CN100341180C - Self humidifying film electrode and its preparing method - Google Patents
Self humidifying film electrode and its preparing method Download PDFInfo
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- CN100341180C CN100341180C CNB2005100375751A CN200510037575A CN100341180C CN 100341180 C CN100341180 C CN 100341180C CN B2005100375751 A CNB2005100375751 A CN B2005100375751A CN 200510037575 A CN200510037575 A CN 200510037575A CN 100341180 C CN100341180 C CN 100341180C
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Abstract
The present invention discloses a self-humidifying film electrode and a preparing method thereof. The preparing method is characterized in that a proton exchanging membrane is preprocessed, carbon carrying platinum catalyst, perfluoro-sulfonic-acid polymer, hydrotropic substance and low boiling point solvent are mixed and coated on one side of the proton exchanging membrane to be dried, and then a hydrophilic hydrogen electrode is obtained; carbon carrying platinum catalyst, perfluoro-sulfonic-acid polymer, hydrophobic substance and low boiling point solvent are mixed and coated on the other side of the proton exchanging membrane to be dried, and then a hydrophobic oxygen electrode is obtained; the automatic humidifying membrane electrode is obtained by adhering two carbon paper sheets and the proton exchanging membrane. The preparing method has the advantages of simplicity, easy operation and low cost. The self-humidifying film electrode has the advantages of small volume and light weight, and can realize the self-humidifying function without using complex gas flow fields. The self-humidifying film electrode simplifies the designing technology and the manufacture technology of a fuel cell system and increases the gravimetric specific power and the volume specific power. A single cell assembled by the membrane electrode has good electric performance. The self-humidifying film electrode avoids the submerging phenomenon and increases the electric performance of fuel cells worked in environment with high current density.
Description
Technical field
The present invention relates to the fuel cell technology field, specifically be meant a kind of preparation method of self-humidifying membrane electrode.
Background technology
Proton Exchange Membrane Fuel Cells (PEMFC) is after alkaline fuel cell (AFC), phosphoric acid fuel cell (PAFC), molten carbonate fuel cell (MCFC) and Solid Oxide Fuel Cell (SOFC), developing rapidly the 5th generation fuel cell.But PEMFC has high power density, high-energy conversion efficiency cold-starting, advantage such as environmentally friendly, is to promise to be power source pollution-free, the zero discharge electric car most.Proton exchange membrane (PEM) is one of core component of PEMFC.It with general chemical power source in the barrier film that uses be very different.It is a kind of selective permeation film of densification, is again the substrate of cell electrolyte (being used to transmit proton) and electrode active material eelctro-catalyst.PEMFC generally adopts the perfluorinated sulfonic acid polymer proton exchange membrane as solid electrolyte.Its electrical property is subjected to the highly significant that influences of proton exchange membrane conductivity.
General proton exchange membrane, as perfluorinated sulfonic resin is the Nafion film, the conduction that needs water to keep the conductivity proton of film when being used for PEMFC, when the hydrone of each sulfonate radical combination in the Nafion film was less than 4, proton exchange membrane just almost can't proton conducting; When the moisture in the membrane electrode is too high, can cause the catalyst in the electrode to be flooded stain again, lose reactivity.In the prior art, normally the reaction gas that enters pile being carried out humidification handles.General outer humidification mode or the interior humidification mode of adopting of humidification.Outer humidification mode is the outside that humidification system is placed on pile, and humidification system is what to separate with pile.This mode can keep the well-hydrated state of pile inner membrance effectively, but has following shortcoming: (1) has increased the volume and weight of fuel cell system, and system relatively disperses, and the gravimetric specific power and the volumetric specific power of pile are lower; (2) start fast or load when changing significantly suddenly when battery, the humidification response often lags behind, can not be synchronous with it in time.Interior humidification mode mainly is applied to the inside of pile, and its humidification auxiliary system and pile constitute an integral body.This mode specifically is the humidification that is used as pile in one section of pile indoor design " false battery " specially, and the aqua storage tank as heating reaches the purpose of reacting gas being carried out humidification.The humidification mode can solve the humidification problem of PEM effectively in this, but because this humidification auxiliary system has occupied suitable volume and weight in pile, also to provide the pure water circulatory system or heating system, and pile packaging technology and Sealing Technology that need be higher, thereby increased the volume and weight of pile system, but also increased technical difficulty.
Self-humidification just is meant a kind of by improving the structure of pile inside, makes it not need can keep by means of external equipment the technology of voltaic pile normal work.At present more about document patent from humidification, No. 6207312 patents of invention of the U.S. disclose the self-humidifying method in a kind of snake type flow field, promptly on bipolar plates, process a kind of multichannel snake type flow field, gas is motion upper and lower, back and forth in snake type smoothness, makes on gas flow direction the generation water anode transmission of quickening negative electrode.The technological operation of this technology is simple, but the electrical property of pile is relatively poor.No. 5766787 patents of invention of the U.S. disclose a kind of with Pt particulate and SiO
2Or TiO
2Etc. the hydrophilic oxide-doped technology of in proton exchange membrane, preparing from humidification three in one membreane electrode (MEA).The Pt particulate has stoped hydrogen, the carrier of oxygen cross-diffusion in film effectively, and the water that utilizes hydrogen, oxygen to be generated in the electrochemical reaction process in film comes moistening MEA.Yet the Pt microparticulate in this MEA film is inhomogeneous, can form local electron channel, thereby causes pile generation self-discharge phenomenon and pile was lost efficacy.In addition, No. 5318863 patents of invention of the U.S. disclose generation water anode back-diffusion that the ultra-thin proton exchange membrane of a kind of usefulness increases the pile negative electrode and have prepared method from humidification MEA.Yet, though this technology has strengthened the retrodiffusion of negative electrode water, cause film to break easily, thereby increased the chance of hydrogen, carrier of oxygen cross-diffusion, shortened the useful life of pile.
Summary of the invention
Purpose of the present invention is exactly in order to solve above-mentioned the deficiencies in the prior art part, and a kind of preparation method of self-humidifying membrane electrode is provided.This self-humidifying membrane electrode can be realized from humidification, and simplify the design and the manufacturing process of fuel cell system.
Purpose of the present invention realizes by following technical solution: the preparation method of described a kind of self-humidifying membrane electrode comprises following step and process conditions:
The first step is successively placed on proton exchange membrane in sulfuric acid solution that mass percent concentration is 3～5% hydrogen peroxide, distilled water, 0.5～1.0mol/L and the distilled water and respectively boiled 0.5～1 hour, and film is carried out preliminary treatment;
Second step became ink shape by 10: 1～4: 0.5～3: 20～200 mass ratio with the supersonic oscillations dispersing and mixing with carbon supported platinum catalyst, perfluorinated sulfonic acid polymer (Nafion), hydroaropic substance and low boiling point solvent, be coated in a side of proton exchange membrane, the carrying capacity of Pt is controlled at 0.1～1.0mg/cm
2, then proton exchange membrane was dried 20～60 minutes down in 60～100 ℃, make hydrophilic hydrogen electrode;
The 3rd step evenly mixed carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, lyophobic dust and low boiling point solvent by 10: 1～4: 1～5: 20～200 mass ratio, was coated in the opposite side of proton exchange membrane, and the carrying capacity of Pt is controlled at 0.1～1.0mg/cm
2, then proton exchange membrane was dried 20～60 minutes down in 60～100 ℃, make the oxygen electrode of hydrophobicity;
The 4th step was fitted into self-humidifying membrane electrode with above-mentioned being coated with the hydrophily hydrogen electrode with the proton exchange membrane of hydrophobicity oxygen electrode with two carbon papers as gas diffusion layers that preliminary treatment is good.
In order to realize the present invention better, described proton exchange membrane is Nafion112, Nafion115 and the Nafion117 film that U.S. Dupont company produces; Described perfluorinated sulfonic acid polymer is that mass percent concentration is 5% Nafion solution; The weight percent content of Pt is 20% in the described carbon supported platinum catalyst; Described solvent is one or more mixtures in distilled water, ethanol, isopropyl alcohol, the acetonitrile; Described hydroaropic substance comprises perfluorinated sulfonic acid polymer, glycerine, succinic acid, propane sulfonic acid, amino acid, SiO
2, TiO
2In one or more mixtures, wherein perfluorinated sulfonic acid polymer is that mass percent concentration is 5% Nafion solution; Described lyophobic dust comprises polysiloxanes, polyethylene and polytetrafluoroethylene (PTFE).
A kind of self-humidifying membrane electrode of the present invention forms by method for preparing exactly.
The present invention compared with prior art has the following advantages and beneficial effect:
1, the preparation method of self-humidifying membrane electrode of the present invention is simple, and is cheap for manufacturing cost.
2, self-humidifying membrane electrode of the present invention need not to adopt complicated gas flowfield, just can realize having simplified the design and the manufacturing process of fuel cell system from humidification.
3, the volume of self-humidifying membrane electrode of the present invention is little, in light weight, does not need just can keep the moistening of pile inner membrance by the humidification auxiliary system, keeps the normal operation and the superperformance of pile, has improved the gravimetric specific power and the volumetric specific power of fuel cell system.
4, the self-humidifying membrane electrode of the present invention monocell good electrical property of assembling has been avoided the generation of electrode water logging phenomenon, has improved the electrical property that fuel cell is worked under high current density.Under low current density its electrical property and outside the poor electrical performance of humidification pile few, and its electrical property is better than the electrical property of the fuel cell of outer humidification under the high current density.
Description of drawings
Fig. 1 is the volt-ampere characteristic figure of fuel cell among the embodiment one;
Fig. 2 is the comparison diagram of fuel cell and outer humidifying fuel cell battery polarization curve among the embodiment two;
Fig. 3 is the comparison diagram of fuel cell polarization curve among embodiment one and the embodiment five.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment one
The first step is successively placed on the Nafion115 film in sulfuric acid solution that mass percent concentration is 5% hydrogen peroxide, distilled water, 0.5mol/L and the distilled water and respectively boiled 0.5 hour, film is carried out preliminary treatment, pretreated Nafion115 film is fixed with four stainless steel clamp, in case film shrinks in air or curl;
Second step is with carbon supported platinum catalyst (U.S. E-TEK company product, down together), perfluorinated sulfonic acid polymer (U.S. Dupont company product quality percent concentration is 5% Nafion solution, down together), SiO
2, isopropyl alcohol and distilled water mixture by 10: 2: 1: 100 mass ratio evenly mixes, and becomes the ink shape with the supersonic oscillations dispersing and mixing, is coated in a side of film, and the carrying capacity of Pt is 0.6mg/cm
2, then this film being placed in the baking oven, baking is 40 minutes under 80 ℃ temperature, has just made hydrophilic hydrogen electrode;
The 3rd step with the mixture of carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, polytetrafluoroethylene (PTFE), isopropyl alcohol and water by 10: 2: 2.5: 100 mass ratio evenly mixes, and is coated in the opposite side of film, and the carrying capacity of Pt is 0.6mg/cm
2, then this film being placed in the baking oven, baking is 40 minutes under 80 ℃ temperature, has just made the oxygen electrode of hydrophobicity;
Carbon paper (U.S. E-TEK company product, down together) and the above-mentioned film that be coated with hydrophily hydrogen electrode and hydrophobicity oxygen electrode of the 4th step with two band diffusion layers that preliminary treatment is good is assembled into self-humidifying membrane electrode (MEA).
Above-mentioned self-humidifying membrane electrode without hot pressing directly and bipolar plates be assembled into monocell, measure the chemical property of this monocell.Fuel gas adopts hydrogen, and oxidant adopts oxygen, works under the condition of liquid cooling.The voltage-current characteristic of battery as shown in Figure 1.The result shows, the electrical property excellence of the self-humidifying membrane electrode of the present invention's preparation, can be outside not adding operate as normal under the condition of humidification system and interior humidification system.The monocell electrical property that the membrane electrode of being done under above-mentioned volt-ampere curve and the hot pressing condition is assembled contrasts, as shown in Figure 3.The result shows, has better electrical property without the membrane electrode of hot pressing.This is because catalyst pulp directly contacts with film, has reduced the concentration gradient of water, and the water anode that more helps the negative electrode generation moves.Membrane electrode is without hot pressing, and it is more intact that the space that forms owing to solvent evaporates in the catalyst keeps, and the voidage height makes the specific area of catalyst bigger, and electrocatalysis characteristic is better.
Embodiment two
The first step is successively placed on the Nafion112 film in sulfuric acid solution that mass percent concentration is 5% hydrogen peroxide, distilled water, 0.8mol/L and the distilled water and respectively boiled 45 minutes, film is carried out preliminary treatment, pretreated proton exchange membrane is fixed with four stainless steel clamp, in case film shrinks in air or curl;
Second step is with carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, TiO
2With the mixture of the mixture of glycerine, ethanol and distilled water by 10: 3: 2: 150 mass ratio evenly mixes, and becomes the ink shape with the supersonic oscillations dispersing and mixing, is coated in a side of film, and the carrying capacity of Pt is 0.4mg/cm
2, then this film being placed in the baking oven, baking is 30 minutes under 100 ℃ temperature, has just made hydrophilic hydrogen electrode;
The 3rd step with the mixture of carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, PTFE, ethanol and distilled water by 10: 3: 4: 150 mass ratio evenly mixes, and is coated in the opposite side of film, and the Pt carrying capacity is 0.4mg/cm
2, then this film is placed in the baking oven, under 100 ℃ temperature, dry by the fire 30min, just made the oxygen electrode of hydrophobicity;
The 4th step was assembled into MEA with the carbon paper of diffusion layer and the film that is coated with hydrophily hydrogen electrode and hydrophobicity oxygen electrode with two.
With above-mentioned MEA without hot pressing directly and bipolar plates be assembled into monocell, measure the chemical property of this monocell.Fuel gas adopts hydrogen, and oxidant adopts oxygen, and battery is worked under the condition of air cooling.The voltage-current characteristic of battery as shown in Figure 2.The result shows that the battery that the prepared membrane electrode of the present invention is assembled is few with the poor electrical performance of battery under low current density that outer humidifying film electrode is assembled, and the former performance is better than the latter under high current density.
Embodiment three
The first step is successively placed on the Nafion117 film in sulfuric acid solution that mass percent concentration is 3% hydrogen peroxide, distilled water, 1.0mol/L and the distilled water and respectively boiled 1 hour, film is carried out preliminary treatment, pretreated proton exchange membrane film is fixed with four stainless steel clamp, in case film shrinks in air or curl;
Second step with the mixture of carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, succinic acid and propane sulfonic acid, acetonitrile by 10: 4: 3: 200 mass ratio evenly mixes, and is mixed into the ink shape with supersonic oscillations, is coated in a side of film, and the Pt carrying capacity is 1.0mg/cm
2, then this film being placed in the baking oven, baking is 60 minutes under 60 ℃ temperature, has just made hydrophilic hydrogen electrode;
The 3rd the step with carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, polysiloxanes, acetonitrile by 10: 4: 5: 200 mass ratio evenly mixes, and is coated in the opposite side of film, and the carrying capacity of Pt is 1.0mg/cm
2, then this film being placed in the baking oven, baking is 60 minutes under 60 ℃ temperature, has just made the oxygen electrode of hydrophobicity;
Carbon paper and the above-mentioned film that be coated with hydrophily hydrogen electrode and hydrophobicity oxygen electrode of the 4th step with two band diffusion layers is assembled into MEA, is assembled into monocell without hot pressing, measures the chemical property of this monocell.The result shows that battery can operate as normal.
Embodiment four
The first step is successively placed on the Nafion115 film and respectively boils 40min in sulfuric acid solution that mass percent concentration is 4% hydrogen peroxide, distilled water, 1.0mol/L and the distilled water film is carried out preliminary treatment, pretreated Nafion film is fixed with four stainless steel clamp, in case film curls in air;
Second step with the mixture of the mixture of carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, amino acid and succinic acid, isopropyl alcohol and water by 10: 1: 0.5: 20 mass ratio evenly mixes, be mixed into the ink shape with supersonic oscillations, be coated in a side of film, the Pt carrying capacity is 0.1mg/cm
2, then this film being placed in the baking oven, baking is 20 minutes under 90 ℃ temperature, has just made hydrophilic hydrogen electrode;
The 3rd step with the mixture of the mixture of carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, polyethylene and PTFE, isopropyl alcohol and water by 10: 1: 0.5: 20 mass ratio evenly mixes, and is coated in the opposite side of film, and the Pt carrying capacity is 0.1mg/cm
2, then this film being placed in the baking oven, baking is 20 minutes under 90 ℃ temperature, just makes the oxygen electrode of hydrophobicity;
Carbon paper and the above-mentioned film that be coated with hydrophily hydrogen electrode and hydrophobicity oxygen electrode of the 4th step with two band diffusion layers is assembled into MEA, is assembled into monocell without hot pressing, measures the chemical property of this monocell.The result shows that battery can operate as normal.
As mentioned above, can realize the present invention preferably.
Claims (8)
1, a kind of preparation method of self-humidifying membrane electrode is characterized in that, comprises following step and process conditions:
The first step is successively placed on proton exchange membrane in sulfuric acid solution that mass percent concentration is 3～5% hydrogen peroxide, distilled water, 0.5～1.0mol/L and the distilled water and respectively boiled 0.5～1 hour, and film is carried out preliminary treatment;
Second step became ink shape by 10: 1～4: 0.5～3: 20～200 mass ratio with the supersonic oscillations dispersing and mixing with carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, hydroaropic substance and low boiling point solvent, be coated in a side of proton exchange membrane, the carrying capacity of Pt is controlled at 0.1～1.0mg/cm
2, then proton exchange membrane was dried 20～60 minutes down in 60～100 ℃, make hydrophilic hydrogen electrode;
The 3rd step evenly mixed carbon supported platinum catalyst, perfluorinated sulfonic acid polymer, lyophobic dust and low boiling point solvent by 10: 1～4: 1～5: 20～200 mass ratio, was coated in the opposite side of proton exchange membrane, and the carrying capacity of Pt is controlled at 0.1～1.0mg/cm
2, then proton exchange membrane was dried 20～60 minutes down in 60～100 ℃, make the oxygen electrode of hydrophobicity;
The 4th step was fitted into self-humidifying membrane electrode with above-mentioned being coated with the hydrophily hydrogen electrode with the proton exchange membrane of hydrophobicity oxygen electrode with two carbon papers as gas diffusion layers that preliminary treatment is good.
According to the preparation method of the described a kind of self-humidifying membrane electrode of claim 1, it is characterized in that 2, described proton exchange membrane is Nafion112, Nafion115 and the Nafion117 film that U.S. Dupont company produces.
According to the preparation method of the described a kind of self-humidifying membrane electrode of claim 1, it is characterized in that 3, described perfluorinated sulfonic acid polymer is that mass percent concentration is 5% Nafion solution.
According to the preparation method of the described a kind of self-humidifying membrane electrode of claim 1, it is characterized in that 4, the weight percent content of Pt is 20% in the described carbon supported platinum catalyst.
According to the preparation method of the described a kind of self-humidifying membrane electrode of claim 1, it is characterized in that 5, described solvent is one or more mixtures in distilled water, ethanol, isopropyl alcohol, the acetonitrile.
According to the preparation method of the described a kind of self-humidifying membrane electrode of claim 1, it is characterized in that 6, described hydroaropic substance comprises perfluorinated sulfonic acid polymer, glycerine, succinic acid, propane sulfonic acid, amino acid, SiO
2, TiO
2In one or more mixtures.
According to the preparation method of the described a kind of self-humidifying membrane electrode of claim 6, it is characterized in that 7, described perfluorinated sulfonic acid polymer is that mass percent concentration is 5% Nafion solution.
According to the preparation method of the described a kind of self-humidifying membrane electrode of claim 1, it is characterized in that 8, described lyophobic dust comprises polysiloxanes, polyethylene and polytetrafluoroethylene.
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Families Citing this family (9)
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| KR100874112B1 (en) | 2007-06-25 | 2008-12-15 | 한화석유화학 주식회사 | Process for preparing of a catalyst solution for fuel cell and a membrane electrode assembly using the same |
| CN101435174B (en) * | 2007-11-14 | 2010-12-22 | 上海河森电气有限公司 | Method for making high performance carbon paper special for fuel cell |
| CN101783409B (en) * | 2010-02-04 | 2012-08-22 | 上海交通大学 | Preparation method of membrane electrode with negative pole being carbon-carried transition metal chelate catalytic agent |
| CN102437343A (en) * | 2011-11-17 | 2012-05-02 | 华南理工大学 | Membrane electrode containing hydrophilic high polymer in anode catalytic layer and preparation method thereof |
| CN111261879A (en) * | 2020-01-23 | 2020-06-09 | 同济大学 | Catalyst slurry containing dispersing aid, catalyst layer prepared from catalyst slurry and fuel cell electrode |
| 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 |
| CN112786937B (en) * | 2021-01-27 | 2022-03-15 | 浙江高成绿能科技有限公司 | Fuel cell membrane electrode and preparation method thereof |
| CN113504285A (en) * | 2021-07-09 | 2021-10-15 | 杭州麦乐克科技股份有限公司 | Preparation method of formaldehyde electrochemical sensor membrane electrode |
| CN113937303B (en) * | 2021-10-14 | 2023-07-21 | 中汽创智科技有限公司 | Catalytic layer electrode composition, catalytic layer electrode containing same and membrane electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001118587A (en) * | 1999-10-15 | 2001-04-27 | Toshiba Corp | Solid polymer type fuel cell and method for operating the same |
| CN1477728A (en) * | 2003-07-11 | 2004-02-25 | 清华大学 | Solid polymer fuel cell unit and its cell stack |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001118587A (en) * | 1999-10-15 | 2001-04-27 | Toshiba Corp | Solid polymer type fuel cell and method for operating the same |
| CN1477728A (en) * | 2003-07-11 | 2004-02-25 | 清华大学 | Solid polymer fuel cell unit and its cell stack |
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