CN102315457B - Passive miniature methanol fuel cell membrane electrode and its preparation method - Google Patents
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Abstract
The invention provides a passive miniature methanol fuel cell membrane electrode and its preparation method. The passive miniature methanol fuel cell membrane electrode is composed of a proton exchange membrane, an anode diffusion layer, an anode catalysis layer, a cathode diffusion layer and a cathode catalysis layer, wherein the cathode catalysis layer is composed of three-layer of superabsorbent nano particles in gradient distribution. The preparation method of the membrane electrode comprises the preparation of the cathode diffusion layer and the anode diffusion layer, the preparation of the anode catalysis layer, the preparation of the cathode catalysis layer and the process of forming membrane electrode by hot pressing. The passive miniature methanol fuel cell membrane electrode of the invention is capable of increasing the volumetric specific energy of a monomer battery, reducing the watered-out degree of the cathode, enhancing the mass transfer of oxygen, raising the power density and the discharge stability of the miniature methanol fuel cell. The invention has the advantages of convenient and rapid operation and easy control.
Description
Technical field:
The present invention relates to a kind of membrane electrode and preparation method thereof.
Background technology:
In recent years, electron and information technology has obtained develop rapidly, under the strong promotion of the market demand, all kinds of microminiature portable type electronic products emerge in succession as mobile phone, notebook computer, MP3, digital image device, personal digital assistant (PDA) etc., bring great convenience to people's life, simultaneously, also the performance of microminiature power supply is had higher requirement.Fuel cell is converted to electric energy by the chemical energy of fuel and oxidant, is not subject to the restriction of Carnot Engine circulation, as long as provide fuel to generate electricity, it has, and energy conversion efficiency is high, environmental friendliness, peace and quiet and reliability high.Micro direct methanol fuel battery (μ DMFC) directly utilizes methyl alcohol to act as a fuel, and oxygen or air, as a kind of fuel cell of oxidant, are compared with other type, and μ DMFC has that fuel source enriches, is easy to carry, the characteristics such as simple in structure.Press the fuel supply mode, μ DMFC is divided into active and passive type.Active referring to needs to utilize additional device as active as pump, valve etc. to control the fuel supply; Passive type does not need the additionaling power source for its postcombustion, the fuel cavity directly and battery be connected to form integral body, more be similar to the chemical cell that tradition is used, with active μ DMFC, compare, passive type μ DMFC is because its system bulk is little, without consuming the electric energy maintenance work, therefore the microminiature power system that becomes preferably.
With active μ DMFC, compare, passive type μ DMFC performance is lower, is mainly due to following reason: the mass transfer of (1) methyl alcohol.Passive type μ DMFC methanol solution fuel arrives Catalytic Layer through diffusion and reacts.In order to accelerate the mass transfer velocity of methyl alcohol, need to improve the concentration of methanol solution.But be subject to the restriction of methanol crossover problem, the concentration ratio of the methanol solution adopted at present is lower, is generally 2～4mol/L, and this just makes the volumetric specific energy of battery greatly reduce.(2) transmission of oxygen.Due to without any additional device, airborne oxygen mainly relies on diffusion and free convection to reach cathode catalysis layer.Because water can only be discharged by diffusion and natural evaporation, its speed reduces greatly, thereby increases the resistance to mass tranfer of oxygen.(3) negative electrode water management.Water is product at negative electrode, and is reactant at anode.In battery discharge procedure, the water of anode can be penetrated into negative electrode under the effect of electric osmose etc., not only causes the heavy losses of water in anode fuel, and has aggravated the water logging problem of negative electrode.Therefore improve the reverse osmosis ability of water from the negative electrode anode, not only can improve the transmission of negative electrode oxygen, and can improve the supply concentration of anode methanol solution, thereby greatly improve the volumetric specific energy of miniature methanol fuel cell.China Patent Publication No. 102005582 discloses a kind of structure and preparation method of direct alcohol fuel cell diaphragm electrode aggregate, built the cathode catalysis layer that polytetrafluoroethylene (PTFE) gradient distributes, thereby form gas delivery passage in cathode catalysis layer, improve the mass transfer of oxygen, but be hydrophobic material due to what adopt, therefore can't significantly improve proton exchange membrane negative electrode one side water concentration, and can't form high hydraulic pressure in proton exchange membrane negative electrode one side, thereby can't significantly improve the reverse osmosis ability of water from the negative electrode anode.
Summary of the invention:
One of purpose of the present invention is to provide a kind of passive miniature methanol fuel cell membrane electrode, it has improved in the battery operation process water from the reverse osmosis ability of negative electrode anode, reduce the content of water in anode one side methanol solution, improved the volumetric specific energy of cell.
Described purpose is achieved by the following scheme:
A kind of passive miniature methanol fuel cell membrane electrode, be comprised of proton exchange membrane, anode diffusion layer, anode catalyst layer, cathode diffusion layer and cathode catalysis layer; Described cathode catalysis layer is comprised of three layers of super water suction nano particle distribution gradient: with cathode diffusion layer nearest for outer, by Pt/C catalyst and Nafion resin, formed; With proton exchange membrane nearest be internal layer, by Pt/C catalyst, Nafion resin and super water suction nano particle, formed; Is intermediate layer between ectonexine, by Pt/C catalyst, Nafion resin and the super water-absorption particle of nanometer, formed equally, but the content of intermediate layer catalyst is less than skin higher than internal layer, and the content of the content of dry Nafion resin and super water suction nano particle all is less than internal layer higher than skin.
The outer field carrying capacity of cathode catalysis layer is 2-4mg.cm-2, and the carrying capacity in intermediate layer is 1-2mg.cm-2, and the carrying capacity of internal layer is 0.5-1mg.cm-2.
Another object of the present invention is to provide a kind of preparation method of passive miniature methanol fuel cell membrane electrode, has advantages of handled easily, is easy to control.
The preparation method of passive miniature methanol fuel cell membrane electrode comprises following preparation process:
A. the preparation of cathode diffusion layer and anode diffusion layer;
B. the preparation of anode catalyst layer;
C. the preparation of cathode catalysis layer;
D. hot pressing becomes membrane electrode;
Wherein, the preparation process of step C cathode catalysis layer is as follows:
By Pt/C catalyst and Nafion Solution Dispersion, in solvent, wherein, by weight percentage, the PtRu/C nanocatalyst is 70-90%, and the Nafion resin is 10-30%; Sonic oscillation 0.5～1h forms uniform slurry (A);
By Pt/C catalyst, Nafion solution with super water suction nanoparticulate dispersed in solvent, by weight percentage, the Pt/C nanocatalyst is that 10-20%, Nafion resin are that 40-60% and super water suction nano particle are 20-50%, mix, sonic oscillation 0.5～1h forms uniform slurry (B);
By Pt/C catalyst, Nafion solution with super water suction nanoparticulate dispersed in solvent, the content of Pt/C nanocatalyst, Nafion resin and super water suction nano particle is between outer (A) and internal layer (B), after mixing, sonic oscillation 0.5～1h forms uniform slurry (C);
The mode that by slurry (A), (C) and (B) adopts spraying or brush is applied to the surface of cathode diffusion layer successively, under the condition of 80～120 ℃, dries, and obtains the cathode gas diffusion electrode.Wherein, the outer field carrying capacity of cathode catalysis layer is 2-4mg.cm-2, and the carrying capacity in intermediate layer is 0.5-2mg.cm-2, and the carrying capacity of internal layer is 0.5-1mg.cm-2.
The preparation process of steps A cathode diffusion layer or anode diffusion layer is as follows: material with carbon element and ptfe emulsion are scattered in to isopropanol water solution, sonic oscillation 0.5～1h, magnetic agitation 0.5h forms uniform slurry afterwards, and wherein PTFE accounts for 30～50% of solid total content; Then by brush or the mode of blade coating by slurry through repeatedly being coated on supporting layer, under the condition of 80-120 ℃, dry, then roasting 20-40min under the condition of 300-380 ℃, obtain diffusion layer, wherein the carrying capacity of microporous layers is 1-5mg.cm-2, and the carrying capacity of Catalytic Layer is 3-6mg.cm-2.
The preparation process of step B Anodic Catalytic Layer is as follows: by PtRu/C catalyst and Nafion Solution Dispersion in the mixed solution that isopropyl alcohol and water form, sonic oscillation 1h forms uniform catalyst pulp, and wherein the Nafion resin accounts for the 10-40% of solid total content; Mode by brushing or blade coating is coated in catalyst pulp the surface of anode diffusion layer several times, under the condition of 80-120 ℃, dries, and obtains the anodic gas diffusion electrode, and wherein the carrying capacity of PtRu/C is 2-5mg.cm-2.
In step D, hot pressing film forming electrode process is as follows: the both sides that the anode gas diffusion layer for preparing and cathode gas diffusion layer are placed in respectively to proton exchange membrane, be combined and be placed on hot press, hot pressing 3-8min under the pressure of 100-200kg.cm-2, at the temperature of 120-140 ℃, make membrane electrode.
Described super water suction nano particle is one or more in the carbon nano-tube CNT of particle diameter below 10 nanometers, silicon dioxide, titanium dioxide, aluminium oxide.
Described solvent is a kind of or several arbitrarily in water, ethanol, isopropyl alcohol, ethylene glycol, glycerol, 1-methoxy-2-propanol (MOP), ether, benzinum, ethyl acetate, acetone.
The present invention adopts super water suction nano particle to regulate and control the water absorbing properties of the vertical degree of depth of passive miniature methanol fuel cell membrane electrode cathode catalysis layer, make the water absorbing capacity of cathode catalysis layer from gas diffusion layers to the proton exchange membrane direction increase gradually, the membrane electrode of this structure can effectively improve the hydraulic pressure of proton exchange membrane negative electrode one side, strengthen negative electrode and return the water effect to anode, improve the supply concentration of anode methanol solution, thereby improved the volumetric specific energy of cell, reduce the water flooding degree of negative electrode simultaneously, strengthen the mass transfer of oxygen, thereby power density and the discharge stability of miniature methanol fuel cell have been improved.That the method for the invention has advantages of is convenient to operation, be easy to control.
The accompanying drawing explanation:
Fig. 1 is structural representation of the present invention.
Embodiment:
Elaborate the preferred embodiment of the present invention below in conjunction with accompanying drawing.
In conjunction with Fig. 1, present embodiment is described.Present embodiment is comprised of proton exchange membrane 1, anode diffusion layer (comprising anode support 2 and anode micro porous layer 3), anode catalyst layer 4, cathode diffusion layer (comprising cathode support layer 5 and cathode micro porous layer 6), cathode catalysis layer 7; Wherein cathode catalysis layer 7 is located at the right side of proton exchange membrane, and the three-decker that becomes gradient to distribute by water absorbing properties forms, and the cathode catalysis layer super water suction nano-particle content nearest apart from proton exchange membrane is the highest, and catalyst content is minimum, and the Nafion resin content is the highest; The right side of cathode catalysis layer 7 is followed successively by cathode micro porous layer 6, cathode support layer 5; Anode catalyst layer 4 is located at the left side of proton exchange membrane 1, and the left side of anode catalyst layer 4 is followed successively by anode micro porous layer 3, anode support 2; Anode support 2, anode micro porous layer 3, anode catalyst layer 4, proton exchange membrane 1, cathode catalysis layer 7, cathode micro porous layer 6, cathode support layer 4 are integral admittedly by described order hot pressing, are membrane electrode of the present invention.
Super water suction nano particle is carbon nano-tube CNT, the silicon dioxide SiO of particle diameter below 10 nanometers
2, titanium dioxide TiO
2And aluminium oxide Al
2O
3In one or more.
The carbon paper that anode support 2 and cathode support layer 5 are E-tek or carbon cloth or other business-like carbon paper or carbon cloth.
The preparation process of passive miniature methanol fuel cell membrane electrode of the present invention is as follows:
The preparation of step 1, cathode diffusion layer and anode diffusion layer
The PTFE emulsion dispersion that to take the 60mg mass percent concentration be 10% is in 2ml isopropanol water (volume ratio of isopropyl alcohol and water 1: 1) solution, sonic oscillation 10min, taking afterwards 14mg carbon dust XC-72R adds in above-mentioned mixed liquor, sonic oscillation 30min, magnetic agitation 30min gets final product to obtain the microporous layers slurries that mix afterwards.The microporous layers slurries are adopted on the carbon paper of mode through repeatedly being coated to 1cm * 1cm of brushing, until weightening finish reaches 4mg.The carbon paper that scribbles microporous layers is dried to 30min at the temperature of 120 ℃, make the surfactant in isopropyl alcohol and water and PTFE emulsion volatilize fully, then process 30min at the temperature of 350 ℃, make at high temperature clinkering of PTFE form network configuration, obtain microporous layers PTFE content and be 30% cathode diffusion layer and anode diffusion layer.
Aforementioned material with carbon element used can be XC-72R (Cabot company), can be also Xc-72 (Cabot company), Black Pearls 2000 (Cabot company) and Ketjen Black (Japanese KBIC) etc.The Etek carbon paper that the thickness of usining is 100-1000 μ m or carbon cloth or other business-like carbon paper or carbon cloth are as the supporting layer of microporous layers.
The preparation of step 2, anode catalyst layer
The Nafion Solution Dispersion that to take the 80mg mass percent concentration be 5% is in 5ml isopropanol water (volume ratio of isopropyl alcohol and water 1: 1) solution, sonic oscillation 10min, take afterwards 16mg catalyst 40%Pt20%Ru/40%C (mass ratio) and add in above-mentioned mixed liquor, sonic oscillation 30min gets final product to obtain the catalyst slurry that mixes.The mode that catalyst slurry is adopted to spraying is through repeatedly being coated on anode diffusion layer, until weightening finish reaches 5mg, processes afterwards 2h and can obtain the anodic gas diffusion electrode under the condition of 100 ℃.
The preparation of step 3, cathode catalysis layer
The Nafion Solution Dispersion that to take the 80mg mass percent concentration be 5% is in 5ml isopropanol water (volume ratio of isopropyl alcohol and water 1: 1) solution, sonic oscillation 10min, take afterwards 16mg catalyst 60%Pt/40%C (mass ratio) and add in above-mentioned mixed liquor, sonic oscillation 30min gets final product to obtain the catalyst slurry (A) that mixes; The Nafion Solution Dispersion that to take the 120mg mass percent concentration be 5% is in 5ml isopropanol water (volume ratio of isopropyl alcohol and water 1: 1) solution, sonic oscillation 10min, take respectively afterwards 10mg catalyst 60%Pt/40%C (mass ratio) and the hydroxylated carbon nano-tube of 4mg and add in above-mentioned mixed liquor, sonic oscillation 30min gets final product to obtain the catalyst slurry (C) that mixes;
The Nafion Solution Dispersion that to take the 200mg mass percent concentration be 5% is in 5ml isopropanol water (volume ratio of isopropyl alcohol and water 1: 1) solution, sonic oscillation 10min, take respectively afterwards 4mg catalyst 60%Pt/40%C (mass ratio) and the hydroxylated carbon nano-tube of 6mg and add in above-mentioned mixed liquor, sonic oscillation 30min gets final product to obtain the catalyst slurry (B) that mixes.
Cathode catalysis layer slurries (A), (C), (B) are sprayed to cathode micro porous layer in order successively, obtain respectively a layer, c layer, b layer in Fig. 1, make the weightening finish of every layer be respectively 3mg, 1.5mg, 0.5mg, process afterwards 2h and can obtain the cathode gas diffusion electrode under the condition of 100 ℃.
The both sides that the anodic gas diffusion electrode for preparing and cathode gas diffusion electrode are placed in respectively to proton exchange membrane, be combined and be placed on hot press, hot pressing 5min under the pressure of 150kg.cm-2, at the temperature of 130 ℃, make the passive miniature methanol fuel cell membrane electrode.
Abovementioned steps one cathode diffusion layer and the preparation of anode diffusion layer, the preparation of step 2 anode catalyst layer, the process that the step 4 hot pressing becomes membrane electrode, can be prepared by any means of prior art.
The described cathode catalysis layer 7 of the present embodiment is that the three-decker that becomes gradient to distribute by water absorbing properties forms; in actual applications; also can be arranged to as required four layers, five layers or more multi-layered; so long as water absorbing properties becomes the gradient distributed architecture as described herein; can realize purpose of the present invention, therefore all within protection scope of the present invention.
Present embodiment is the exemplary illustration of this patent not to be limited to its protection range; those skilled in the art can also carry out part to it and change; as long as no the Spirit Essence that exceeds this patent, all be considered as the replacement that is equal to this patent, all within the protection range of this patent.
Claims (10)
1. a passive miniature methanol fuel cell membrane electrode, be comprised of proton exchange membrane, anode diffusion layer, anode catalyst layer, cathode diffusion layer and cathode catalysis layer, it is characterized in that:
Described cathode catalysis layer is comprised of three layers of super water suction nano particle distribution gradient: with cathode diffusion layer nearest for outer, by Pt/C catalyst and Nafion resin, formed, by weight percentage, the PtRu/C nanocatalyst is 70-90%, and the Nafion resin is 10-30%; With proton exchange membrane nearest be internal layer, by Pt/C catalyst, Nafion resin and super water suction nano particle, formed, by weight percentage, the Pt/C nanocatalyst is that 10-20%, Nafion resin are that 40-60% and super water suction nano particle are 20-50%; Is intermediate layer between ectonexine, by Pt/C catalyst, Nafion resin and the super water-absorption particle of nanometer, formed equally, but the content of intermediate layer catalyst is less than skin higher than internal layer, and the content of the content of dry Nafion resin and super water suction nano particle all is less than internal layer higher than skin.
2. passive miniature methanol fuel cell membrane electrode according to claim 1, is characterized in that the outer field carrying capacity of cathode catalysis layer is 2-4mg.cm
-2, the carrying capacity in intermediate layer is 1-2mg.cm
-2, the carrying capacity of internal layer is 0.5-1mg.cm
-2.
3. the preparation method of the described passive miniature methanol fuel cell membrane electrode of claim 1 or 2 is characterized in that comprising following preparation process:
The preparation of A, cathode diffusion layer and anode diffusion layer;
The preparation of B, anode catalyst layer;
The preparation of C, cathode catalysis layer;
D, hot pressing become membrane electrode;
Wherein, the preparation process of step C cathode catalysis layer is as follows:
By Pt/C catalyst and Nafion Solution Dispersion, in solvent, wherein, by weight percentage, the PtRu/C nanocatalyst is 70-90%, and the Nafion resin is 10-30%; Sonic oscillation 0.5～1h forms uniform slurry (A);
By Pt/C catalyst, Nafion solution with super water suction nanoparticulate dispersed in solvent, by weight percentage, the Pt/C nanocatalyst is that 10-20%, Nafion resin are that 40-60% and super water suction nano particle are 20-50%, mixes, and sonic oscillation 0.5～1h forms uniform slurry (B);
By Pt/C catalyst, Nafion solution with super water suction nanoparticulate dispersed in solvent, the content of Pt/C nanocatalyst, Nafion resin and super water suction nano particle is between outer (A) and internal layer (B), after mixing, sonic oscillation 0.5～1h forms uniform slurry (C);
The mode that by slurry (A), (C) and (B) adopts spraying or brush is applied to the surface of cathode diffusion layer successively, under the condition of 80～120 ℃, dries, and obtains the cathode gas diffusion electrode.
4. the preparation method of passive miniature methanol fuel cell membrane electrode according to claim 3, it is characterized in that, in steps A, the preparation process of cathode diffusion layer or anode diffusion layer is as follows: material with carbon element and ptfe emulsion are scattered in to isopropanol water solution, sonic oscillation 0.5～1h, magnetic agitation 0.5h forms uniform slurry afterwards, and wherein PTFE accounts for 30～50% of solid total content; Then by brush or the mode of blade coating by slurry through repeatedly being coated on supporting layer, under the condition of 80-120 ℃, dry, then roasting 20-40min under the condition of 300-380 ℃, obtain diffusion layer, wherein the carrying capacity of microporous layers is 1-5 mg.cm
-2.
5. the preparation method of passive miniature methanol fuel cell membrane electrode according to claim 3, it is characterized in that, the preparation process of step B Anodic Catalytic Layer is as follows: by PtRu/C catalyst and Nafion Solution Dispersion in the mixed solution that isopropyl alcohol and water form, sonic oscillation 1h forms uniform catalyst pulp, and wherein the Nafion resin accounts for the 10-40% of solid total content; Mode by brushing or blade coating is coated in catalyst pulp the surface of anode diffusion layer several times, under the condition of 80-120 ℃, dries, and obtains the anodic gas diffusion electrode, and wherein the carrying capacity of PtRu/C is 2-5 mg.cm
-2.
6. the preparation method of passive miniature methanol fuel cell membrane electrode according to claim 3, it is characterized in that, in step D, hot pressing film forming electrode process is as follows: the both sides that the anode gas diffusion layer for preparing and cathode gas diffusion layer are placed in respectively to proton exchange membrane, be combined and be placed on hot press, at 100-200kg.cm
-2Pressure under, hot pressing 3-8min at the temperature of 120-140 ℃, make membrane electrode.
7. according to the preparation method of the described passive miniature methanol fuel cell membrane electrode of claim 3-6 any one, it is characterized in that, super water suction nano particle is one or more in the carbon nano-tube CNT of particle diameter below 10 nanometers, silicon dioxide, titanium dioxide, aluminium oxide.
8. according to the preparation method of the described passive miniature methanol fuel cell membrane electrode of claim 3-6 any one, it is characterized in that, described solvent is a kind of or several arbitrarily in water, ethanol, isopropyl alcohol, ethylene glycol, glycerol, 1-methoxy-2-propanol (MOP), ether, benzinum, ethyl acetate, acetone.
9. according to the preparation method of the described passive miniature methanol fuel cell membrane electrode of claim 3-6 any one, it is characterized in that, in step c, the outer field carrying capacity of cathode catalysis layer is 2-4mg.cm
-2, the carrying capacity in intermediate layer is 0.5-2mg.cm
-2, the carrying capacity of internal layer is 0.5-1mg.cm
-2.
10. according to the preparation method of the described passive miniature methanol fuel cell membrane electrode of claim 3-6 any one, it is characterized in that, the carrying capacity of anode catalyst layer is 3-6mg.cm
-2.
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| CN103022509B (en) * | 2012-12-10 | 2014-08-13 | 哈尔滨工业大学 | Micro direct methanol fuel cell membrane electrode and preparation method thereof |
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| CN104064778A (en) * | 2014-06-30 | 2014-09-24 | 中国东方电气集团有限公司 | Fuel cell and fuel cell membrane electrode thereof |
| CN105098216A (en) * | 2015-08-19 | 2015-11-25 | 哈尔滨工业大学 | Micro direct methanol fuel cell membrane electrode assembly and preparation method therefor |
| CN105161736A (en) * | 2015-08-19 | 2015-12-16 | 哈尔滨工业大学 | Miniature direct methanol fuel cell membrane electrode and preparation method thereof |
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| CN109713319A (en) * | 2018-12-27 | 2019-05-03 | 哈尔滨工业大学 | Application of the carbon aerogels as cathode water absorption layer in micro direct methanol fuel battery membrane electrode |
| CN111628198B (en) * | 2019-02-28 | 2021-08-24 | 长城汽车股份有限公司 | Fuel cell membrane electrode |
| CN110289423A (en) * | 2019-05-17 | 2019-09-27 | 同济大学 | A kind of membrane electrode with catalyst gradient |
| CN110808392B (en) * | 2019-10-25 | 2021-02-23 | 山东魔方新能源科技有限公司 | Fuel cell membrane electrode and preparation process thereof |
| CN113991126B (en) * | 2021-10-28 | 2023-07-28 | 一汽解放汽车有限公司 | Membrane electrode of gradient proton exchange membrane fuel cell and preparation method and application thereof |
| CN114122413A (en) * | 2021-10-29 | 2022-03-01 | 上海氢晨新能源科技有限公司 | Membrane electrode catalyst layer with gradient pore structure and preparation method and application thereof |
| 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 |
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