CN102104159A - Novel gas diffusion layer used for fuel cell, preparation and application - Google Patents
Novel gas diffusion layer used for fuel cell, preparation and application Download PDFInfo
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- CN102104159A CN102104159A CN2009102485330A CN200910248533A CN102104159A CN 102104159 A CN102104159 A CN 102104159A CN 2009102485330 A CN2009102485330 A CN 2009102485330A CN 200910248533 A CN200910248533 A CN 200910248533A CN 102104159 A CN102104159 A CN 102104159A
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Abstract
The invention discloses a gas diffusion layer used for a fuel cell and a preparation method thereof. In a microscopic structure, the double-pore distribution of the diffusion layer is formed by nano-scale hydrophilic micropores and micron-sized hydrophobic macropores; and the structure contributes to that the gas diffusion layer has high-efficiency draining and air guiding functions at the same time. In macrocosmic, the porosity and the aperture of the diffusion layer are in anisotropic distribution on the whole of the diffusion layer; the diffusion layer is in asymmetric conical pore distribution in the direction vertical to the plane of the gas diffusion layer; the porosity and the aperture are decreased gradually from outside to inside; the inside is the side on which an attached catalyst layer is connected with the proton exchange membrane on the diffusion layer when in application; the porosity and the aperture of the diffusion layer are in uniform distribution in the direction parallel to the plane of the gas diffusion layer; and the distribution contributes to improving the mass transfer and the electrical conduction efficiency of the diffusion layer. The invention discloses a preparation technology for preparing micro-porous layers in layers by using pore-forming materials with different types and different grain diameters so as to realize the fuel cell gas diffusion layer of which the porosity and the aperture can be controlled accurately.
Description
Technical field
The present invention proposes a kind of new gas diffusion layer and preparation method who is used for fuel cell.The diplopore that constitutes diffusion layer by the hydrophobic macropore of the hydrophilic aperture of nm level and um level on this diffuse layer structure microcosmic distributes, and this structure helps realizing gas diffusion layers draining efficiently and air guide function.The porosity of gas diffusion layers and aperture present the anisotropy distribution on the whole on the macroscopic view, and this distribution more can improve the mass transfer and the electrical efficiency of diffusion layer.Diffusion layer be that asymmetric coniform hole distributes on the direction that is being parallel to proton exchange membrane then is that uniform porous distributes on perpendicular to the direction of proton exchange membrane.Thereby the invention discloses and a kind ofly use variety classes and the layering of particle diameter pore creating material to prepare the gas diffusion layers technology of preparing that microporous layers realizes that porosity and aperture can accurately be controlled.
Background technology
Fuel cell is a kind of electrochemical appliance that chemical energy is converted into electric energy, Proton Exchange Membrane Fuel Cells is wherein a kind of, it is normally by proton exchange membrane, the two sides of film all joins with the Catalytic Layer that contains the catalytic activity component, and the outside of Catalytic Layer is to be the gas diffusion layers of main component by carbon paper or carbon cloth.The outside again of gas diffusion layers is to be equipped with to have the bipolar plates of gas flow channel and satisfactory electrical conductivity, and when fueling and oxidant, the gas diffusion layers with afflux performance conducts the current to external circuit.
As seen its core reaction of fuel cell relates to the gas-liquid-solid three-phase electrocatalytic reaction, and this reaction relates to the transmittance process of three kinds of materials again: the transmission of (1) gas, aqueous water.(2) transmission of reacting gas.(3) migration of electronics.The effect of gas diffusion layers is exactly to realize above-mentioned three kinds of critical components that transmittance process carries out smoothly, the transmission performance of gas diffusion layers is a key factor that influences Proton Exchange Membrane Fuel Cells (PEMFC) performance, especially battery is when low pressure/normal pressure service conditions or high current density discharge, and it is particularly outstanding that the influence of three kinds of material Transfer seems.Above-mentioned preceding two kinds of transmittance processs all are to carry out in certain micro channel, the migration of electronics needs diffusion layer that the good conductive ability is arranged, the factor that influences these three kinds of transmittance processs influences each other again, mutual restriction, therefore to porosity, the pore structure of diffusion layer, the research of pore size distribution is a very important job.Gas diffusion layers is made of three kinds of components usually: 1) diffusion layer skeleton supporter such as carbon paper, carbon cloth, carbon felt or wire netting, 2) conductive fine powder such as carbon dust/graphite powder, 3) hydrophober such as PTFE/PVF2 etc., in order to realize this three kinds of transmittance processs, need be to influencing the various influencing factors of diffusion layer performance, conductive fine powder such as carbon dust, hydrophober such as PTFE/PVF2 content, diffusion layer supporter such as carbon paper type, the porosity of diffusion layer, pore structure, the grade of pore size distribution is done a large amount of systematic researches.
In the research in the past, the hydrophobic gas-diffusion electrode of most of fuel cells uses polytetrafluoroethylene resin (PTFE) as hydrophober and adhesive, and this polymer has high thermal stability and high chemically-resistant degradation property.Yet, PTFE is not dissolved in any known appearance agent, therefore must use with form of suspension, this makes the method for making gas diffusion layers become complicated and difficult, in particular, when PTFE is used as the adhesive of gas diffusion layers, be difficult to structure, porosity and the pore size of control gaseous diffusion layer among the general preparation method.Certainly, the hydrophober that the hydrophobic gas-diffusion electrode also can be used other is Kynoar resin (PVF2) for example, the polyvinylidene fluoride allyl resin, low-molecular-weight fluoropolymers such as poly-inclined to one side fluorine vinyl chloride resin, but the hydrophobicity of these materials and chemical stability and thermal stability are all not as PTFE.
Be coated on diffusion layer skeleton supporter such as the carbon paper after the gas-diffusion electrode of hydrophobic type fuel cell uses PTFE and carbon dust or graphite powder to mix usually, PTFE is as adhesive and hydrophober.U.S. Patent No. 4,847,173 have described PTFE and other polymer mixed with carbon and have prepared the big method of gas diffusion layers.U.S. Patent No. 3,899,354 have described the gaseous diffusion layer method of another kind of preparation carbon and PTFE or other polymer, and it is that the suspension of the mixture of PTFE and carbon is sprayed onto heat-agglomerating then on the carbon paper.U.S. Patent No. 8,697,582 have described another kind of preparation gas-diffusion electrode method, activated carbon and Kynoar resin (PVF2) or other polymer are dissolved in organic solvent obtain mixture, this mixture is coated on the diffusion layer skeleton carbon paper, the diffusion layer of following of low temperature preparation is put in the non-solvent of PVF2 with the wet phase inversion mode formation porous gas diffusion layer of condensing, this method step is a lot, use toxic solvents, unfavorable environmental protection, this method is difficult to pore structure, porosity and the pore size of accurate control gaseous diffusion layer.
Up to the present, the technology of preparing of gas diffusion layers does not also obtain due attention, general patent and article are most of mixed to saying together diffusion layer and Catalytic Layer, and special argumentation diffuse layer structure and preparation technology are seldom arranged.From the conventional as can be known gas diffusion layers preparation method of existing document is that above-mentioned carbon dust and simple mixing of two kinds of components of hydrophober are coated on diffusion layer supporter such as the carbon paper, also there are some researchers in above-mentioned leveling material, to add some pore creating materials, but to three kinds of components constituting gas diffusion layers spatial distribution how, how draining, conduction, three kinds of functions of gas transmission realize also lacking the theory analysis of system.
Summary of the invention
The present invention proposes a kind of gaseous diffusion layer structure efficiently at first theoretically, porosity, pore structure, pore size distribution formation to diffusion layer have been carried out the argumentation of system, division of functionality has been carried out in the diffusion layer diplopore distribution that is made of aperture and macropore, indicated the effect and the structure condition of hydrophilic aperture and hydrophobic macropore.The present invention proposes by using variety classes and the layering of particle diameter pore creating material to prepare the new gas diffusion layer technology of preparing that microporous layers realizes that porosity and aperture and pore structure can accurately be controlled again for realizing that above-mentioned diffuse layer structure has indicated concrete preparation technology.
The purpose of this invention is to provide a kind of fuel cell with the preparation method of gaseous diffusion layer structure and new gas diffusion layer efficiently, is a kind of simple, can business-like gas diffusion layers technology of preparing.
The present invention has innovated gaseous diffusion layer structure, and the diplopore that constitutes this diffusion layer by the hydrophobic macropore of the hydrophilic aperture of nm level and um level on the microcosmic is distributed with to be beneficial to realizes draining efficiently and air guide function; The porosity of gas diffusion layers and aperture present mass transfer and the electrical efficiency that the anisotropy distribution more can improve diffusion layer on the whole on the macroscopic view.It in the diffusion layer asymmetric tapered pore size distribution perpendicular to the gaseous diffusion layer plane, the porosity of diffusion layer and aperture ecto-entad reduce gradually, described inboard is meant adheres to the side that Catalytic Layer connects proton exchange membrane on the diffusion layer when using, the outside is that gas diffusion layers connects flow field one side.Then be that uniform porous distributes on the direction that is parallel to the gaseous diffusion layer plane in the diffusion layer.
Method of the present invention is based on following principle: gas diffusion layers is made up of two kinds of holes, the hydrophilic small aperture scope of nm level is 1-200nm, constitute by hydrophilic conductive nano micro mist, this part is nanometer level microporous to be the aperture of conductive fine powder particle inside, PTFE is because particle diameter can not enter inside, hole greatly, so this part hole water guide: the hydrophobic macropore diameter scope of um level is 0.2um-500um, constitute by conductive nano micro mist and hydrophober, the two mixes, fully contact, under the effect of pore creating material, form specific spatial distribution, remove pore creating material, inner surface and outer surface that hydrophober is evenly distributed on um level macropore form gas port. and conductive fine powder is meant that the B.E.T surface area is the carbon dust of 30-2000m2/g, graphitization carbon dust and metal fine powder.
The present invention comes layering to prepare microporous layers by using variety classes and particle diameter pore creating material, thereby has realized the accurate control of fuel battery gas diffusion layer mesopore rate and aperture and pore structure.
Concrete preparation technology uses pore creating material and the carbon dust and the hydrophober preparation leveling material of variety classes and particle diameter respectively, be coated on diffusion layer supporter such as the carbon paper in batches, remove pore creating material and on perpendicular to the direction of gaseous diffusion layer plane, form asymmetric tapered pore size distribution, the porosity of diffusion layer and aperture ecto-entad reduce gradually, then are that uniform porous distributes on the direction that is parallel to the gaseous diffusion layer plane.
Concrete preparation process is as follows:
A) preparation contains the dispersion suspension liquid of conductive fine powder and hydrophober, the two dry weight part by weight 0.1-1: 0.1-10 adds and the conductive fine powder weight ratio is the pore creating material of 0.1-1: 0.1-10, and the particle diameter of pore creating material is 10nm-500um, ultrasonic agitation is even, makes the leveling material;
B), form regulating course the leveling material dipping of a) preparation be coated on the diffusion layer supporter (for example carbon paper, carbon cloth, carbon felt or wire netting);
C) b) preparation the regulating course drying;
D) twice or the operation of twice above repetition a-c step, layering prepares microporous layers, pore creating material in each leveling material: the part by weight of conductive fine powder reduces gradually, the particle diameter of pore creating material reduces gradually simultaneously, the ratio of conductive fine powder and hydrophober remains unchanged, make the porosity and the aperture of the gas diffusion layers of preparation present anisotropy on the whole, form the porosity of gas diffusion layers and the asymmetric pore size distribution that the aperture increases from inside to outside gradually, described inboard is meant adheres to the side that Catalytic Layer connects proton exchange membrane on the diffusion layer when using, then be that uniform porous distributes on the direction that is parallel to the gaseous diffusion layer plane, thereby guarantee that gas evenly transmits to Catalytic Layer, the thickness of gas diffusion layers is 10-400um, and mean porosities is 10%-90%.
Pore creating material is a polyethylene glycol among the present invention, glycerine, ethylene glycol, vaseline, adipic acid, positive ten pure organic/polymer pore creating materials, ammonium chloride, ammonium oxalate, ammonium formate, ammonium acetate, ammonium nitrate, ammonium carbonate, lithium carbonate, sodium carbonate, potash is inorganic/the organic salt pore creating material. the particle size range of pore creating material is 10nm-500um.
The invention effect
By using variety classes and the layering of particle diameter pore creating material to prepare microporous layers, this technology of preparing can realize the accurate control of porosity, aperture and the pore structure of fuel battery gas diffusion layer in the fuel battery gas diffusion layer preparation process in the present invention.
The present invention makes the gas diffusion layers of preparation form asymmetric tapered pore size distribution on perpendicular to the direction of gaseous diffusion layer plane, the porosity of diffusion layer and aperture ecto-entad reduce gradually, then be that uniform porous distributes on the direction that is parallel to the gaseous diffusion layer plane, this distribution more can improve the mass transfer and the electrical efficiency of diffusion layer.
The gas diffusion layers of the present invention preparation can be used as the Catalytic Layer supporter and prepares catalyst in its orifice surface and forms gas-diffusion electrode (CCS method), also can with proton exchange membrane on have the assembling of Catalytic Layer (CCM method) assembly to form gas diffusion electrode assembly-MEA component application in fuel cell and electrolytic cell.
Description of drawings:
Fig. 1 fuel cell MEA assembles schematic diagram, and the gas diffusion layers of the present invention's preparation is at the MEA outermost layer.
1 is gas diffusion layers among the figure, and 2 is Catalytic Layer, and 3 is proton exchange membrane, and 4 is the MEA outside, and 5 is the MEA inboard.
The structural representation of the gas diffusion layers of Fig. 2 the present invention preparation forms asymmetric pore size distribution on diffusion layer is vertical, the porosity of diffusion layer and aperture ecto-entad reduce gradually, transversely then is that uniform porous distributes in diffusion layer; 6 is conductive carbon powder among the figure, and 7 is the hydrophobic gas port, and 8 is reacting gas, and 9 is hydrophober;
Fig. 3 is the A# and the D# fuel battery performance comparison diagram of different diffusion layer preparations under the atmospheric air condition, the present invention is pore creating material with the ammonium carbonate, adopt the single face levelling process, divide five layers of preparation gas diffusion layers, prepare catalyst in its orifice surface and form gas-diffusion electrode (CCS method), than higher, the draining conduction and the gaseous diffusion performance of diffusion layer are good with kind electrode fuel battery assembled performance.
Fig. 4 is the B# and the D# fuel battery performance comparison diagram of different diffusion layer preparations under the atmospheric air condition, show that the present invention is pore creating material with the ammonium oxalate, adopt two-sided levelling process, the electrode assembled battery performance of dividing five layers of preparation gas diffusion layers and the preparation of CCM method is than higher.
Fig. 5 is fuel cell performance curve figure under the atmospheric air condition, show that the present invention is pore creating material with ammonium chloride, adopt two-sided levelling process, divide five layers of preparation gas diffusion layers, prepare catalyst in its orifice surface and form gas-diffusion electrode (CCS method), the assembled battery performance is relatively good under low/normal pressure service conditions.
Embodiment
Embodiment 1:
With the ammonium carbonate is pore creating material, adopts the single face levelling process, divides five layers of preparation gas diffusion layers, the CCS legal system power backup utmost point.
1. the preparation of diffusion layer
(1) batching and coating for the first time
(a), press 0.8mg carbon dust/cm according to the carbon paper area
2Carbon paper takes by weighing the XC-72 carbon dust and places beaker, presses 70ml ethanol/g carbon dust, adds absolute ethyl alcohol, and sonic oscillation stirred one minute.
(b) it is heavy to press carbon dust: PTFE dry weight=1: 1.5 takes by weighing the hydrophober PTFE emulsion of 30% (wt.).Be added drop-wise in the feed liquid, sonic oscillation stirs 2 minutes feed liquids and is till the prepared Chinese ink shape.
(c) heavy by carbon dust: pore creating material dry weight=take by weighing the ammonium carbonate pore creating material that through 400 mesh sieves divide join in above-mentioned feed liquid at 1: 1.9, sonic oscillation, stirred one minute. after stir finishing feed liquid is placed on bath temperature and is in 95～98 ℃ the hot water and stir, aging 1 minute feed liquid is the flocculation state.Leave standstill to topple in 10 minutes and supernatant liquor, promptly get the feed liquid for preparing.
(d) carbon paper that hydrophobisation was handled lies on the glass plate, the feed liquid for preparing is divided transfer to equably for 2 times on the carbon paper, evenly feed liquid is coated to the carbon paper surface with scraper plate.It is dry to put into 80 degree baking ovens.
(2) coating for the second time
Step (a) above repeating-to step (d), this time step (c) is by carbon dust: the ammonium carbonate pore creating material of pore creating material dry weight=take by weighing through 600 mesh sieves branch at 1: 1.7 joins in the above-mentioned feed liquid, and all the other steps are the same.
(3) coating for the third time
Step (a) above repeating is to step (d), and this time step (c) is by carbon dust: the ammonium carbonate pore creating material of pore creating material dry weight=take by weighing through 800 mesh sieves branch at 1: 1.5 joins in the above-mentioned feed liquid, and all the other steps are the same.
(4) the 4th coatings
Step (a) above repeating is to step (d), and this time step (c) is by carbon dust: the ammonium carbonate pore creating material of pore creating material dry weight=take by weighing through 1000 mesh sieves branch at 1: 1.3 joins in the above-mentioned feed liquid, and all the other steps are the same.
(5) the 5th coatings
Step (a) above repeating is to step (d), and this time step (c) is by carbon dust: the ammonium carbonate pore creating material of pore creating material dry weight=take by weighing through 1200 mesh sieves branch at 1: 1.1 joins in the above-mentioned feed liquid, and all the other steps are the same.
2. the roasting of diffusion layer
(1) carbon paper that will coat diffusion layer is placed on 0.5hr in 100 ℃ of baking ovens, and the record of weighing under the room temperature as weight before the roasting, is sent into the oven dry kiln roasting then.Be warming up to 340 ± 10 ℃, constant temperature 30～40 minutes.
(2) cut off the power supply of drying oven, treat that temperature is reduced to below 100 ℃ workpiece is taken out.
(3) diffusion layer that roasting is good is weighed, and record is as weight after the roasting.
3. the preparation of Catalytic Layer
The gas diffusion layers for preparing prepares catalyst according to the known Catalytic Layer preparation method of document in its orifice surface and forms gas-diffusion electrode (CCS method).
Two CCS method electrode holders are at proton exchange membrane two Side assembling MEA, and this MEA is numbered A#, is put into the test of fuel cell evaluating apparatus.
Embodiment 2:
With the ammonium oxalate is pore creating material, adopts the single face levelling process, divides five layers of preparation gas diffusion layers, the CCM legal system power backup utmost point.
The preparation of diffusion layer is with embodiment 1, replace ammonium carbonate as pore creating material with ammonium oxalate during preparation gas diffusion layers leveling material, the CCS method is adopted in the preparation of Catalytic Layer, prepare catalyst according to the known method of document at proton exchange membrane two Side and form electrode, two gas diffusion layers that prepare are clipped in CCS method electrode two Side assembling MEA, this MEA is numbered B#, is put into the test of fuel cell evaluating apparatus.
Embodiment 3:
With ammonium chloride is pore creating material, adopts the single face levelling process, divides five layers of preparation gas diffusion layers, the CCS legal system power backup utmost point.
The preparation method of diffusion layer and Catalytic Layer is with embodiment 1, and difference is that pore creating material changes ammonium chloride into.
Two CCS method electrode holders that prepare are at proton exchange membrane two Side assembling MEA, and this MEA is numbered C#, are put into the test of fuel cell evaluating apparatus.
Comparative Examples:
Prepare gas diffusion layers according to the document known method, adopt, be numbered D# with above-mentioned three embodiment the same terms assembling MEA.
It is as follows that fuel cell is estimated the concrete operations parameter: the Water Tank with Temp.-controlled temperature is 70 ℃, and battery temperature is 70 ℃, and the humidifier temperature is 68-70 ℃, adopts normal pressure (ambient pressure) operating condition, and hydrogen and air are strict regulates control by stoichiometric proportion; The hydrogen stoichiometric proportion is 1.17, and the air stoichiometry ratio is 2.5.
Claims (7)
1. high performance gas diffuse layer structure that is used for fuel cell, it is characterized in that: this diffusion layer is distributed by the diplopore that the hydrophobic macropore of the hydrophilic aperture of nm level and um level constitutes diffusion layer on the microstructure, and the gas diffusion layers of this structure possesses draining efficiently and air guide function simultaneously; The porosity of diffusion layer and aperture present the anisotropy distribution on the whole at diffusion layer on the macroscopic view, promptly, diffusion layer presents asymmetric tapered pore size distribution structure on perpendicular to the direction of gaseous diffusion layer plane, the porosity of diffusion layer and aperture ecto-entad reduce gradually, and described inboard is meant adheres to the side that Catalytic Layer connects proton exchange membrane on the diffusion layer when using; The porosity of diffusion layer and aperture then are even distributions on the direction that is parallel to the gaseous diffusion layer plane, and this being distributed with is beneficial to mass transfer and the electrical efficiency that improves diffusion layer.
2. gaseous diffusion layer structure as claimed in claim 1, it is characterized in that: the hydrophilic small aperture scope of nm level is 1-200nm, constitute by hydrophilic conductive nano micro mist, this part is nanometer level microporous to be the aperture of conductive fine powder particle inside, hydrophober is because particle diameter can not enter inside, hole greatly, so this part hole is used for draining: the hydrophobic macropore diameter scope of um level is 0.2um-500um, constitute by conductive nano micro mist and hydrophober, the two mixes, fully contact, form specific spatial distribution under the effect of pore creating material, remove pore creating material, inner surface and outer surface that hydrophober is evenly distributed on um level macropore form gas port.
3. the preparation method of the described diffuse layer structure of claim 1 is characterized in that: concrete preparation process is as follows,
A) preparation contains the dispersion suspension liquid of conductive fine powder and hydrophober, the two dry weight part by weight 0.1-1: 0.1-10 adds and the conductive fine powder weight ratio is the pore creating material of 0.1-1: 0.1-10, and the particle diameter of pore creating material is 10nm-500um, ultrasonic agitation is even, makes the leveling material;
B), form regulating course the leveling material dipping of a) preparation be coated on the diffusion layer supporter (for example carbon paper, carbon cloth, carbon felt or wire netting);
C) b) preparation the regulating course drying;
D) twice or the operation of twice above repetition a-c step, layering prepares microporous layers, pore creating material in each leveling material: the part by weight of conductive fine powder reduces gradually, the particle diameter of pore creating material reduces gradually simultaneously, the ratio of conductive fine powder and hydrophober remains unchanged, make the porosity and the aperture of the gas diffusion layers of preparation present anisotropy on the whole, form the porosity of gas diffusion layers and the asymmetric pore size distribution that the aperture increases from inside to outside gradually, described inboard is meant adheres to the side that Catalytic Layer connects proton exchange membrane on the diffusion layer when using, then be that uniform porous distributes on the direction that is parallel to the gaseous diffusion layer plane, thereby guarantee that gas evenly transmits to Catalytic Layer, the thickness of gas diffusion layers is 10-400um, and mean porosities is 10%-90%.
4. preparation method as claimed in claim 3 is characterized in that: described conductive fine powder is meant that the B.E.T surface area is carbon dust, graphitization carbon dust and the metal fine powder of 30-2000m2/g.
5. preparation method as claimed in claim 3, it is characterized in that: hydrophober is meant polyfluorinated ethylene resin PTFE, polyvinylidene fluoride resin PVF2, poly(perfluoropropene) resin, poly-inclined to one side fluorine allyl resin, polyvinylidene fluoride allyl resin or low-molecular-weight fluoropolymer, hydrophober can be one or more mixtures of above-mentioned substance, hydrophober can be water-based dispersion suspension liquid, also can be the polymer micro mist, hydrophober and conductive fine powder weight ratio be 1: 0.1-10.
6. preparation method as claimed in claim 3 is characterized in that: pore creating material is a polyethylene glycol, glycerine, ethylene glycol, vaseline, adipic acid, positive ten pure organic/polymer pore creating materials, ammonium chloride, ammonium oxalate, ammonium formate, ammonium acetate, ammonium nitrate, ammonium carbonate, lithium carbonate, sodium carbonate, potash is inorganic/one or more mixtures in the organic salt, and the particle size range of pore creating material is 10nm-500um, the weight ratio of pore creating material and conductive fine powder is 1: 0.1-100.
7. the application of each described gas diffusion layers among the claim 1-7, it is characterized in that: this gas diffusion layers is as the Catalytic Layer supporter, and form gas-diffusion electrode (CCS method) at the surface preparation catalyst of its aperture side, perhaps with proton exchange membrane on catalyst-loaded (CCM method) assembly assembling of forming form gas diffusion electrode assembly-MEA; This electrode or MEA are used for fuel cell or electrolytic cell.
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