CN106935879A - A kind of preparation method of compound cathode of solid oxide fuel battery current collecting material - Google Patents
A kind of preparation method of compound cathode of solid oxide fuel battery current collecting material Download PDFInfo
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- CN106935879A CN106935879A CN201710263582.6A CN201710263582A CN106935879A CN 106935879 A CN106935879 A CN 106935879A CN 201710263582 A CN201710263582 A CN 201710263582A CN 106935879 A CN106935879 A CN 106935879A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0226—Composites in the form of mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0206—Metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0215—Glass; Ceramic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M2008/1293—Fuel cells with solid oxide electrolytes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The present invention relates to fuel cell field, especially a kind of preparation method of compound cathode of solid oxide fuel battery current collecting material.Ag particles are prepared into LCN Ag composite cathode boundary materials with LCN particles by mechanical mixture, Ag is silver, and LCN is ceramics, and the ratio of Ag particles is 5wt% ~ 30wt%, the size scope of Ag particles is 0.1 μm ~ 5 μm, and the size scope of LCN particles is 0.05 μm to 2 μm.Invention LCN Ag cathode interface materials both can be used alone, it is also possible to is jointly formed sandwich construction with other cathode contacts materials and uses.Technical staff can suitably select the ratio of Ag in the calcine technology and composite of LCN according to actual needs, so as to solve that perovskite structure ceramic high temperature electric conductivity is not enough, and metal Ag prices are higher, be easy to the problem reunited.
Description
Technical field
The present invention relates to fuel cell field, especially a kind of compound cathode of solid oxide fuel battery current collecting material
Preparation method.
Background technology
With economic fast development, the traditional energy supply mode based on fossil energy is hard to carry on.One side
Face, substantial amounts of waste water, waste gas, waste residue does great damage to environment, and " greenhouse effects " also turn into human social
Huge obstruction；On the other hand, fossil fuel causes a large amount of energy losses in the process for being converted into electric energy or mechanical energy, its fuel
Utilization rate only has 33% ~ 35%.Hydrogen Energy and fuel cell are to realize one of clean energy, the important channel of low-carbonization development.Combustion
Material battery is the TRT that a kind of chemical energy that will be present in fuel and oxidant is converted into electric energy, is turned with energy
The advantages of efficiency high is changed with module extendibility.
SOFC belongs to third generation fuel cell, and the main feature that it is different from other fuel cells exists
In the oxide for using solid ionic conductive as electrolyte, with advantages below：(1) structure of whole solid state, appearance structure
Design has more flexibility；(2) running temperature is high, and electrode reaction dynamics is fast, it is not necessary to use noble metal catalyst；(3) fuel
Using variation, CO and H can be not only used2Deng as fuel gas, it is also possible to reform and use coal gas, methane and liquid fuel；
(3) it is adapted to thermoelectricity to join altogether, energy utilization efficiency is up to 80% or so.
For being operated in 800oFor the intermediate temperature SOFC of below C, the contact resistance produced by cathode interface is far above sun
Pole, both have the difference of the order of magnitude.Therefore, the interface performance between metal connector and cell cathode has become the middle temperature of restriction
The bottleneck of SOFC technologies development.In order to reduce the area specific resistance at interface between the two, it is necessary to make using the material of electronic conduction high
It is cathode interface layer.As shown in figure 1, cathode interface layer is located between cell cathode and metal connector, ensureing electric current collection
On the premise of efficiency, by modulating the granularity of powder, the porosity inside optimization boundary layer is allowed to meet air arrival three-phase
Interface, the requirement for participating in electrochemical reaction.
Cathode interface contact problems are the principal elements for causing SOFC Performance data to decay.Anode-side
In reproducibility fuel atmosphere, generally using nickel slurry and nickel foam as contact material, metallic nickel can galvanic anode with
Quick electronic conduction passage is formed between metal connector, and cathode interface contact material is in high temperature oxidative atmosphere, boundary
Surface contact state is complex.Consideration based on material cost and matched coefficients of thermal expansion, it is impossible to select stable performance, it is conductive
The good noble metal Au of property, Pt.A kind of porous high-temperature electric conduction ceramic material is filled generally between negative electrode and connector to be improved
Cathode interface is contacted, and its Main Function is：(1) effective conductive path is formed between negative electrode and metal connector, external circuit is passed
The electronics led is conducted to cathode surface by metal connector, is smoothed out Cathodic oxygen reduction；(2) interracial contact material
It is that the ceramic powder of one layer of flexibility is piled up and formed, the thermal stress that adjacent component is produced by thermal expansion coefficient difference can be discharged,
Effectively prevent the stress destruction that connector is produced with ceramic electrode directly contact.LaxSr with perovskite structure1- xMnO3（LSM）It is the most frequently used negative electrode and interface current collecting material, LSM has electron conduction higher, shows at high temperature
Good chemical property.But with the operating temperature reduction of SOFC, the electronic conductivity of LSM has declined, it is impossible to completely
Meet its performance requirement as cathode interface material.
The content of the invention
In order to overcome the shortcomings of that existing battery cannot keep conductance at low temperature, the invention provides a kind of solid oxygen
The preparation method of compound fuel battery complex cathode current collecting material.
The technical solution adopted for the present invention to solve the technical problems is：A kind of compound cathode of solid oxide fuel battery
The preparation method of current collecting material, Ag particles are prepared into LCN-Ag composite cathode boundary materials, Ag with LCN particles by mechanical mixture
It is silver, LCN is ceramics, and the ratio of Ag particles is 5 wt% ~ 30 wt%, and the size scope of Ag particles is 0.1 μm ~ 5 μm,
The size scope of LCN particles is 0.05 μm to 2 μm.
According to another embodiment of the invention, further include that the LCN particles are using metal cation, non-chelated
Solution mixed by polymer and solvent is dried and calcined and forms, and calcining heat is 700oC~1200 oC, soaking time is insulation
Time is 1 ~ 5 h.
According to another embodiment of the invention, further include that the cation source is the nitrate of metal, sulfuric acid
Salt or chlorate, solution are the PVA aqueous solution, are 1 according to PVA hydroxyls and all metal cation positive charge mol ratios：4 weigh
PVA, is 90 in temperatureo12h is stirred under C bath temperatures and obtains solution.
The beneficial effects of the invention are as follows invention LCN-Ag cathode interface materials both can be used alone, it is also possible to it
His cathode contacts material is jointly formed sandwich construction and uses.Technical staff can suitably select the calcining of LCN according to actual needs
The ratio of Ag in technique and composite so that it is not enough to solve perovskite structure ceramic high temperature electric conductivity, and metal Ag prices compared with
Problem that is high, being easy to reunion.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is cathode of solid oxide fuel cell current collector layer and metal connector relation schematic diagram；
Fig. 2 is the LCN-Ag cathode interfaces material of different Ag contents in operating temperature 750oElectric performance test figure during C；
Fig. 3 is the area specific resistance change of 10 thermal cycle tests of LCN-Ag cathode interfaces material of different Ag contents, temperature range
200 oC ~750 oTest chart in C.
Specific embodiment
If Fig. 1 is cathode of solid oxide fuel cell current collector layer and metal connector relation schematic diagram, Fig. 2 is different Ag
The LCN-Ag cathode interfaces material of content is in operating temperature 750oElectric performance test figure during C, Fig. 3 is different Ag contents
The area specific resistance change of 10 thermal cycle tests of LCN-Ag cathode interfaces material, temperature range 200oC ~750 oTest in C
Figure.A kind of preparation method of compound cathode of solid oxide fuel battery current collecting material, Ag particles are mixed by machinery with LCN particles
Conjunction is prepared into LCN-Ag composite cathode boundary materials, and Ag is silver, and LCN is ceramics, and the ratio of Ag particles is 5 wt% ~ 30 wt%, Ag
The size scope of particle is 0.1 μm ~ 5 μm, and the size scope of LCN particles is 0.05 μm to 2 μm.The LCN
Particle is to be dried and calcined using the solution mixed by metal cation, non-chelated polymer and solvent to form, and calcining heat is
700 oC~1200 oC, soaking time is that soaking time is 1 ~ 5 h.The cation source be the nitrate of metal, sulfate or
Chlorate, solution is the PVA aqueous solution, is 1 according to PVA hydroxyls and all metal cation positive charge mol ratios：4 weigh PVA,
Temperature is 90o12h is stirred under C bath temperatures and obtains solution.The mechanical mixture is that polishing processes Ag particles and LCN particles,
And binding agent is used as by ethyl cellulose and terpinol bonds Ag particles and LCN particles.
Present invention selection has the perovskite structural material LaCo compared with highly electron conductive0.6Ni0.4O3-δ(LCN) as high
Warm conducting ceramic material.Purity is low during to overcome solid reaction process to prepare powder and the big shortcoming of particle size, and the present invention is used
Wet chemical method prepares cathode interface material.This technology, as chelating agent, esterification process is promoted with ethylene glycol using citric acid
In polymerization.Cation is typically derived from metal nitrate, and other salts have also considered.Select different cation presomas
One important consideration is its solubility in aqueous.Non-chelated polymerization is chosen by the polymer for attempting different polyhydroxy
Species type, and determine the relation between its molecular weight and solution viscosity.Then, according to selected presoma, polymer, solvent with
And perovskite-like structure material is configured to the solution of cation-non-chelated polymer-solvent, optimize composition proportion.In solution
During dry and powder calcination, by studying the relation between this process and the size distribution of prepared material, it is determined that
Optimal calcining heat and time.In a preferred embodiment, calcining heat 800oC, is incubated 3 h, and LCN powder granules are about
100 nm, its particle with calcining heat raise with holding time and be roughened.By 650oMore than C powder calcinations, can be with
The single Ca-Ti ore type LCN powders of phase structure are obtained, 400oC and 800oBetween C, the electrical conductivity of material is higher than 1100 S
cm-1, the material of preparation can meet the use requirement of sofc cathode boundary material in granularity and pattern.
Metal Ag has a price of relative moderate, and the advantages of excellent electron conduction, but metal Ag is easy at high temperature
Roughening, with high volatile the characteristics of, which has limited its directly as cathode interface contact material use.To give full play to gold
Belong to the high conductivity of Ag, and the stable characteristic of LCN powder characteristics, the present invention is prepared for quality point by the method for mechanical mixture
Number is respectively 10 wt%, the LCN-Ag composite cathode boundary materials of 20 wt%, 30 wt%.It is incubated in 750oC by sample,
200 oC to 750oThe conducting performance test of C thermal cycles, determines optimal Ag compositely proportionals.In a preferred embodiment, 10
The electric conductivity of the LCN-Ag cathode interface materials of wt% and 20 wt% is substantially better than single LCN as interracial contact material,
Main reason is that Ag particles are dispersed in LCN, it is embedded in the three-dimensional net structure of LCN matrixes, forms one quickly
Conductive path, improves the electric conductivity of LCN-Ag composite cathode boundary layers.It is multiple when bringing up to 30 wt% with Ag mass fractions
Condensation material electric conductivity is less than single LCN materials, and there is migration to reunite, reduce particle at high temperature to be primarily due to Ag particles
The trend of surface energy.10 wt% Ag powder favorable dispersibility in LCN matrixes, the presence of ceramic powder can reduce the high temperature of Ag
Diffusion rate, prevents the roughening of Ag powder.With increasing for Ag contents, Ag particle agglomeration phenomenons are more next serious, and to the three-dimensional knots of LCN
Structure produces destruction, is mostly derived from Ag particles and migrates the cavity for leaving at high temperature, and forms big in primary fine powder reuniting
The stress produced to LCN matrixes around during grain.In a preferred embodiment, the LCN-Ag samples of 10 wt% and 20 wt%
Relatively stable performance is shown in 10 thermal cycles.In composite and metal connector interface, Ag particles are uniform
Its surface is dispersed in, the real contact area of composite and connector has been further expanded, electronic conductivity is improve.If
Ag contents increase, and Ag will be with metal connector oxide on surface Cr2O3Chemically react, form substantial amounts of AgCrO2Phase, from
And increase interface contact resistance.In a preferred embodiment, the boundary of display LCN-Ag cathode interfaces material and metal connector
Face is well combined.
Non-chelated polymer is PVA (polyvinyl alcohol), and process for preparation is as follows：First, prepared by the PVA aqueous solution, by 16.5 grams
PVA is immersed in 220 grams of water, and stirring is allowed to fully swelling for 5 hours under normal temperature, and stirring is to being completely dissolved into limpid solution.2nd, divide
Another name amount lanthanum nitrate hexahydrate, cabaltous nitrate hexahydrate, the g of Nickelous nitrate hexahydrate 129.90,52.39 g, 34.90 g, are added to it
In the middle of the PVA aqueous solution of preceding preparation.80oC stirring in water bath obtains well mixed solution in 5 hours, need not in whipping process
Sealing container.Again by high-temperature calcination, LaCo is finally given0.6Ni0.4O3Ceramic powder, can be as sofc cathode afflux material
Material.
In the present invention, above-mentioned LCN-Ag cathode interfaces material both can be used alone, it is also possible to other cathode contacts
Material is jointly formed sandwich construction and uses.Those skilled in the art can suitably select the calciner of LCN according to actual needs
The ratio of Ag in skill and composite so that it is not enough to solve perovskite structure ceramic high temperature electric conductivity, and metal Ag prices it is higher,
The problem for being easy to reunite.
Claims (4)
1. a kind of preparation method of compound cathode of solid oxide fuel battery current collecting material, it is characterized in that, Ag particles with LCN
Grain is prepared into LCN-Ag composite cathode boundary materials by mechanical mixture, and Ag is silver, and LCN is ceramics, and the ratio of Ag particles is 5
The size scope of wt% ~ 30 wt%, Ag particle is 0.1 μm ~ 5 μm, the size scope of LCN particles for 0.05 μm extremely
2 μm。
2. the preparation method of a kind of compound cathode of solid oxide fuel battery current collecting material according to claim 1, its
Be characterized in, the LCN particles be dry and calcine using the solution mixed by metal cation, non-chelated polymer and solvent and
Into calcining heat is 700oC~1200 oC, soaking time is that soaking time is 1 ~ 5 h.
3. the preparation method of a kind of compound cathode of solid oxide fuel battery current collecting material according to claim 2, its
It is characterized in that the cation source is nitrate, sulfate or the chlorate of metal, and solution is the PVA aqueous solution, according to PVA hydroxyls
Base is 1 with all metal cation positive charge mol ratios：4 weigh PVA, are 90 in temperatureo12h is stirred under C bath temperatures to obtain
Solution.
4. the preparation method of a kind of compound cathode of solid oxide fuel battery current collecting material according to claim 1, its
It is characterized in that the mechanical mixture is polishing treatment Ag particles and LCN particles, and is used as by ethyl cellulose and terpinol viscous
Agent is tied to bond Ag particles and LCN particles.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022013903A1 (en) * | 2020-07-11 | 2022-01-20 | Ｄｏｗａエレクトロニクス株式会社 | Perovskite-type composite oxide powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103811774A (en) * | 2014-02-28 | 2014-05-21 | 南京工业大学 | Electrocatalyst with mixed precious metal and perovskite oxides |
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2017
- 2017-04-21 CN CN201710263582.6A patent/CN106935879A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103811774A (en) * | 2014-02-28 | 2014-05-21 | 南京工业大学 | Electrocatalyst with mixed precious metal and perovskite oxides |
Non-Patent Citations (2)
| Title |
|---|
| AYHAN SARIKAYA: "Silver composites as a high stable cathode current collectors for solid oxide fuel cell", 《MATERIALS RESEARCH SOCIETY》 * |
| 王方中: "固体氧化物燃料电池LaCo0.6Ni0.6O(3-δ)接触材料及Pd催化阴极反应动力学研究", 《中国博士学位论文全文数据库 工程科技Ⅱ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022013903A1 (en) * | 2020-07-11 | 2022-01-20 | Ｄｏｗａエレクトロニクス株式会社 | Perovskite-type composite oxide powder |
| CN115768727A (en) * | 2020-07-11 | 2023-03-07 | 同和电子科技有限公司 | Perovskite-type composite oxide powder |
| JP7474328B2 (en) | 2020-07-11 | 2024-04-24 | Ｄｏｗａエレクトロニクス株式会社 | Perovskite-type composite oxide powder |
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