CN105734606A - Structure of ultrathin membrane electrode for SPE water electrolysis and preparation and application of structure - Google Patents
Structure of ultrathin membrane electrode for SPE water electrolysis and preparation and application of structure Download PDFInfo
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Abstract
The invention provides a structure of an ultrathin membrane electrode for SPE water electrolysis and a preparation method of the structure. The preparation method comprises the steps that firstly, a gold foil is adopted as a raw material, an dealloy method is adopted for obtaining a nano porous gold thin membrane, and then the thin membrane is transfer-printed to an ion exchange membrane; and the nano porous gold thin membrane is adopted as a supporting layer to carry a catalyst, and the ultrathin membrane electrode is manufactured. The manufactured membrane electrode has the beneficial effects of being small in catalyst carrying amount, high in utilization rate, easy to amplify and the like. The manufactured membrane electrode can be used for a water electrolysis pool, a regenerative fuel cell and other electrochemical reactors.
Description
Technical field
The present invention relates to solid polymer electrolyte (SPE) water electrolysis field, be specially structure and the preparation method of a kind of SPE water electrolysis ultrathin electrodes.Prepared ultrathin electrodes can be used for water electrolytic cell, regeneratable fuel cell.
Background technology
Along with technology, economic development, the demand of the energy is continued to increase by human society.A kind of cleaning, efficient energy storage technology become the demand of the whole mankind.And the ecological environment increasingly worsened forces people to strengthen the dynamics of research and development.
Hydrogen cleans as one, efficient energy carrier, it has also become the research emphasis of countries in the world government and research institution.Electrolytic lye hydrogen producing technology was once the mainstream technology of large-scale hydrogen manufacturing.But its electrolyte is susceptible to run off, and environment is had harm by the asbestos diaphragm of use, causes that this technology is eliminated.And solid polymer electrolytic technology (SolidPolymerElectrolyte, SPE), owing to there is environmental friendliness, producing the advantages such as hydrogen purity is high, energy efficiency high, is easily maintained, become study hotspot.
Membrane electrode assembly (MEA) is the core component of SPE water electrolysis.Traditional MEA preparation method can be divided into two big classes.One class is GDE method, and another kind of is CCM method.Compared with GDE, CCM has the advantages such as Catalytic Layer is thin, catalyst amount is low.At present, the MEA employing being applied to SPE water electrolysis is prepared by CCM method.But hydrophilic stronger for CCM causes that the gas produced in electrolytic process is easily assembled in Catalytic Layer, reduces catalyst utilization.The working environment special with the difference of the swellability of film and SPE water electrolysis due to the Catalytic Layer of CCM (runs for a long time under water environment, reaction produces the washing away Catalytic Layer such as hydrogen, oxygen), it is easily caused the stripping of Catalytic Layer and film, thus the contact resistance increased between Catalytic Layer and film, reduce proton conductivity, affect the life-span of SPE water electrolytic cell.
Patent CN1967916A describes the painting method of a kind of SPE water electrolysis part cocrystallization Catalytic Layer.Adhering to decorative layer respectively in the solid polymer membrane both sides processed through part cocrystallization, the slurry preparing decorative layer is made up of solid polymer and low boiling point solvent.Decorative layer adopt the methods such as spraying support the catalyst such as Pt, Ir.After adopting cocrystallization to process, the adhesion between Catalytic Layer and film strengthens, and the tensile strength of CCM improves about 25%.But cathode catalysis layer Pt load amount is 0.1-3.0mgcm in this patent-2, anode catalyst layer oxygen-separating catalyst load amount is 0.5-5.0mgcm-2。
Patent CN102260877A adopts sand paper that solid electrolyte film is polished, thus reaching the purpose increasing Catalytic Layer with the adhesion of film.Again catalyst pulp is coated on transfer plate, Catalytic Layer is transferred to ion exchange membrane both sides.The standby electrode cathode catalyst loading of this patent system is 1.45 ± 0.5mg/cm2, anode catalyst load amount is 4.2 ± 1.0mg/cm2, and dielectric film is through polishing so that it is and mechanical strength reduces, and affects cell life.
Patent WO2004021481-A1 describes a kind of method by nano-porous gold (NPG, nanoporousgold) for Proton Exchange Membrane Fuel Cells.First, nano-porous gold is transferred in the precursor solution of Pt, in reactor, then introduces hydrazine steam, on the inner surface of nano-porous gold, finally define the Pt layer of about 3nm.Adopt the power of battery of this nanomaterial assembly at 140mWcm-2Left and right.This patent is using the nanoporous gold thin film structure as self-supporting, but in the process of preparation, nanoporous gold thin film is frangible, which increases the difficulty of nano-porous gold finishing so that this functional material of nanoporous gold thin film is restricted in engineer applied.The hydrazine that this patent adopts is poisonous.
Nanoporous gold thin film has the features such as abundant specific surface area, the three-dimensional pore structure of UNICOM, excellent electric conductivity, good resistance to corrosion.The thickness of the thin film of nano-porous gold can between 100nm-1000nm flexible modulation.
This patent adopts hot-pressing technique, in advance by nano-porous gold film hot-pressing in ion exchange membrane both sides, solves nanoporous gold thin film mechanical strength low, the problem not easily carrying out finishing.
Under the effect of temperature and pressure, nanoporous gold thin film is anchored on ion exchange membrane.Under ensure that the premise that the mechanical strength of ion exchange membrane does not reduce, we obtain the membrane electrode assembly with good combination power.Using the thin layer electrode that nanoporous gold thin film is prepared as supporting layer, there is ultra-thin thickness, the pore structure of three-dimensional UNICOM.The separation of this timely conveying being conducive to reactant and product；The specific surface area that nano-porous gold enriches can provide more catalyst attachment point, can improve the dispersion of catalyst；The metallic bond formed between noble metal catalyst and nano-porous gold can improve the stability of catalyst；Nano-porous gold itself has good resistance to corrosion, can improve the stability of electrode.
Summary of the invention
The preparation method of a kind of water electrolysis ultrathin membrane electrode, comprises the following steps:
1) preparating acid etching solution: the nitric acid of preparation concentration 5.4-15.8mol/L or the perchloric acid of 1-10mol/L are as etching solution；
2) native gold is immersed in above-mentioned acid etch solution, at 10 DEG C-40 DEG C, react 5min-24h, obtain nanoporous gold thin film；
3) nanoporous gold thin film is transferred to from acid etch solution in water and cleans, remove the acid of film surface residual, then move in substrate.Substrate can be that mica sheet, sheet glass, stainless steel substrates, copper sheet, titanium sheet, aluminium flake etc. have hydrophilic and the material of certain mechanical strength；
4) adopt pressure sintering that from substrate surface, nanoporous gold thin film is transferred to ion exchange membrane surface.Ion exchange membrane can be the alkaline anion-exchange membranes such as Nafion PEM or A201.During transfer pressure be sized to 0.1～10MPa, the time is 0.5～30min, and temperature is 50～200 DEG C；
5) remove substrate, clean thin film；
6) adopt electrochemical reduction or chemical reduction method catalyst-loaded in the nanoporous gold thin film be carried on ion exchange membrane surface.
The electrochemical reducing adopted includes: cyclic voltammetric electro-deposition, pulse electrodeposition, permanent electricity electro-deposition and constant voltage electro-deposition.Electrochemical reducing comprises the steps of 1) build three-electrode system, to be fitted with the thin film of nanoporous gold thin film as working electrode；2) preparation 0.1-3.0MH containing precious metal salt2SO4；In electrolyte, precious metal salt is 0.1mM-10mMIrCl6 2-、0.1mM-10mMPtCl6 2-、0.1mM-10mMIr3+、0.1mM-10mMPd2+And it is a kind of or more than two kinds；3) nano-porous gold is applied reduction potential or reduction current, until having supported the catalyst of required carrying capacity.
The chemical reduction method adopted is immersion reduction method, and reducing agent is the NaBH of 0.1mM-1M4Or aqueous ascorbic acid.Chemical reduction method comprises the steps of 1) by the thin film dipped 1s-3min in the aqueous solution containing precious metal salt of nanoporous gold thin film；Precious metal salt in aqueous solution used is 0.1mM-10mMIrCl6 2-、0.1mM-10mMPtCl6 2-、0.1mM-10mMIr3+、0.1mM-10mMPd2+In a kind of solution or two kinds of solution mixed above；2) by through step 1) thin film that processes is placed in deionized water and cleans；3) by through step 2) thin film that processes is placed in the aqueous solution of reducing agent；Reducing agent is the NaBH of 1mM-1M4The aqueous ascorbic acid of aqueous solution or 1mM-1M；Time 1s-5min；4) 1 is repeated)～3) until having supported the catalyst of required carrying capacity.
7) by the electrode of preparation at the 3%H of 80 DEG C2O2Solution boils 40min, then at the 0.5MH of 80 DEG C2SO4In boil 40min, then in the deionized water of 80 DEG C, boil 30min, dry standby.
The catalyst supported is Pt, Pd, Ru, Rh, Ir, Au, Ag, Ni, Co, the simple substance of Cu and Fe and two or more alloy thereof.
The present invention has a characteristic that
1. nano porous metal thin film is transferred to ion exchange membrane surface by the present invention, solves the problem that nano porous metal film strength is low；
2. the present invention adopts nanoporous gold thin film as supporting layer, is effectively increased dispersion and the stability of catalyst, the pore structure of nanoporous gold thin film three-dimensional UNICOM and ultra-thin thickness, is conducive to the separation of reactant conveying and product；
3. it is low that the electrode that prepared by the present invention has noble metal dosage, the feature that catalyst utilization is high.
Accompanying drawing explanation
Fig. 1 embodiment of the present invention 1 prepares the flow chart of thin layer electrode.
Fig. 2 embodiment of the present invention 1 is prepared the SEM figure of nanoporous gold thin film.
The SEM figure of thin layer economic benefits and social benefits electrode NPG (30) PtPdIr of preparation in Fig. 3 embodiment of the present invention 1.
The SEM figure of thin layer economic benefits and social benefits electrode NPG (30) PtIr of preparation in Fig. 4 embodiment of the present invention 2.
Thin layer electrode NPG (30) PtPdIr of Fig. 5 embodiment of the present invention 1 preparation I-V performance curve in electrolyzer.
Thin layer electrode NPG (30) PtIr of Fig. 6 embodiment of the present invention 2 preparation I-V performance curve in electrolyzer.
Thin layer electrode NPG (30) PtIr of Fig. 7 embodiment of the present invention 2 preparation I-V performance curve in a fuel cell.
Detailed description of the invention
Following example will be further illustrating the present invention.
Embodiment 1
With 12K native gold (Au50Ag50Wt.%) for raw material, native gold is cut into suitably sized (2.1cm*2.1cm), native gold is come at deionized water surface spreading, and be transferred in the nitric acid of dilution (nitric acid, deionized water volume ratio be 2:1), the control response time is 30min, and prepared nano-porous gold is labeled as NPG (30).Being transferred in deionized water by the nanoporous gold thin film (NPG, nanoporousgoldfilm) obtained after removal alloying, now nanoporous gold thin film is opened at deionized water surface spreading；Change deionization 3-4 time, remove the nitric acid in nanoporous gold thin film；Nanoporous gold thin film is transferred to mica sheet (size 2.5cm × 4.0cm), at room temperature dries；Nafion211 film is covered in the side of nanoporous gold thin film, 150 DEG C, 5MPa when hot pressing 3min；Carefully remove mica sheet, clean the Nafion membrane obtained with deionized water.Opening size test shows, prepared nano-porous gold thickness is 100nm, and porosity is 59.92%, and characteristic aperture is 8.02nm.
Potentiostatic method is adopted to deposit Pt, Pd, Ir in nanoporous gold thin film.Concrete operational approach: build three-electrode system, be connected as working electrode using the Nafion211 thin film being fitted with nanoporous gold thin film with wire, with high purity graphite plate for electrode, with saturated calomel electrode for reference electrode；Before plating, working electrode is placed in the 0.5MH of abundant deoxygenation2SO4In solution, adopting cyclic voltammetry (CV) to remove the pollutant on surface, the electromotive force interval of cyclic voltammetry is (0.0V, 1.7V) (vs.RHE), sweeps speed 100mV/s, scans 30min；Then working electrode is switched in electroplate liquid, the composition of electroplate liquid: 1.0mMH2IrCl6、2.0mMH2PtCl6、0.5mMPdCl2, 0.5MH2SO4As supporting electrolyte；The electromotive force of electro-deposition is-0.141V (vs.SCE), deposits 10min.By the prepared electrode 3%H at 80 DEG C2O2Solution boils 40min, then at the 0.5MH of 80 DEG C2SO4In boil 40min, then in the deionized water of 80 DEG C, boil 30min, dry standby.ICP test shows, the Ir loading of electrode prepared by this method is: 10.6 μ g/cm2, Pt loading is: 17.1 μ g/cm2, Pd loading is: 6.7 μ g/cm2.Obtained electrode designations is NPG (30) PtPdIr.Opening size test shows, prepared NPG (30) PtPdIr.Porosity is 23.4%, and characteristic aperture is 4.21nm.
Electrolyzer test condition: the electrode area of cathode and anode is 4.0cm2, cathode side adopts GDE as electrode；Electrolyzer temperature 80 DEG C；Anode-side discharge 10mL/min；Normal pressure runs.Water electrolytic cell is at 500mAcm-2Time decomposition voltage be 1.60V.
Embodiment 2
The preparation of nanoporous gold thin film and transfer process are referring to embodiment 1.
Adopt constant potential electrodeposition process coelectrodeposition deposition Pt, Ir in nanoporous gold thin film.Concrete operational approach: build three-electrode system, be connected as working electrode using the Nafion211 thin film being fitted with nanoporous gold thin film with wire, with high purity graphite plate for electrode, with saturated calomel electrode for reference electrode；Before plating, working electrode is placed in the 0.5MH of abundant deoxygenation2SO4Adopting cyclic voltammetry (CV) to remove the pollutant on surface in solution, the electromotive force interval of cyclic voltammetry is (0.0V, 1.7V) (vs.RHE), sweeps speed 100mV/s, scans 30min；Then working electrode is switched in electroplate liquid, the composition of electroplate liquid: 0.4mMH2IrCl6、0.5mMH2PtCl6、0.5MH2SO4As supporting electrolyte；The electromotive force of electro-deposition is-0.041V (vs.SCE), deposits 20min.By the prepared electrode 3%H at 80 DEG C2O2Solution boils 40min, then at the 0.5MH of 80 DEG C2SO4In boil 40min, finally in the deionized water of 80 DEG C, boil 30min, dry standby.ICP test shows, the Ir loading of electrode prepared by this method is: 17.6 μ g/cm2, Pt loading is: 27.2 μ g/cm2.Obtained electrode designations is NPG (30) PtIr.Opening size test shows, prepared NPG (30) PtIr.Porosity is 26.75%, and characteristic aperture is 5.74nm.
Electrolyzer test condition: the electrode area of cathode and anode is 4.0cm2, cathode side adopts GDE as electrode；Electrolyzer temperature 80 DEG C；Anode-side discharge 10mL/min；Normal pressure runs.Water electrolytic cell is at 500mAcm-2Time decomposition voltage be 1.67V.
Fuel cell battery testing condition: negative electrode, anode electrode area be 4.0cm2, anode-side adopts GDE as electrode；H2/O2Flow: 50/100sccmcm-1；Battery temperature 65 DEG C, saturated humidification, 0.05MPa inlet pressure.The peak power density of fuel cell is 220mWcm-2(723mAcm-2)。
Claims (10)
1. the SPE water electrolysis structure of ultrathin membrane electrode, it is characterized in that: side or the two side surface hot pressing of ion exchange membrane have the nanoporous gold thin film as supporting layer, on supporting layer inner surface, deposited catalyst forms catalyst layer again, is ultrathin membrane electrode.
2. the structure described in claim 1, it is characterised in that: the nanoporous gold thin film as supporting layer has three-dimensional linked hole structure, and characteristic aperture is at 2nm-500nm, and porosity is 20%-70%, and film thickness is at 100nm-1000nm；On supporting layer inner surface, the loading of deposited catalyst is 5 μ gcm-2～100 μ gcm-2, catalyst is island or continuous film distribution at nanoporous gold thin film inner surface.
3. the preparation method of structure described in a claim 1 or 2, it is characterised in that: as the nanoporous gold thin film hot pressing in advance of supporting layer on ion exchange membrane, then on supporting layer deposited catalyst, finally electrode is carried out purified treatment, obtains ultrathin membrane electrode.
4. the preparation method described in claim 3, it is characterised in that: described nano-porous gold film hot-pressing, to the method on ion exchange membrane surface, comprises the following steps:
1) preparating acid etching solution；Acid etch solution is the perchloric acid of the nitric acid of concentration 5.4-15.8mol/L or 1-10mol/L；
2) native gold is immersed in above-mentioned acid etch solution, be obtained by reacting nanoporous gold thin film；The time of acid etch is 5min-24h, and etching temperature is 10 DEG C-80 DEG C；
3) nanoporous gold thin film is transferred to from acid etch solution in deionized water and cleans, remove the acid of film surface residual, then move in substrate；
4) adopt pressure sintering that from substrate surface, nanoporous gold thin film is transferred to ion exchange membrane surface, remove substrate, clean thin film；The pressure applied during hot pressing is sized to 0.1～10MPa, and the time is 0.5～30min, and temperature is 50～200 DEG C.
5. the preparation method described in claim 4, it is characterised in that:
Step 3) in, substrate used is that mica sheet, sheet glass, stainless steel substrates, copper sheet, titanium sheet or aluminium flake etc. have hydrophilic and the material of certain mechanical strength；
Step 4) in, ion exchange membrane used includes the alkaline anion-exchange membranes such as Nafion PEM and A201.
6. the preparation method described in claim 4, it is characterised in that: step 4) in, the nanoporous gold thin film as supporting layer has three-dimensional linked hole structure, and characteristic aperture is at 2nm-500nm, and porosity is 20%-70%, and film thickness is at 100nm-1000nm.
7. the preparation method described in claim 4, it is characterised in that: the method for described catalyst loading can be electrochemical reducing or chemical reduction method；
Described electrochemical reducing, comprises the steps of
1) three-electrode system is built, to be fitted with the thin film of nanoporous gold thin film as working electrode；
2) electrolyte is the 0.1-3.0MH containing precious metal salt2SO4；In electrolyte, precious metal salt is 0.1mM-10mMIrCl6 2-、0.1mM-10mMPtCl6 2-、0.1mM-10mMIr3+、0.1mM-10mMPd2+And it is a kind of or more than two kinds；
3) nano-porous gold is applied reduction potential or reduction current；Electrochemical reduction method includes: cyclic voltammetric electro-deposition, pulse electrodeposition, permanent electricity electro-deposition or constant voltage electro-deposition；Until having supported the catalyst of required carrying capacity；
Described chemical reduction method, comprises the steps of
1) by the thin film dipped 1s-3min in the aqueous solution containing precious metal salt of nanoporous gold thin film；Precious metal salt in aqueous solution used is 0.1mM-10mMIrCl6 2-、0.1mM-10mMPtCl6 2-、0.1mM-10mMIr3+、0.1mM-10mMPd2+In a kind of solution or two kinds of solution mixed above；
2) by through step 1) thin film that processes is placed in deionized water and cleans；
3) by through step 2) thin film that processes is placed in the aqueous solution of reducing agent；Reducing agent is the NaBH of 1mM-1M4The aqueous ascorbic acid of aqueous solution or 1mM-1M；Time 1s-5min；
4) 1 is repeated)～3) until having supported the catalyst of required carrying capacity.
8. the preparation method described in claim 7, it is characterised in that:
The catalyst of preparation is island or continuous film distribution in nanoporous gold surface；The catalyst of preparation is one or more alloys in Pt, Pd, Ru, Rh, Ir, Au, Ag, Ni, Co, Cu or Fe.
9. the preparation method described in claim 4, it is characterised in that: described electrode purification method, comprise the following steps:
1) by the electrode of preparation at the 3%H of 80 DEG C2O2Solution boils 40min；
2) will through step 1) electrode that processes is at the 0.5MH of 80 DEG C2SO4In boil 40min；
3) by through step 2) electrode that processes boils 30min in the deionized water of 80 DEG C, dries standby.
10. the application of structure described in a claim 1 or 2, it is characterised in that: described electrode can be used in water electrolytic cell, regeneratable fuel cell or other electrochemical reactor.
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| CN108075139A (en) * | 2016-11-18 | 2018-05-25 | 中国科学院大连化学物理研究所 | Based on the ordering membrane electrode of metal oxide nano band and its preparation and application |
| CN108107090A (en) * | 2017-11-09 | 2018-06-01 | 国家电网公司 | A kind of detection method of solid polymer electrolyte water electrolytic cell membrane electrode pollution |
| CN109599580A (en) * | 2018-12-24 | 2019-04-09 | 天津理工大学 | A kind of ultra-thin membrane electrode and its preparation method and application for neat liquid fuel cell |
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| TWI677596B (en) * | 2018-11-30 | 2019-11-21 | 財團法人工業技術研究院 | Membrane electrode assembly and method for hydrogen evolution by electrolysis |
| US10900133B2 (en) | 2018-11-30 | 2021-01-26 | Industrial Technology Research Institute | Nitride catalyst and method for manufacturing the same |
| US10914012B2 (en) | 2018-11-30 | 2021-02-09 | Industrial Technology Research Institute | Membrane electrode assembly and method for hydrogen evolution by electrolysis |
| US10914011B2 (en) | 2018-11-30 | 2021-02-09 | Industrial Technology Research Institute | Membrane electrode assembly and method for hydrogen evolution by electrolysis |
| CN109599580A (en) * | 2018-12-24 | 2019-04-09 | 天津理工大学 | A kind of ultra-thin membrane electrode and its preparation method and application for neat liquid fuel cell |
| CN111020618A (en) * | 2019-11-28 | 2020-04-17 | 北京中氢源工程科技有限公司 | Multifunctional hydrogen absorption machine |
| CN112760598A (en) * | 2020-12-30 | 2021-05-07 | 昆明理工大学 | Porous noble metal-based membrane electrode and preparation method and application thereof |
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