layer, anode catalyst layer, proton exchange membrane, cathode catalysis layer, cathode diffusion layer, it is characterized in that described anode and cathode catalysis layer by graphene aerogel, PTFE and Pt is catalyst based is mixed.
2. high temperature proton exchange film fuel cell membrane electrode according to claim 1, is characterized in that the preparation method of described graphene aerogel is as follows: by hydro thermal method directly by the graphene aerogel by graphite oxide aqueous dispersions.
3. high temperature proton exchange film fuel cell membrane electrode according to claim 1, it is characterized in that the total weight of described graphene aerogel and PTFE and the catalyst based mass ratio of Pt are 1/4-1/10, the mass ratio of graphene aerogel and PTFE is 2:1-10:1.
4. a preparation method for high temperature proton exchange film fuel cell membrane electrode described in claim 1, is characterized in that described method step is as follows:
One, the preparation process of negative electrode and anode diffusion layer;
Two, the preparation process of anode catalyst layer:
Get a certain amount of PtRu/C catalyst, wherein Pt, Ru atomic ratio is 1:1-1:2, PtRu accounts for the 60-90% of total catalyst weight, mix with pure water, sonic oscillation, then appropriate graphene aerogel nano particle and a small amount of PTFE solution is added, add appropriate aqueous isopropanol again, controlling graphene aerogel and the total weight of PTFE and the mass ratio of PtRu/C catalyst is 1/4-1/10, the mass ratio of graphene aerogel and PTFE is 2:1-10:1, and supersonic oscillations, magnetic agitation are to forming uniform Anode inks;
Anode inks is evenly coated onto on anode diffusion layer, after oven dry, just obtains anode catalyst layer;
Three, the preparation process of cathode catalysis layer:
Weigh a certain amount of Pt/C catalyst, wherein Pt accounts for the 35%-85% of total catalyst weight, add the mixing of appropriate ultra-pure water, sonic oscillation, then graphene aerogel, PTFE solution and appropriate isopropyl alcohol is added, wherein the mass ratio of graphene aerogel and PTFE gross mass and Pt/C mixture is 1/4-1/10, and the mass ratio of graphene aerogel and PTFE is 2:1-10:1, and supersonic oscillations, magnetic agitation are to forming uniform cathode inks;
Brushed by cathode inks or spray to cathode diffusion layer on the surface, oven dry can obtain cathode catalysis layer;
Four, the processing procedure of proton exchange membrane;
Five, membrane electrode hot pressing.
5. the preparation method of high temperature proton exchange film fuel cell membrane electrode according to claim 4, is characterized in that described anode catalyst layer Pt carrying capacity is 1-4mg/ cm
2.
6. the preparation method of high temperature proton exchange film fuel cell membrane electrode according to claim 4, is characterized in that described cathode catalysis layer Pt carrying capacity is 3-6mg/ cm
2.
7. the preparation method of high temperature proton exchange film fuel cell membrane electrode according to claim 4, is characterized in that the carrying capacity of described positive and negative pole diffusion layer is 2-7mg.cm
-2.
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Cited By (8)
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CN106169587A (en) * | 2016-08-15 | 2016-11-30 | 陈隽 | A kind of new fuel cell of high alcohol-rejecting ability and preparation method thereof |
CN106784942A (en) * | 2017-01-23 | 2017-05-31 | 吉林大学 | A kind of high intensity, the high temperature proton conductive composite membrane of high proton conductivity and its application in high-temperature fuel cell |
WO2018113485A1 (en) * | 2016-12-19 | 2018-06-28 | 华南理工大学 | Membrane electrode of high power density proton exchange membrane fuel cell and preparation method therefor |
CN109638293A (en) * | 2018-10-26 | 2019-04-16 | 浙江博氢新能源有限公司 | High-temperature fuel cell membrane electrode and preparation method thereof and assemble method |
CN110854403A (en) * | 2019-10-24 | 2020-02-28 | 江苏大学 | High-temperature membrane fuel cell electrode capable of relieving loss of phosphoric acid electrolyte and preparation method thereof |
CN111628183A (en) * | 2020-05-27 | 2020-09-04 | 先进储能材料国家工程研究中心有限责任公司 | Preparation method of fuel cell catalyst slurry |
CN112186216A (en) * | 2019-07-05 | 2021-01-05 | 深圳市南科燃料电池有限公司 | Packaging method and membrane electrode assembly |
CN112825366A (en) * | 2019-11-21 | 2021-05-21 | 中国科学院大连化学物理研究所 | High-temperature proton membrane fuel cell membrane electrode based on hydrogen-poor reformed gas feeding, preparation and application |
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CN103831103A (en) * | 2014-03-14 | 2014-06-04 | 哈尔滨工业大学 | Graphene aerogel catalyst and preparation method thereof |
CN103943877A (en) * | 2014-04-29 | 2014-07-23 | 哈尔滨工业大学 | Membrane electrode of direct alcohol type fuel battery and preparation method thereof |
KR20140141838A (en) * | 2013-05-31 | 2014-12-11 | 한양대학교 산학협력단 | Preparation method of carbon-metal-metal oxide complex for fuel cell catalyst and carbon-metal-metal oxide complex for fuel cell catalyst using the same |
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CN103831103A (en) * | 2014-03-14 | 2014-06-04 | 哈尔滨工业大学 | Graphene aerogel catalyst and preparation method thereof |
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Cited By (9)
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CN106169587A (en) * | 2016-08-15 | 2016-11-30 | 陈隽 | A kind of new fuel cell of high alcohol-rejecting ability and preparation method thereof |
WO2018113485A1 (en) * | 2016-12-19 | 2018-06-28 | 华南理工大学 | Membrane electrode of high power density proton exchange membrane fuel cell and preparation method therefor |
CN106784942A (en) * | 2017-01-23 | 2017-05-31 | 吉林大学 | A kind of high intensity, the high temperature proton conductive composite membrane of high proton conductivity and its application in high-temperature fuel cell |
CN106784942B (en) * | 2017-01-23 | 2019-08-06 | 吉林大学 | A kind of high-intensitive, high temperature proton conductive composite membrane of high proton conductivity and its application in high-temperature fuel cell |
CN109638293A (en) * | 2018-10-26 | 2019-04-16 | 浙江博氢新能源有限公司 | High-temperature fuel cell membrane electrode and preparation method thereof and assemble method |
CN112186216A (en) * | 2019-07-05 | 2021-01-05 | 深圳市南科燃料电池有限公司 | Packaging method and membrane electrode assembly |
CN110854403A (en) * | 2019-10-24 | 2020-02-28 | 江苏大学 | High-temperature membrane fuel cell electrode capable of relieving loss of phosphoric acid electrolyte and preparation method thereof |
CN112825366A (en) * | 2019-11-21 | 2021-05-21 | 中国科学院大连化学物理研究所 | High-temperature proton membrane fuel cell membrane electrode based on hydrogen-poor reformed gas feeding, preparation and application |
CN111628183A (en) * | 2020-05-27 | 2020-09-04 | 先进储能材料国家工程研究中心有限责任公司 | Preparation method of fuel cell catalyst slurry |
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