CN103882467B - A kind of preparation method of SPE water electrolysis part cocrystallization Catalytic Layer coat film - Google Patents
A kind of preparation method of SPE water electrolysis part cocrystallization Catalytic Layer coat film Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of part cocrystallization Catalytic Layer coat film for SPE water electrolytic cell.The step of this preparation method is: use solvent flashing method to prepare the solid polymer dielectric film of partially crystallizable；Decorative layer and Catalytic Layer is adhered to successively on gained film surface；The solid polymer dielectric film being coated with decorative layer and Catalytic Layer carries out cocrystallization process.The present invention can be prevented effectively from film Fragmentation Phenomena in cocrystallization Catalytic Layer coat film preparation process, increase the adhesion of Catalytic Layer and solid polymer dielectric film, strengthen Catalytic Layer hydrophobicity, reduce water electrolysis voltage, improve SPE water electrolysis stability, extend the SPE water electrolytic cell life-span.
Description
Technical field
The present invention relates to solid polymer electrolyte (SPE) water electrolysis field, the preparation method of a kind of SPE water electrolysis part cocrystallization Catalytic Layer coat film.
Background technology
Along with constantly consuming of conventional fossil fuel and being on the rise of environmental problem, the regenerative resource of cleaning such as solar energy and wind energy etc. are by the highest attention of people.But these energy can not exist on steady and continuous ground, is in use required to carry out energy storage.Hydrogen Energy cleans as one, efficient energy carrier, becomes countries in the world government and the study hotspot of Corporation R & D mechanism.Water electrolysis is the technology of a kind of highly developed preparation High Purity Hydrogen at present.Compared with traditional alkaline water electrolytic, solid polymer water electrolysis, owing to having environmental friendliness, producing that hydrogen purity is high, energy efficiency high, be easily maintained and the advantage such as safe and reliable, receives the highest attention of people.
Membrane electrode is the place that SPE water electrolysis reaction occurs, and is its core component.The preparation method of tradition MEA can be divided into two big classes, and a class is GDE method, and another kind of is CCM method.The advantages such as compared with GDE, it is low that CCM has catalyst loading, and Catalytic Layer is thin, and hydrophilic is strong, therefore main employing CCM method in current SPE water electrolysis.But hydrophilic stronger for CCM causes the gas produced in electrolytic process easily to be assembled in Catalytic Layer, reduces catalyst utilization, makes decomposition voltage raise, affect decomposition voltage stability.And, due to the working environment (work long hours in water environment and Catalytic Layer is washed away by a large amount of product gas) that CCM Catalytic Layer is special with the difference of the swellability of film and SPE water electrolysis, all it is easily caused the stripping of Catalytic Layer and film, thus increase the contact resistance between Catalytic Layer and film, reduce proton conduction property, affect the life-span of SPE water electrolytic cell.
Patent CN102260877A uses the method for sand papering to be roughened film, thus reaches the purpose increasing Catalytic Layer with membranous layer binding force.Although this method can increase the adhesion of Catalytic Layer and film layer to a certain extent, but can greatly reduce the mechanical performance of film, affect the life-span of electrolyzer.
Patent CN102386420A improves the stripping problem of Catalytic Layer and film layer by adding catalysis glue layer between film and Catalytic Layer.Wherein catalysis glue layer is made up of the solid polymer electrolyte of 60% ~ 80% and the catalyst of 20% ~ 40%, and this relatively low catalyst ratio causes catalyst utilization to reduce, thus reduces battery performance, increases battery cost.
Patent JP5538934 uses chemical deposition, makes catalyst direct-reduction be deposited on inside film.Although the Catalytic Layer that this method obtains is firmly combined with dielectric film, interface resistance is low, but catalyst granules is relatively big, causes catalyst utilization low, and deposits to catalyst film within and easily cause film short-circuit.
Patent CN101008087A, by directly adhering to Catalytic Layer in indefinite form solid polymer dielectric film both sides, then carries out the method that membrane electrode is prepared in cocrystallization process, the stripping lamination problem can being effectively improved between film and electrode.But due to the poor mechanical properties of indefinite form solid polymer dielectric film, easily cause film to crush during preparation attachment Catalytic Layer；And the granule in Catalytic Layer is easily accessible inside film, film is caused to be susceptible to short circuit.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of SPE water electrolysis part cocrystallization Catalytic Layer coat film (CCM), solve Catalytic Layer and the breakable problem of film in gas transmission property difference in the stripping of film layer and Catalytic Layer and cocrystallization CCM preparation process in tradition CCM, reduce decomposition voltage, improve stability, extend cell life.
The present invention is achieved through the following technical solutions:
Described CCM includes a kind of solid polymer dielectric film and the decorative layer on adjacent films two sides and Catalytic Layer.Casting method, the tape casting or spraying process etc. is used to prepare the solid polymer dielectric film of partially crystallizable；Spraying process, silk screen print method, transfer printing etc. is used to be attached to described polymer dielectric film two sides, obtain decorative layer by solid polymer electrolyte solution；Use spraying process, silk screen print method, transfer printing etc. that anode and cathode inks are attached to the decorative layer surface on film two sides respectively, obtain CCM；Above-mentioned CCM is carried out crystallization treatment, forming part cocrystallization CCM.
Described polymer dielectric is perfluorinated sulfonic resin, sulfonated polyether-ether-ketone or SPSF；Described solid polymer electrolyte solution includes solid polymer electrolyte and low boiling point solvent, and its volume ratio is 1:10 ~ 1:1；Described catalyst pulp includes catalyst, polyelectrolyte solution and low boiling point solvent, and wherein polymer is about 1:1 ~ 10:1 with catalyst weight than the volume ratio for 1:9 ~ 1:1, low boiling point solvent and polyelectrolyte solution.Low boiling point solvent is deionized water, ethanol, isopropanol etc..Catalyst includes containing Pt(or Ir) granule.Containing Pt(or Ir) granule includes loaded Pt(or Ir) granule.
The present invention provides the preparation method of a kind of CCM.The method includes following step:
(1) casting method, the tape casting or spraying process etc. are used to prepare indefinite form solid polymer dielectric film at 40-100 DEG C；Described polymer dielectric film and decorative layer are perfluorinated sulfonic resin, sulfonated polyether-ether-ketone or SPSF.
(2) carry out above-mentioned indefinite form solid polymer dielectric film crystallizing 10-300min under 110-140 DEG C and vacuum condition, obtain the solid polymer dielectric film of partially crystallizable.
(3) above-mentioned gained solid polymer dielectric film can be carried out pretreatment, to remove organic impurities and inorganic metal ion, and make film H+Change.
(4) decorative layer is adhered on the solid polymer dielectric film two sides at above-mentioned partially crystallizable respectively.
(5) film after attachment decorative layer is dried 10-60min, to remove low boiling point solvent under 40-100 DEG C and vacuum condition.
(6) anode catalyst layer and cathode catalysis layer are adhered to respectively on above-mentioned decorative layer surface.
(7) the above-mentioned film being coated with Catalytic Layer is carried out at 110-200 DEG C secondary crystallization 20-500min, form cocrystallization CCM.
The invention have the advantages that
(1) present invention uses the method for solid polymer electrolyte cocrystallization total with in film for Catalytic Layer, realize Catalytic Layer and form more effectively winding with the macromolecular chain in membrane interface layer, the adhesion of Catalytic Layer and solid polymer dielectric film can be effectively increased, avoid Catalytic Layer and the stripping of film layer in water electrolysis process, improve SPE water electrolysis stability, extend the SPE water electrolytic cell life-span.
(2) present invention can be effectively increased the adhesion of Catalytic Layer and solid polymer dielectric film, reduces Catalytic Layer and film layer contact resistance, reduces water electrolysis voltage, improves water electrolytic cell performance, reduces water battery pond energy consumption.
(3) present invention can be effectively increased Catalytic Layer mechanical performance, it is to avoid in water electrolysis process, Catalytic Layer cracks, and improves SPE water electrolysis stability, extends the SPE water electrolytic cell life-span.
(4) present invention by carrying out partially crystallizable process by indefinite form solid polymer dielectric film, strengthens the mechanical performance of solid polymer dielectric film, is prevented effectively from film Crushing Problem in cocrystallization CCM preparation process.
(5) present invention can be effectively improved Catalytic Layer hydrophobicity, promotes the eliminating of aerogenesis, it is to avoid gas is assembled in Catalytic Layer, improves catalyst utilization, reduces water electrolysis voltage, improves water electrolytic cell performance, reduces water battery energy consumption.
Accompanying drawing explanation
Fig. 1 is before stability test (a:CCM-1(part cocrystallization), b:CCM-2(non-co-crystallize)) with test after (c:CCM-1, d:CCM-2) CCM section SEM figure；
Fig. 2 is the contact angle figure on anode catalyst layer surface；
In Fig. 3, a is two kinds of CCM at 80 DEG C, EIS figure under 1.45V, and b is two kinds of CCM at 80 DEG C, E-I figure under normal pressure；
Fig. 4 is the stability test figure of two kinds of CCM；
Before in Fig. 5, a is two kinds of CCM stability tests with stability test after at 80 DEG C, EIS figure under 1.45V；B be before two kinds of CCM stability tests with stability test after at 80 DEG C, E-I figure under normal pressure.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.Following embodiment is illustrative, is not determinate, it is impossible to limit protection scope of the present invention with following embodiment.
The preparation method of part cocrystallization CCM, step includes:
(1) casting is used to prepare indefinite form solid polymer dielectric film.Method is: area and thickness according to pre-casting film take a certain amount of solid polymer electrolyte solution, dry at 40-100 DEG C and after obtaining solid polymer electrolyte resin, add the high boiling solvent (such as DMAC, DMF etc.) that mass fraction is 40-90%, make solid polymer electrolyte resin dissolve at 40-100 DEG C, by above-mentioned gained solution stirring uniformly after at 40-100 DEG C casting film.
(2) above-mentioned gained solid polymer dielectric film is carried out partially crystallizable 10-300min under 110-140 DEG C and vacuum condition.
(3) film pretreatment: by film 3-8% hydrogen peroxide, process 30-60min under the conditions of 70-100 DEG C after with deionized water at 70-100 DEG C at process 30-60min, again in 0.2-1.0M sulphuric acid, process 30-60min under the conditions of 70-100 DEG C, finally at 70-100 DEG C, process 30-60min with deionized water.Film room temperature for storage after processing is standby in deionized water.
(4) at above-mentioned film surface attachment decorative layer: fixed by the solid polymer dielectric film that pretreated thickness is 0.05-0.175mm, one layer of slurry being mixed into by solid polymer electrolyte solution and isopropanol is sprayed respectively on film two sides.In slurry, solid polymer electrolyte consumption is 0.1-2mgcm-2.Vacuum 40-100 DEG C dries 10-60min, respectively forms one layer of decorative layer on film two sides.
(5) in above-mentioned decorative layer surface spraying Catalytic Layer: fixed by the solid polymer dielectric film being attached with decorative layer, one layer of slurry being mixed into by catalyst, solid polymer electrolyte solution and isopropanol is sprayed respectively on film two sides.Slurry middle-jiao yang, function of the spleen and stomach (cloudy) electrode catalyst consumption is 0.5-5.0mgcm-2(0.1-3.0mgcm-2), solid polymer electrolyte consumption is 0.1-2mgcm-2.40-100 DEG C of vacuum dries 10-60min, obtains CCM.
(6) above-mentioned CCM is carried out at 110-200 DEG C secondary crystallization 20-500min, forming part cocrystallization CCM.
Embodiment 1
A kind of SPE water electrolytic cell part cocrystallization CCM, including Nafiion film, anode modification layer, cathodic modification layer, anode catalyst layer and cathode catalysis layer.Wherein, the side of Nafion membrane is followed successively by anode modification layer and anode catalyst layer, and opposite side is followed successively by cathodic modification layer and cathode catalysis layer.The black Nafion with 25wt.% of the anode catalyst layer Ir containing 75wt.%, cathode catalysis layer contains the Pt/C (40wt.%) and the Nafion of 25wt.% of 75wt.%.
Its preparation method is as follows:
1, preparation indefinite form Nafion membrane: weigh about 40gNafion solution and put in small beaker, adds about 20gDMAC after drying at 60 DEG C, makes dry Nafion resin dissolve at 60 DEG C.Last casting film at 60 DEG C, thickness is about 120 μm.
2, prepare the Nafion membrane of partially crystallizable: gained indefinite form Nafion membrane is crystallized under the conditions of 120 DEG C of vacuum 2h, take out after temperature is down to room temperature.It is calculated its degree of crystallinity by XRD swarming fitting process and is about 8%.
3, above-mentioned gained Nafion membrane is carried out pretreatment: by film 5% hydrogen peroxide, process 40min under the conditions of 80 DEG C after at 80 DEG C, process 30min with deionized water, in 0.5M sulphuric acid, under the conditions of 80 DEG C, process 30min, finally at 80 DEG C, process 30min with deionized water.Film room temperature for storage after processing is standby in deionized water.
4, prepared by Nafion decorative layer: weighs about 0.86g5wt.%Nafion solution and puts in small beaker, add 3mL isopropanol, ultrasonic uniformly, at ambient temperature gained pulp spraying is coated in the one side of pretreated film.
Same proportioning and method is used to prepare Nafion decorative layer at the another side of film.After two sides all completes the spraying of Nafion slurry, film is vacuum dried at 80 DEG C 40min.
5, prepared by anode catalyst layer: weighs the black catalyst of 0.14gIr and puts in small beaker, adds 6mL isopropanol and 0.96g5wt.%Nafion solution, ultrasonic uniformly, at ambient temperature gained pulp spraying is coated in anode Nafion decorative layer surface, obtains anode catalyst layer.
6, prepared by cathode catalysis layer: weighs 0.072g40wt.%Pt/C catalyst and puts in small beaker, add 5mL isopropanol and 0.48g5wt.%Nafion solution, ultrasonic uniformly, at ambient temperature gained pulp spraying is coated in negative electrode Nafion decorative layer surface, obtains cathode catalysis layer.
7, Catalytic Layer processes with the cocrystallization of film: the above-mentioned film being coated with Catalytic Layer is crystallized at 120 DEG C of vacuum 2h, takes out, i.e. obtain part cocrystallization CCM after being down to room temperature.
8, prepared by MEA: carbon paper is placed in the cathode side of above-mentioned CCM as cathode diffusion layer, at 120 DEG C, hot pressing 1min under 0.5MPa, obtains SPE water electrolysis MEA after cooling.
Part cocrystallization CCM had carried out initial crystallization process due to Nafion membrane before preparation CCM, and therefore mechanical performance improves (tensile strength improves about 25%), the most broken during preparation CCM.
As a comparison, using traditional CCM preparation method to be prepared for non-co-crystallization CCM: solid polymer dielectric film is commercialization Nafion115 film (crystalline film) that Dupont company produces, preparing of its finishing coat and Catalytic Layer is described above, but without the cocrystallization processing procedure of Catalytic Layer Yu film, MEA preparation is as mentioned above.
Being respectively used in SPE water electrolytic cell by MEA prepared by the MEA prepared by part cocrystallization CCM and traditional CCM, its water electrolysis performance is as shown in Figure 3.Electrolyzer running temperature is 80 DEG C, and normal pressure runs.As can be seen from Figure, compared with tradition CCM, part cocrystallization CCM has relatively low ohmage, electrochemistry resistance and decomposition voltage, and has higher stability (Fig. 4 and Fig. 5).This raising being primarily due to cocrystallization process caudacoria and Catalytic Layer adhesion can effectively reduce film layer and the contact resistance of Catalytic Layer and proton-conduction resistance, thus reduces decomposition voltage；And the hydrophobic enhancing of Catalytic Layer (Fig. 2) is conducive to the eliminating of aerogenesis after cocrystallization process, improve the utilization rate of catalyst, reduce decomposition voltage.Further, the raising of film and Catalytic Layer adhesion can be prevented effectively from the layering of film and Catalytic Layer, thus improves the stability of water electrolytic cell.
CCM cross section SEM before and after electrolyzer stability test schemes as shown in Figure 1.As can be seen from Figure, CCM is after stability test for tradition, and its Catalytic Layer and film layer occur in that serious stripping, and cocrystallization CCM still contacts well, has no that any crackle produces.
Embodiment 2
Indefinite form Nafion membrane crystallization temperature is 140 DEG C, and crystallization time is 30min；The membrane crystallization temperature being coated with Catalytic Layer is 160 DEG C, and crystallization time is 4h；Prepared by indefinite form Nafion membrane, Nafion membrane pretreatment, and prepared by Nafion decorative layer, prepared by Catalytic Layer, and MEA is prepared as described in Example 1.
Part cocrystallization CCM had carried out initial crystallization process due to Nafion membrane before preparation CCM, and therefore mechanical performance improves (tensile strength improves about 20%), the most broken during preparation CCM.
Embodiment 3
The workbench of spraying decorative layer and Catalytic Layer uses in the vacuum thermal station of 60-80 DEG C of heating, and remaining process is as described in Example 1.
Embodiment 4
A kind of SPE water electrolytic cell part cocrystallization CCM, including sulfonated polyether-ether-ketone (SPEEK) film, anode modification layer, cathodic modification layer, anode catalyst layer and cathode catalysis layer.Wherein, the side of SPEEK film is followed successively by anode modification layer and anode catalyst layer, and opposite side is followed successively by cathodic modification layer and cathode catalysis layer.The black Nafion with 25wt.% of the anode catalyst layer Ir containing 75wt.%, cathode catalysis layer contains the Pt/C (70wt.%) and the Nafion of 25wt.% of 75wt.%.
Its preparation method is as follows:
1, preparation indefinite form SPEEK film: weigh sulfonated polyether-ether-ketone (SPEEK) powder that about 0.7g sulfonation degree is about 60-70%, add about 15gDMAC, make SPEEK dissolve at 60 DEG C.Last casting film at 60 DEG C.
2, prepare the SPEEK film of partially crystallizable: gained indefinite form SPEEK film is crystallized under the conditions of 120 DEG C of vacuum 2h, take out after temperature is down to room temperature.
2, use method same as in Example 1 that the SPEEK film of gained partially crystallizable carries out pretreatment, application Nafion decorative layer and Catalytic Layer.
3, Catalytic Layer processes with the cocrystallization of film: by above-mentioned film vacuum heat 2h at 120 DEG C being coated with Catalytic Layer, takes out, i.e. obtain part cocrystallization CCM after being down to room temperature.
4, method same as in Example 1 is used to prepare MEA.
Part cocrystallization CCM had carried out initial crystallization process due to SPEEK film before preparation CCM, and therefore mechanical performance improves (tensile strength improves about 25%), the most broken during preparation CCM.
Compared with tradition CCM, part cocrystallization CCM has relatively low ohmage, electrochemistry resistance and decomposition voltage, and has higher stability.This raising being primarily due to cocrystallization process caudacoria and Catalytic Layer adhesion can effectively reduce film layer and the contact resistance of Catalytic Layer and proton-conduction resistance, thus reduces decomposition voltage.Further, the raising of film and Catalytic Layer adhesion can be prevented effectively from the layering of film and Catalytic Layer, thus improves the stability of water electrolytic cell.
Claims (8)
1. the SPE water electrolysis preparation method of part cocrystallization Catalytic Layer coat film, Catalytic Layer coat film (CCM) includes polymer dielectric film, anode modification layer, cathodic modification layer, anode catalyst layer and cathode catalysis layer, described polymer dielectric film two sides attachment anode modification layer and cathodic modification layer, anode catalyst layer and cathode catalysis layer the most successively, it is characterised in that:
Operating procedure includes:
(1) area and thickness according to pre-casting film take a certain amount of solid polymer electrolyte resin, and adding mass fraction is the high boiling solvent of 40-90%, makes solid polymer electrolyte solution, and described high boiling solvent is DMAC, DMF；
(2) use casting method, the tape casting or spraying process by above-mentioned gained solution solvent flashing film forming at 40-100 DEG C；
(3) carry out above-mentioned indefinite form solid polymer dielectric film crystallizing 10-300min under 110-140 DEG C and vacuum condition, obtain the solid polymer dielectric film of partially crystallizable；
(4) solid polymer dielectric film of step (3) gained partially crystallizable is carried out pretreatment, to remove organic impurities and inorganic metal ion, and make film H+Change；
(5) the solid polymer dielectric film both side surface at above-mentioned pretreated partially crystallizable adheres to anode modification layer, cathodic modification layer respectively；
Prepare the slurry used by decorative layer to be mixed by solid polymer and low boiling point solvent, wherein the mass fraction of solid polymer electrolyte is 1-10%, and the low boiling point solvent described in step (5) is one or two or more kinds in deionized water, ethanol, isopropanol；
(6) film after attachment decorative layer is dried 10-60min under 40-100 DEG C and vacuum condition；
(7) use spraying process, transfer printing, knife coating or silk screen print method at above-mentioned anode modification layer surface attachment anode catalyst layer；Use spraying process, transfer printing, knife coating or silk screen print method at above-mentioned cathodic modification layer surface attachment cathode catalysis layer；
(8) the above-mentioned film being coated with Catalytic Layer is carried out secondary crystallization 20-500min, forming part cocrystallization CCM at 110-200 DEG C.
Preparation method the most according to claim 1, it is characterised in that: the solid polymer of preparation indefinite form solid polymer dielectric film is perfluorinated sulfonic resin, sulfonated polyether-ether-ketone or SPSF.
Preparation method the most according to claim 1, it is characterized in that: the pre-treatment step described in step (4) is: volumetric concentration 3-8% hydrogen peroxide, process 30-60min under the conditions of 70-100 DEG C after with deionized water at 70-100 DEG C at process 30-60min, again in 0.2-1.0M sulphuric acid, process 30-60min under the conditions of 70-100 DEG C, finally at 70-100 DEG C, process 30-60min with deionized water.
Preparation method the most according to claim 1, it is characterised in that: the preparation of the solid polymer dielectric film both side surface decorative layer described in step (5) uses spraying process, transfer printing, knife coating or silk screen print method.
Preparation method the most according to claim 1, it is characterised in that: anode modification layer, cathodic modification layer thickness described in step (5) are 1-20 μm.
Preparation method the most according to claim 1, it is characterised in that: the cathode catalysis layer slurry described in step (7) is made up of Pt/C catalyst, solid polymer electrolyte and low boiling point solvent；Solid polymer is 1:9～1:1 with the mass ratio of Pt/C catalyst, and the mass fraction of solid polymer electrolyte is 1-10%；In Pt/C catalyst, Pt mass fraction is 20-70%；
Anode catalyst layer slurry described in step (7) is made up of oxygen-separating catalyst, solid polymer electrolyte and low boiling point solvent；Solid polymer electrolyte resin is 1:9～1:1 with the mass ratio of oxygen-separating catalyst, and the mass fraction of solid polymer electrolyte is 1-10%.
Preparation method the most according to claim 6, it is characterised in that:
Oxygen-separating catalyst is that Ir is black, IrO2、RuO2, one or two or more kinds in Pt/C, in Pt/C catalyst, Pt mass fraction is 20-70%.
8. according to the preparation method described in claim 6 or 7, it is characterised in that:
Cathode catalysis layer Pt load amount is 0.1-3.0mgcm-2；In anode catalyst layer, oxygen-separating catalyst load amount is 0.5-5.0mgcm-2。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1983684A (en) * | 2005-12-16 | 2007-06-20 | 中国科学院大连化学物理研究所 | Ordered membrane electrode of proton-exchange membrane fuel battery |
| CN101008087A (en) * | 2006-01-25 | 2007-08-01 | 中国科学院大连化学物理研究所 | Preparation method of film electrode for solid polymer electrolyte water electrolysis |
| CN102260877A (en) * | 2011-07-06 | 2011-11-30 | 山东赛克赛斯氢能源有限公司 | Preparation method of ion membrane electrode for pure water electrolysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1983684A (en) * | 2005-12-16 | 2007-06-20 | 中国科学院大连化学物理研究所 | Ordered membrane electrode of proton-exchange membrane fuel battery |
| CN101008087A (en) * | 2006-01-25 | 2007-08-01 | 中国科学院大连化学物理研究所 | Preparation method of film electrode for solid polymer electrolyte water electrolysis |
| CN102260877A (en) * | 2011-07-06 | 2011-11-30 | 山东赛克赛斯氢能源有限公司 | Preparation method of ion membrane electrode for pure water electrolysis |
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