CN106229533B - Compound Multilayer Film Electrode of hydrophilic/hydrophobic and preparation method thereof - Google Patents
Compound Multilayer Film Electrode of hydrophilic/hydrophobic and preparation method thereof Download PDFInfo
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- CN106229533B CN106229533B CN201610717402.2A CN201610717402A CN106229533B CN 106229533 B CN106229533 B CN 106229533B CN 201610717402 A CN201610717402 A CN 201610717402A CN 106229533 B CN106229533 B CN 106229533B
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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]
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- 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
Abstract
The invention discloses compound Multilayer Film Electrodes of a kind of hydrophilic/hydrophobic and preparation method thereof；The membrane electrode includes anode catalyst layer, proton exchange membrane and cathode catalysis layer, wherein cathode catalysis layer is the three-layer composite structure with hydrophilic gradient, one layer close to proton membrane is hydrophilic modifying layer, it is hydrophobically modified layer close to the side of gas diffusion layers, it is unmodified layer among two layers, to form hydrophilic gradient in cathode catalysis layer.Hydrophilic layer can play moisture-keeping function to proton exchange membrane and Catalytic Layer intermediate ion polymer under low relative humidity, to reduce the ionic conduction resistance of membrane electrode.Hydrophobic layer reduces the capillary pressure gradient between Catalytic Layer and gas diffusion layers, it is suppressed that high relative humidity, which is lauched from diffusion layer to Catalytic Layer, to spread.Scheme through the invention can reach the purpose of water distribution in optimization Catalytic Layer.
Description
Technical field
The present invention relates to Proton Exchange Membrane Fuel Cells technical fields, and in particular to one kind is for pem fuel electricity
Compound Multilayer Film Electrode of the hydrophilic/hydrophobic in pond and preparation method thereof.
Background technique
Core component of the membrane electrode as fuel cell, includes anode catalyst layer, proton exchange membrane and cathode catalysis layer,
It is the reacting environment of fuel cell, realizes conversion of the chemical energy to electric energy.The Catalytic Layer of membrane electrode is mainly porous structure, instead
It answers gas to enter Catalytic Layer by duct to be reacted, the water of generation is discharged by duct.Under low humidity conditions, contain in Catalytic Layer
Water is less, and proton membrane conductivity reduces, battery performance decline；Under high humidity, liquid water is accumulated in Catalytic Layer, leads to electricity
Water floods, performance decline.Therefore guarantee that the water balance in Catalytic Layer is the effective means for improving battery performance.Currently, for urging
Changing layer water balance, there are mainly two types of modification modes.One is doping hydroaropic substance, guarantees that battery still can under the low humidity
Moisture, which is provided, for proton membrane guarantees its lower resistivity.The second is doping lyophobic dust, prevents high humility (or high current)
Lower battery water logging.Two improvements are respectively suitable for the situation run under low humidity and high humidity.Single doping (is only adulterated
Hydrophilic or hydrophobic substance) amount it is lower when, it is hydrophilic variation it is smaller.Improve doping will lead to catalysis layer porosity reduction again,
Influence battery mass transfer.Therefore, it is necessary to reasonable modification strategies to improve battery performance.
Summary of the invention
It is a kind of for pem fuel it is an object of the invention in view of the deficiency of the prior art, provide
Compound Multilayer Film Electrode of the hydrophilic/hydrophobic of battery and preparation method thereof.The present invention is innovatively by hydrophobically modified layer and hydrophilic
Modified layer is combined in same Catalytic Layer.
The purpose of the present invention is achieved through the following technical solutions:
In a first aspect, the present invention relates to a kind of compound Multilayer Film Electrode of hydrophilic/hydrophobic, including anode catalyst layer, proton
Exchange membrane and cathode catalysis layer, the cathode catalysis layer have hydrophilic gradient；Close to gas diffusion on the cathode catalysis layer
The side of layer is hydrophobicity, is hydrophily close to the side of proton exchange membrane.
Preferably, the cathode catalysis layer is the three-layer composite structure with hydrophilic gradient, close to proton exchange membrane
One layer is hydrophilic modifying layer, and one layer close to gas diffusion layers is hydrophobically modified layer, and centre is unmodified layer.
Preferably, the hydrophilic modifying of the hydrophilic modifying layer by cathode inks doping silicon dioxide come real
It is existing.
Preferably, the hydrophobically modified of the hydrophobically modified layer by cathode inks adulterated PTFE realize.
Second aspect, the invention further relates to a kind of preparation method of compound Multilayer Film Electrode of hydrophilic/hydrophobic above-mentioned, institutes
The method of stating includes the following steps:
Three parts of S1, configuration cathode inks；
S2, the doping silicon dioxide in wherein a cathode inks, form hydrophilic slurry；It is urged in another cathode
Adulterated PTFE in agent slurry forms water-repellent slurry；
S3, one side surface of proton exchange membrane successively spray the hydrophilic slurry, undoped cathode inks, dredge
Water slurry forms the cathode catalysis layer with hydrophilic modifying layer, unmodified layer, hydrophobically modified layer three-layer composite structure.
Preferably, in step S2, the partial size of the silica adulterated in cathode inks is 15nm.Of the invention
In system, grain diameter influence's processing performance of silica.
Preferably, after step S3 further include:
S4, Anode inks are sprayed in another side surface of the proton exchange membrane of sprayed cathode Catalytic Layer, is formed
Anode catalyst layer is to get the compound Multilayer Film Electrode of the hydrophilic/hydrophobic.
Preferably, the cathod catalyst selected in the cathode inks of step S1 is Pt/C catalyst.Wherein, ion
Resin uses business Nafion, and solvent is ethyl alcohol；The mass fraction of carbon is the quality of 0.3~0.4%, Nifion and carbon in slurry
Than for 0.7~0.9:1.
Preferably, in step S3, every layer of platinum carrying capacity is 0.08~0.1mg/cm in the cathode catalysis layer2。
Preferably, which is characterized in that the mass percentage of silica is 30~35wt% in the hydrophilic modifying layer.
Preferably, the mass percentage of PTFE is 30~35wt% in the hydrophobically modified layer.
Compared with prior art, the invention has the following beneficial effects:
1) membrane electrode is modified the method for mostly using single doping at present, i.e., only adulterates hydrophilic or hydrophobic substance, cause to contact
The span of angle distribution is smaller；The present invention expands the contact angles gradient of Catalytic Layer, realizes bigger capillary pressure ladder
Degree is more conducive to liquid water and spreads to single direction.
2) current method of modifying adapts to high humility or low-humidity environment with can only making membrane electrode unicity；The present invention is in height
It is all had the advantage that under humidity and low-moisture conditions firstly, the capillary pressure of Catalytic Layer becomes larger from the inside to the outside, is conducive to anti-
The water that should be generated is migrated to proton membrane first, reduces the internal resistance of cell；Secondly, outside is pore hydrophobic layer, capillary pressure is greater than
Diffusion layer is conducive to superfluous water and discharges.
3) present invention optimizes the spatial distributions of modified layer: hydrophilic layer is contacted with proton membrane, ensure that the wetting of proton membrane；
Hydrophobic layer is contacted with the microporous layers of carbon paper surface, is promoted extra water to being discharged outside Catalytic Layer, is played and microporous layers class
As act on；Intermediate unmodified layer is transition zone, realizes the continuity of contact angle gradient between two modified layers, also prevents
It is interfered with each other between incompatible modified layer.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is film electrode structure schematic diagram of the present invention；
Fig. 2 is the contact angle test schematic diagram of each modified layer of membrane electrode；Wherein, (a) is silica modified rear catalysis
The contact angle of layer is (b) contact angle of unmodified Catalytic Layer, (c) is the contact angle of the modified Catalytic Layer of PTFE；
Fig. 3 is the performance curve test schematic diagram of comparative example and embodiment；
Fig. 4 is the high-frequency resistance test schematic diagram of comparative example and embodiment；
Fig. 5 is the ac impedance measurement schematic diagram of comparative example and embodiment；
Fig. 6 is the constant current attenuation test schematic diagram of comparative example and embodiment.
Specific embodiment
The following describes the present invention in detail with reference to examples.Following embodiment will be helpful to those skilled in the art
The present invention is further understood, but the invention is not limited in any way.It should be pointed out that those skilled in the art
For, without departing from the inventive concept of the premise, it can also make certain adjustments and improvements.These belong to guarantor of the invention
Protect range.
Embodiment
The present embodiment be related to a kind of compound Multilayer Film Electrode of the hydrophilic/hydrophobic for Proton Exchange Membrane Fuel Cells and its
Preparation method.
The present embodiment realizes the deposition of multilayer film by electrostatic spray.Three parts of Pt/C catalyst pulps are prepared first, from
Subtree rouge uses business Nafion, and solvent is ethyl alcohol.The mass fraction of carbon is the mass ratio of 0.39%, Nafion and carbon in slurry
It is 0.8.Be separately added into wherein two parts of slurries 15nm partial size silica and 60% PTFE emulsion as hydrophilic slurry
And water-repellent slurry.Prepared slurry ultrasonic vibration is used to spray after twenty minutes.The present embodiment is existed using electrostatic spray
Nafion proton film surface sprays Catalytic Layer, and spraying temperature is 90 DEG C, order are as follows: hydrophilic slurry, unmodified slurry, hydrophobic slurry
Material.After cathode completes, anode catalyst layer is sprayed at the proton membrane back side using unmodified slurry.Membrane electrode after the completion is as schemed
Shown in 1.Platinum carrying capacity in every layer of cathode is about 0.1mg/cm2(three layers of total 0.3mg/cm2).The quality of silica in hydrophilic layer
Percentage composition is about 30wt%, and the mass percentage of PTFE is about 30wt% in hydrophobic layer.Fig. 2, which gives, carries out Catalytic Layer
Contact angle test after hydrophilically modified.For unmodified Catalytic Layer, contact angle is 146.9 °.Using silica modified
Afterwards, contact angle is reduced to 138.1 °, it is known that the doping of silica improves the hydrophily of Catalytic Layer.Similarly, the doping of PTFE mentions
The high hydrophobicity of Catalytic Layer, contact angle are increased to 152.6 °.According to formula:
Δ p is additonal pressure in capillary, and σ is surface tension, and r is capillary radius.The increase of contact angle improves attached
Plus-pressure.For the present embodiment, additonal pressure is gradually increased from one side of proton membrane to diffusion layer side, is formd and is promoted water
To the barometric gradient of anode side reflux, the conductivity of film ensure that.
Fig. 3 gives the cell performance curve of membrane electrode.The production method of reference examples is identical with embodiment, and difference exists
The modified materials such as undoped silicon dioxide and PTFE in Catalytic Layer.From the figure 3, it may be seen that comparative example and embodiment are opposite 100%
Performance under humidity is nearly identical.Although embodiment is adulterated by hydrophilic silica, do not go out under high current
Existing water logging, this outermost PTFE layers of explanation have effectively acted as drainage, ensure that the mass-transfer performance of battery.When relatively wet
When degree is down to 67%, battery internal water accumulation is reduced, and mass transfer improves, and two performances are all promoted.The performance of embodiment is obviously high
In comparative example, this is because ponding also causes proton film resistance to increase under the conditions of low relative humidity while reduction, affect
Battery performance.The Modification design of embodiment improves water to the reverse osmosis of anode direction, reduces the resistance of film, performance be better than than
Compared with example.
Fig. 4 is resistivity of two kinds of membrane electrodes under different humidity, it can be clearly seen that the resistance of embodiment under low humidity
Rate is significantly lower than the resistance of comparative example, explains the reason of performance of comparative example is better than embodiment.Under high humidity, two
Resistivity is essentially identical.This illustrates that film conductivity after sufficiently soaking reaches highest, and resistance is not to restrict battery performance
Principal element.The ac impedance spectroscopy that Fig. 5 is two.In low frequency range, embodiment also embodies lower mass transfer under the low humidity
Resistance.
The present embodiment is in current density 800mA/cm2, carried out the test under the conditions of dry gas.Battery is first in 800mA/
cm2, air is switched to dry gas at 0s time point, examines battery in 15 minutes by operation to stable state under 100% humidity
Voltage attenuation.The about 16mV as shown in fig. 6, embodiment has decayed in 15 minutes, the about 35mV and comparative example has then been decayed.Thus may be used
See, the capillary pressure gradient of embodiment can more promote the reverse osmosis of water, effectively keep the humidity of proton membrane, exist to promote battery
Performance under the conditions of more dry.In addition, embodiment occurs what voltage more times was flown up during the test relative to comparative example
Phenomenon, this is because also illustrating that the water content of membrane electrode in embodiment is higher caused by " breakthrough " of liquid water.
In conclusion the present invention embodies preferably water balance characteristic.Firstly, the modified layer of three-decker establishes effectively
Capillary pressure gradient, make reaction in water to anode direction spread, reduce the film resistivity under low relative humidity.Its
It is secondary, it introduces hydrophobic PTFE and effectively prevents battery water logging under high humility.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (7)
1. a kind of compound Multilayer Film Electrode of hydrophilic/hydrophobic, including anode catalyst layer, proton exchange membrane and cathode catalysis layer,
It is characterized in that, the cathode catalysis layer has hydrophilic gradient；Side on the cathode catalysis layer close to gas diffusion layers is
Hydrophobicity is hydrophily close to the side of proton exchange membrane；
The cathode catalysis layer is the three-layer composite structure with hydrophilic gradient, and one layer close to proton exchange membrane changes to be hydrophilic
Property layer, be hydrophobically modified layer close to one layer of gas diffusion layers, centre is unmodified layer；The hydrophilic modifying of the hydrophilic modifying layer
By in cathode inks doping silicon dioxide realize；The hydrophobically modified of the hydrophobically modified layer in cathode by urging
Adulterated PTFE is realized in agent slurry.
2. a kind of preparation method of the compound Multilayer Film Electrode of hydrophilic/hydrophobic as described in claim 1, which is characterized in that institute
The method of stating includes the following steps:
Three parts of S1, configuration cathode inks；
S2, the doping silicon dioxide in wherein a cathode inks, form hydrophilic slurry；In another cathod catalyst
Adulterated PTFE in slurry forms water-repellent slurry；
S3, the hydrophilic slurry, undoped cathode inks, hydrophobic slurry are successively sprayed in one side surface of proton exchange membrane
Material forms the cathode catalysis layer with hydrophilic modifying layer, unmodified layer, hydrophobically modified layer three-layer composite structure.
3. the preparation method of the compound Multilayer Film Electrode of hydrophilic/hydrophobic as claimed in claim 2, which is characterized in that step S3
Later further include:
S4, Anode inks are sprayed in another side surface of the proton exchange membrane of sprayed cathode Catalytic Layer, forms anode
Catalytic Layer is to get the compound Multilayer Film Electrode of the hydrophilic/hydrophobic.
4. the preparation method of the compound Multilayer Film Electrode of hydrophilic/hydrophobic as claimed in claim 2, which is characterized in that step S1
Cathode inks in the cathod catalyst selected be Pt/C catalyst.
5. the preparation method of the compound Multilayer Film Electrode of hydrophilic/hydrophobic as claimed in claim 4, which is characterized in that step S3
In, every layer of platinum carrying capacity is 0.08~0.1mg/cm in the cathode catalysis layer2。
6. the preparation method of the compound Multilayer Film Electrode of hydrophilic/hydrophobic as described in any one of claim 2~5, feature
It is, the mass percentage of silica is 30~35wt% in the hydrophilic modifying layer.
7. the preparation method of the compound Multilayer Film Electrode of hydrophilic/hydrophobic as described in any one of claim 2~5, feature
It is, the mass percentage of PTFE is 30~35wt% in the hydrophobically modified layer.
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| CN106848355A (en) * | 2017-02-20 | 2017-06-13 | 南京大学 | The electrostatic spinning and electrostatic spraying preparation method of a kind of membrane electrode CCM |
| CN109390592B (en) * | 2017-08-04 | 2021-12-31 | 上海汽车集团股份有限公司 | Membrane electrode and preparation method thereof |
| CN107611452A (en) * | 2017-08-15 | 2018-01-19 | 华南理工大学 | A kind of preparation method of the membrane electrode containing three-dimensional hydrophobic cathode catalysis layer |
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| CN108063267B (en) * | 2017-12-26 | 2020-06-05 | 新源动力股份有限公司 | Catalytic layer with multilayer structure for fuel cell and preparation method thereof |
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| CN112072120B (en) * | 2020-09-07 | 2021-07-20 | 贵州梅岭电源有限公司 | Hydrophilic/hydrophobic membrane electrode relating to ionic liquid |
| CN113130951B (en) * | 2021-04-02 | 2022-07-29 | 上海电气集团股份有限公司 | Membrane electrode, preparation method thereof and fuel cell |
| CN114520339A (en) * | 2022-01-26 | 2022-05-20 | 浙江天能氢能源科技有限公司 | CCM for fuel cell and preparation method thereof |
| CN115075056B (en) * | 2022-06-21 | 2023-09-26 | 华南理工大学 | Carbon fiber paper with directional water transmission function and preparation method and application thereof |
| CN114976162A (en) * | 2022-07-22 | 2022-08-30 | 上海明天观谛氢能科技有限公司 | Fuel cell membrane electrode and preparation method thereof |
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