CN101286564B - Composite anode for direct methanol fuel cell and method for making the same - Google Patents
Composite anode for direct methanol fuel cell and method for making the same Download PDFInfo
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- CN101286564B CN101286564B CN2008100381597A CN200810038159A CN101286564B CN 101286564 B CN101286564 B CN 101286564B CN 2008100381597 A CN2008100381597 A CN 2008100381597A CN 200810038159 A CN200810038159 A CN 200810038159A CN 101286564 B CN101286564 B CN 101286564B
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Abstract
The invention provides a composite anode of a direct-methanol fuel cell and a manufacturing method thereof. The invention is characterized in that the composite anode is composed of a supporting layer, a diffusion layer and a catalyzing layer, wherein, the diffusion layer is the structure of a network channel which is composed of carbon nano-tubes. The typical characteristics of the preparation process are that: (1) a certain amount of the carbon nano-tubes or the carbon nano-tubes added with a certain amount of other carbon materials are dispersed in isopropanol aqueous solution to obtain a sizing agent (A); (2) a certain amount of polyfluortetraethylene latex is added into the (A) and evenly dispersed to form serosity (B); (3) the (B) is evenly coated on the supporting layer, and the diffusion layer (C) loaded by the supporting layer is formed after 300-350 DEG C high-temperature roasting; (4) the (C) is coated with a layer of PtRu catalyst and then heat pressed with a cathode and a Nafion membrane to obtain a membrane electrode aggregation (MEA). Therefore, the transmission efficiency of the fuel at the anode is improved and the internal resistance of the battery is reduced so as to enhance the power density and service life of the battery.
Description
Technical field
The present invention relates to composite anode and manufacture method that direct methanol fuel cell is used, relate to a kind of composite anode and manufacture method that can improve performance of direct methanol fuel cells and stability thereof or rather, the use of this composite anode can improve the mass-transfer efficiency of liquid fuel, has improved the performance and the stability thereof of battery effectively.
Background technology
Over past ten years, along with the fast development of portable type electronic product (as mobile phone, palmtop PC, MP3 etc.) with popularize, the cry of customer requirements high-energy-density chemical power source grows to even greater heights.In order to adapt to the demand of various novel microelectronic products to the battery high-energy-density, since the mid-90 in 20th century, many renowned companies of countries in the world and scientific research institution constantly make great efforts to attempt to develop low power fuel cell, expectation can be applied to compact power, as the power supply as miniaturized electronicss such as laptop computer, digital camera and mobile phone power supplys.
Directly alcohol fuel battery (DAFCs) is the fuel cell that a class is used liquid fuels such as methyl alcohol, formic acid and ethanol, and they have the following advantages: fuel source is abundant, and is cheap, and is easy to carry and stores; System is simple, the fuel direct oxidation; Theoretical specific energy density height, uses the liquid fuel handling safety reliable at compact conformation; Microminiaturized potentiality are big, compare with hydrogen-oxygen proton exchange membrane fuel cell, and the safety issue when directly alcohol fuel battery does not exist storing hydrogen and transportation can more effectively realize the miniaturized design and the application of fuel cell.So DAFC is the preferred compact power of miniaturized electronics power supply, has wide Commercial Prospect.
In 20 end of the centurys, directly be that the fuel cell of fuel, especially direct methanol fuel cell (DMFC) become the focus of research and development with alcohols, and obtained considerable progress.Yet direct methanol fuel cell will reach practical application and also have many science and problem technology to remain further to be solved, and mainly face two technical problems: (1) methanol electro-oxidizing speed is slow.Because methanol oxidation is a kind of from the poisoning process, oxidation overpotential height makes that the more theoretical electromotive force of actual output voltage is much lower; (2) methyl alcohol easily is penetrated into negative electrode by solid electrolyte film, has not only reduced fuel availability, also makes cathod catalyst to the reduction of hydrogen reduction activity, produces " mixed potential " on oxygen cathode, causes battery performance to reduce.Anode fuel concentration is high more, and fuel strides that the speed of film transmission is just fast more, be penetrated into negative electrode in the unit interval quantity of methyl alcohol is just many more, causes the decay of battery performance just big more.Therefore, in order to alleviate the power density of striding direct alcohol fuel batteries such as film transmission, lifting DMFC of methyl alcohol, the working concentration of methanol solution to be reduced usually.But when the methanol solution that adopts low concentration acted as a fuel, methanol solution was limited in the transmission speed of electrode interior, causes battery controlled by mass transfer, makes that the power density of fuel cell system is very low.And directly there is the limited problem of mass transfer too in aminic acid fuel battery, and formic acid is very fast in the catalytic oxidation speed of catalyst surface, will directly not cause the battery system performance not good if mass transfer catches up with.Therefore, how directly to realize the effective mass transfer technology of fuel in the alcohol fuel battery system, it is crucial keeping suitable fuel transmission speed.
Summary of the invention
The invention provides a kind of direct alcohol fuel battery composite anode, preparation method, improved the transmission of liquid fuel effectively in electrode interior, guaranteed the efficient mass transfer of fuel, thereby improved the performance and the stability thereof of fuel cell system to catalyst surface.
The invention provides a kind of composite anode, preparation method that can improve performance of direct methanol fuel cells and stability thereof.Described composite anode is to be made of supporting layer, diffusion layer and Catalytic Layer.Described composite anode is to be supporting layer with carbon paper or carbon cloth, the mixture that applies earlier finely dispersed carbon nanotube-based material with carbon element and binding agent is as diffusion layer, apply the noble metal catalyst of one deck energy catalyzing alcohols fuel generation electroxidation then as required again, as platinum-ruthenium etc., by steps such as proper heat treatment, the composite anode of electrochemical reaction takes place in it to prepare energy high efficiency of transmission liquid fuel and catalysis.It is characterized in that diffusion layer is made of the structure of network channel carbon nano-tube.
Now that each step division is as follows:
1, the preparation of anode diffusion layer slurry: with the mixture of certain quantity of carbon nanometer pipe or carbon nano-tube and other material with carbon element in the ultrasonic aqueous solution that is scattered in isopropyl alcohol.Add entry and isopropyl alcohol mixture by every milligram of carbon dust 0.02-2mL amount, wherein the volume ratio of water and isopropyl alcohol is controlled at 0.5-3.Carbon nano-tube can be single wall, double-walled or the multi-walled carbon nano-tubes (SWNTs, DWMTs, MWNTs) of different model and different tube diameters, other material with carbon element can be deceived activated carbon etc. for business-like XC-72 carbon, XC-72R carbon, BP-2000 and Ketjen, in the mixture of carbon nano-tube and other material with carbon element, the quality percentage composition of carbon nano-tube is controlled in the 100%-20% scope.Said mixture mechanical agitation or ultrasonic agitation 0.5-4h can be obtained finely dispersed slurries A.
2, in slurry A, add a certain amount of polytetrafluoroethylene as binding agent,, form equal slurries B through mechanical agitation or ultrasonic agitation 0.5-4h.Wherein binding agent accounts for the 10-40% of material with carbon element mass percent.
3, the preparation of diffusion layer: get carbon paper that thickness is 10 μ m-2mm or carbon cloth or other business-like carbon paper supporting layer as combination electrode, the prepared slurries B of step (2) is coated on the supporting layers such as carbon paper or carbon cloth equably by brushing or spraying, through high-temperature roasting 10min-3h in about 300-350 ℃ air, nitrogen or argon gas, promptly form the diffusion layer of supporting layer load, wherein the carrying capacity of material with carbon element is controlled to be 0.3-2.5mgcm
-2High temperature sintering helps making the fully volatilizations such as surfactant that are mixed with among solvent, the PTFE, and the redistribution of PTFE clinkering at high temperature meanwhile enters in the slit of diffusion layer, constitutes a kind of structure of network channel.
4, the preparation of anode catalyst layer slurries: catalyst slurry comprises noble metal catalyst, Nafion resin and dispersant.Wherein catalyst comprises business-like noble metal catalysts such as Pt-Ru is black, Pt-Ru/C.The 15%-20% that the Nafion resin accounts for the Catalytic Layer dry weight presses 0.025-0.5mLmg
-1The amount mixed liquor that adds entry and isopropyl alcohol make dispersant (volume ratio of water and isopropyl alcohol is 0.5-2), 40 ℃ of following ultrasonic agitation 2h of control temperature can obtain finely dispersed catalyst slurry.
5, the preparation of anode catalyst layer: the prepared catalyst slurry of step 4 being coated in uniformly on the diffusion layer of step 3 preparation, drying 1-5h under through 105 ℃, eliminate solvent remaining in the Catalytic Layer, is 5-15min 150 ℃ of following heat treatments then.The composite anode of electrochemical reaction takes place in it can to obtain energy high efficiency of transmission liquid fuel and catalysis.
6, flow process makes MEA as shown in Figure 1.The preparation condition of negative electrode is as follows: the TGP-H-060 with the 20wt.% hydrophobicity makes supporting layer, and diffusion layer consists of 2mgcm
-2The PTFE of Vulcan XC-72 and 20wt.%, Catalytic Layer is 6mgcm by the Pt carrying capacity
-2Constitute with 20wt.%Nafion, preparation process is identical with the anode preparation process.Composite anode, negative electrode and Nafion film form the membrane electrode assembly of " three-in-one " through hot pressing in 3 minutes under 130 ℃, 6MPa.
The composite anode of the present invention's preparation can improve the transmission of liquid fuel in electrode interior effectively, be applied to significantly improve in the membrane electrode assembly of direct methanol fuel cell the stability (seeing embodiment for details) of the maximum power density and the constant current discharge of fuel cell system, and it is simple to have method, easy operating, characteristics such as environmental friendliness have application promise in clinical practice.
Description of drawings
Fig. 1 membrane electrode assembly preparation technology flow chart;
Fig. 2 direct methanol fuel cell MEA performance testing device;
1. methyl alcohol storage tank 2. anode collector 3. seal washer 4.MEA 5. seal washers 6. cathode current collectors 7. cathode branch faggings;
The different material with carbon elements of Fig. 3 are made MEA measured polarization curve and power density curve (fuel is the methanol aqueous solution of 2M) of full passive type operation under 25 ℃ of condition of normal pressure that anode MPL makes;
The different material with carbon elements of Fig. 4 are made 4 hours constant current discharge curves of MEA that anode MPL makes, and (fuel is the methanol aqueous solution of 2M, and discharge current density is 40mAcm
-2);
(fuel is the methanol aqueous solution of 2M to Fig. 5, and discharge current density is 40mAcm in order to make long-time life test curve that anode MPL makes MEA with L.MWNTs10
-2);
Fig. 6 different model carbon nano-tube is made MEA measured polarization curve and power density curve (fuel is the methanol aqueous solution of 2M) of full passive type operation under 25 ℃ of condition of normal pressure that anode MPL makes;
Fig. 7 different model carbon nano-tube is made 7 hours constant current discharge curves of MEA that anode MPL makes, and (fuel is the methanol aqueous solution of 2M, and discharge current density is 40mAcm
-2);
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, illustrating substantive distinguishing features of the present invention and obvious improvement, but embodiments of the present invention only limit to the described mode of embodiment absolutely not.
1. the Vulcan XC-72 that takes by weighing 19.8mg adds among the container a, 19.7mg MWNTs places container b, in container c, add 9.8mgVulcan XC-72 and 9.8mgMWNTs, adding the 40mg mass percentage concentration respectively in three containers then is that the PTFE emulsion of 12.4wt% and the mixed liquor of 1mL water and isopropyl alcohol (volume ratio of isopropyl alcohol and water is 1: 1) are made binding agent and dispersant, and ultrasonic dispersion 2h can obtain uniform slurries.
2. it is black to take by weighing 80.3mg Pt-Ru, add the 100mg ultra-pure water with all catalyst wetting after, adding the 267.3mg quality is the Nafion solution of 5.3wt% than concentration, the mixed liquor (volume ratio of isopropyl alcohol and water is 1: 1) that adds 3mL water and isopropyl alcohol is then made dispersant, and the control temperature is lower than 40 ℃ of ultrasonic dispersion 2h.
3. (its model is TGP-H-060 to get the carbon paper that 3 areas are about 3cm*3cm, hydrophobicity is 0wt.%) supporting layer of the Heyang utmost point of writing in reply, the prepared 3 parts of slurries of step 1 are coated in the zone of 2cm*2cm on the carbon paper respectively uniformly, make carbon paper increase weight respectively 5.0mg, 5.5mg, 5.0mg and three carbon papers are labeled as a, b, c accordingly by institute's pasting liquid.The three makes polymer clinkering redistribution under this temperature all through 350 ℃ of high temperature sintering half an hour, enters in the slit among the MPL, constitutes a kind of hydrophobic network channel.
4. on the basis of step 3, the prepared catalyst slurry of step 2 is coated in respectively on three diffusion layers uniformly, make its increase weight respectively 31.6mg, 31.7mg, 31.7mg, dry 3h down through 105 ℃ again, eliminate dispersant remaining in the Catalytic Layer, then at 150 ℃ of following heat treatment electrode 10min.Cut out the wherein zone of 2cm*2cm, the composite anode of electrochemical reaction takes place in it can to obtain having high efficiency of transmission liquid fuel and catalysis.
5. with the negative electrode of a 4cm*4cm of above-mentioned similar method preparation, make supporting layer with the TGP-H-060 of 20wt.% hydrophobicity, diffusion layer consists of 2mgcm
-2The PTFE of Vulcan XC-72 and 20wt.%, Catalytic Layer is 6mgcm by the Pt carrying capacity
-2Constitute with 20wt.%Nafion.The electrode of bulk is cut into the small electrode of four 2cm*2cm, get wherein three respectively with above-mentioned three composite anodes pairing, with the hot pressing 3 minutes under 130 ℃, 6MPa together of Nafion117 dielectric film, can obtain three MEA, it is labeled as a, b, c accordingly.
6. respectively above-mentioned MEA is assembled into monocell with device shown in Figure 2 and carries out performance test (Fig. 3) and stability test (Fig. 4).The maximum power density of a, b, c is respectively 28.1mWcm
-2, 24.4mWcm
-2, 21.3mWcm
-2, the introducing of MWNTs helps improving performance and the stability of MEA.Fig. 5 is the result of sample c life test, and through 300 hours constant current discharges, voltage was still stable.
1. take by weighing 20mg S.MWNTs, L.MWNTs respectively, (wherein S represents short tube for L.SWMTs, L.DWNTs, L represents long tube, used carbon nano-tube is nanometer port, Shenzhen Co., Ltd product, purity is all greater than 95%) place container A, B, C, D, adding the 40mg quality respectively in 4 containers then is that the PTFE emulsion of 12.4wt.% and the mixed liquor of 1mL water and isopropyl alcohol (volume ratio of isopropyl alcohol and water is 1: 1) are made binding agent and dispersant than concentration, and ultrasonic dispersion 2h can obtain uniform slurries.
2. it is black to take by weighing 110mg Pt-Ru, add the 140mg ultra-pure water with all catalyst wetting after, adding the 367mg quality is the Nafion solution of 5.3wt.% than concentration, the mixed liquor (volume ratio of isopropyl alcohol and water is 1: 1) that adds 4mL water and isopropyl alcohol is then made dispersant, and the control temperature is lower than 40 ℃ of ultrasonic dispersion 2h.
3. (its model is TGP-H-060 to get the carbon paper that 4 areas are about 3cm*3cm, hydrophobicity is 0wt.%) supporting layer of the Heyang utmost point of writing in reply, the prepared 4 parts of slurries of step 1 are applied in the zone of 2cm*2cm on it respectively uniformly, make carbon paper increase weight respectively 4..9mg, 5.0,4.9mg, 4.8mg and four carbon papers are labeled as A, B, C, D accordingly by institute's pasting liquid.Four all through 350 ℃ of high temperature sintering half an hour, make fully volatilizations such as the solvent that is mixed with in dispersant, the polymer and surfactant, and the redistribution of polymer clinkering at high temperature meanwhile enters in the slit among the MPL, constitutes a kind of network channel.
4. on the basis of step 3, the prepared catalyst slurry of step 2 is coated in respectively on four diffusion layers uniformly, make its increase weight respectively 32.6mg, 31.7mg, 30.2mg, 29.5, dry 3h down through 105 ℃ again, eliminate dispersant remaining in the Catalytic Layer, then at 150 ℃ of following heat treatment electrode 10min.The zone that cuts out 2cm*2cm wherein very can the high efficiency of transmission liquid fuel and catalysis its composite anode of electrochemical reaction takes place.
5. with the negative electrode of a 4cm*4cm of above-mentioned similar method preparation, make supporting layer with the TGP-H-060 of 20wt.% hydrophobicity, diffusion layer consists of 2mgcm
-2The PTFE of Vulcan XC-72 and 20wt.%, Catalytic Layer is 6mgcm by the Pt carrying capacity
-2Constitute with 20wt.%Nafion.The electrode of bulk is cut into the small electrode of four 2cm*2cm, with the hot pressing 3 minutes under 130 ℃, 6MPa together of above-mentioned four composite anodes pairing and Nafion117 dielectric film, can obtains four MEA respectively, it is labeled as A, B, C, D accordingly.
6. respectively above-mentioned MEA is assembled into monocell with device shown in Figure 2 and carries out performance test (Fig. 6) and stability test (Fig. 7).The maximum power density of A, B, C, D is respectively 29.0mWcm
-2, 28.1mWcm
-2, 26.8mWcm
-2, 26.0mWcm
-2The carbon nano-tube of different model is made the mass transfer that anode diffusion layer all helps liquid fuel, and the performance of battery and stability are all better.
Claims (6)
1. the manufacture method of the composite anode used of a direct methanol fuel cell, described composite anode is made of supporting layer, diffusion layer and Catalytic Layer, it is characterized in that making step is:
1. the preparation of anode diffusion layer slurry: with the mixture of carbon nano-tube or carbon nano-tube and other material with carbon element in the ultrasonic aqueous solution that is scattered in isopropyl alcohol, add water and the isopropyl alcohol mixture of 0.02-2mL in the mixture of every milligram of carbon nano-tube or carbon nano-tube and other material with carbon element, wherein the volume ratio of water and isopropyl alcohol is controlled at 0.5-3; Carbon nano-tube is single wall, double-walled or the multi-walled carbon nano-tubes of different model and different tube diameters, and material with carbon element is the black activated carbon of business-like XC72 carbon, XC72R carbon, BP2000 or Ketjen; The mass percent of carbon nano-tube and other material with carbon element is controlled in the 100%-20% scope; The mixture mechanical agitation or the ultrasonic agitation of carbon nano-tube or carbon nano-tube and other material with carbon element are promptly obtained finely dispersed slurries A;
2. add polytetrafluoroethylene as binding agent in slurry A, through mechanical agitation or ultrasonic agitation, form uniform slurries B, wherein binding agent accounts for the 10-40% of mass percent of the mixture of carbon nano-tube or carbon nano-tube and other material with carbon element;
3. the preparation of diffusion layer: get carbon paper or carbon cloth supporting layer as combination electrode, the 2. prepared slurries B of step is coated on carbon paper or the carbon cloth equably by brushing or spraying, through high-temperature roasting in 300-350 ℃ of air, nitrogen or argon gas, promptly form the diffusion layer of supporting layer load, wherein the carrying capacity of the mixture of carbon nano-tube or carbon nano-tube and other material with carbon element is controlled to be 0.3-2.5mgcm
-2, polytetrafluoroethylene clinkering at high temperature redistribution enters in the slit of diffusion layer, constitutes a kind of network channel;
4. the preparation of anode catalyst layer slurries: catalyst slurry comprises noble metal catalyst, Nafion resin and dispersant; Wherein catalyst is the black or business-like noble metal catalyst of Pt-Ru/C of Pt-Ru; The Nafion resin accounts for the 15%-20% of Catalytic Layer dry weight, makes dispersant with the mixed liquor of water and isopropyl alcohol, is controlled at 40 ℃ of following ultrasonic agitation of temperature, obtains finely dispersed catalyst slurry;
5. the preparation of anode catalyst layer: the 4. prepared catalyst slurry of step is coated on the diffusion layer that 3. step prepare uniformly, and, eliminates solvent remaining in the Catalytic Layer, then 150 ℃ of following heat treatments through 105 ℃ of oven dry down; The composite anode of electrochemical reaction takes place in it to obtain transmitting liquid fuel and catalysis.
2. the manufacture method of the composite anode of using by the described direct methanol fuel cell of claim 1 is characterized in that during step 1. that the carbon nano-tube carbon nano-tube or the mixture machinery of carbon nano-tube and other material with carbon element or the time of ultrasonic agitation are 0.5-4h.
3. the manufacture method of the composite anode of using by the described direct methanol fuel cell of claim 1 is characterized in that as the carbon paper of supporting layer or the thickness of carbon cloth be 2 μ m-2mm.
4. the manufacture method of the composite anode of using by the described direct methanol fuel cell of claim 1 is characterized in that the volume ratio of water and isopropyl alcohol was 0.2-2 during step 4..
5. the manufacture method of the composite anode of using by the described direct methanol fuel cell of claim 1 is characterized in that drying time is 1-5 hour during step 5., and heat treatment time is 5-15 minute.
6. the manufacture method of the composite anode of using by the described direct methanol fuel cell of claim 1 is characterized in that described diffusion layer is to constitute the network channel structure by carbon nano-tube.
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| CN102610797B (en) * | 2011-12-16 | 2015-01-28 | 北京鼎能开源电池科技股份有限公司 | Manufacturing method of lithium iron phosphate anode |
| CN105789569B (en) * | 2014-12-19 | 2019-02-26 | 中国科学院大连化学物理研究所 | A kind of multilevel structure composite material and its preparation and application |
| CN109301258B (en) * | 2018-09-11 | 2021-08-31 | 先进储能材料国家工程研究中心有限责任公司 | Fuel cell gas diffusion layer and preparation method thereof |
| CN109461940A (en) * | 2018-10-31 | 2019-03-12 | 安徽明天氢能科技股份有限公司 | A kind of novel gas diffusion layers structure and preparation method thereof |
| CN110364743A (en) * | 2019-06-17 | 2019-10-22 | 江苏大学 | A kind of dual-catalysis layer structure electrode and preparation method and its application in high temperature membrane cell |
| WO2022140890A1 (en) * | 2020-12-28 | 2022-07-07 | 深圳烯湾科技有限公司 | Composite carbon nanotube film, preparation method therefor, and layered heating device |
| CN113521880A (en) * | 2021-06-30 | 2021-10-22 | 武汉理工大学 | Photothermal regeneration mask core layer material and preparation method thereof |
| CN113948725B (en) * | 2021-10-20 | 2022-11-15 | 中自环保科技股份有限公司 | Preparation method of dual-functional microporous layer type gas diffusion layer, gas diffusion layer and catalytic electrode |
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