CN108110277A - A kind of preparation method of solid oxide fuel cell seal pad - Google Patents
A kind of preparation method of solid oxide fuel cell seal pad Download PDFInfo
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- CN108110277A CN108110277A CN201611050269.6A CN201611050269A CN108110277A CN 108110277 A CN108110277 A CN 108110277A CN 201611050269 A CN201611050269 A CN 201611050269A CN 108110277 A CN108110277 A CN 108110277A
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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
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/028—Sealing means characterised by their material
- H01M8/0282—Inorganic material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
- C04B37/025—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of glass or ceramic material
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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
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/0276—Sealing means characterised by their form
-
- 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
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/0286—Processes for forming seals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/10—Glass interlayers, e.g. frit or flux
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Electrochemistry (AREA)
- Sustainable Energy (AREA)
- Sustainable Development (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Structural Engineering (AREA)
- Fuel Cell (AREA)
Abstract
A kind of preparation method of solid oxide fuel cell seal pad, it is characterised in that using glass as sealing basic material, biscuit is made by the method for tape casting；Using NiO, YSZ, LSM, (Mn, Co)3O4Powder is waited to be coated on biscuit upper and lower surface as needed as coating material.After drying to be coated, gasket is placed in the position to be sealed of two components to be sealed, is warming up to more than the softening temperature of glass to realize sealing in electric furnace.Sealing cushion raw material of the present invention is simple, prepare and uses process convenient, at low cost, and the chemical compatibility that the use of coating can be between composite enhancement and battery component, reduces the thermal stress at seal interface in Thermal Cycling, so as to improve sealing effect.
Description
Technical field
The present invention relates to a kind of preparation method of elevated-temperature seal pad, especially suitable for solid oxide fuel cell (SOFC)
High intermediate temperature sealing between ceramic component and stainless steel connector.
Background technology
Solid oxide fuel cell (SOFC) is a kind of green cleaning, safe and reliable energy conversion device, will be stored
Chemical energy in fuel is directly translated into electric energy without Carnot cycle, substantially increases the utilization rate of fuel.In recent years
Come, all had made great progress in terms of critical material, the system integration, but the elevated-temperature seal problem of battery is not yet resolved,
This is also one of principal element for limiting SOFC commercialization processes.
In SOFC systems, the main function of sealing material is to provide reliable sealing, ensures that oxygen and fuel gas are not sent out
Raw to mix and to outward leakage, connection monocell provides certain machinery surely into a complete system under battery operating temperature
It is qualitative.This requires sealing materials with good air-tightness, good thermal matching and chemical compatibility between adjacent component,
Long-time stability etc. under oxidation and reducing atmosphere.
Main sealing means have means of press seals and hard sealing.Means of press seals refers to sealing material and part to be sealed by external force
It compresses to realize sealing, research at present is concentrated mainly on mica material.The accurate heat of storeroom is not required in the sealing means
Match somebody with somebody, but the introducing of pressue device increases the complexity of system.Hard sealing refers to carry out between sealing material and component to be sealed hard
Connection, sealing material cannot generate the sealing means of plastic deformation after sealing.Common material mainly has metal (such as brazing, silver
Slurry, alloy etc.), glass, glass-ceramic etc..Wherein, metal material is good with good toughness, sealing strength height and thermal circulation performance
The advantages that, but metal material is easily oxidised in use, need to do insulation processing.Glass and glass-ceramic, which have, to be prepared
Simply, the advantages that of low cost, thus as widely studied and application object.
Patent CN1469497A, CN1660954A, CN1494176A etc. disclose silicate glass, sillico aluminate glass and
Borosilicate glass obtains the suitable sealing material of high mechanical strength, good insulating, the coefficient of expansion, suitable for high temperature
The sealing of SOFC.But continual crystallization will cause the change of material expand coefficient to glass at high temperature, cause seal interface
Place generates stress, so as to influence sealing effect.To solve this problem, patent CN102699561A, CN101079476A,
CN101684034A, CN103570372A etc. disclose the composite seals such as glass-metal or glass-ceramic.Which profit
Sealing is realized with the softening of glass, and metal or ceramic fillers provide necessary mechanical strength, avoid glass at high temperature
Excess flow.But when using glass-metal or glassceramic composites, the consistency problem between different component is not allowed to neglect
Depending on.When the coefficient of expansion difference of two kinds of materials is big or severe reaction occurs, it will generate stress in interface, influence material sheet
The stability and sealing effect of body.
To solve the problems, such as that glass-metal or two group partition inter-capacitive of glassceramic composites are bad, the present invention uses
Biscuit is made by the method for tape casting as sealing basic material in glass；Using NiO, YSZ, LSM, (Mn, Co)3O4Wait powder
End is respectively coated as needed as coating material in biscuit both sides.After drying to be coated, gasket is placed in portion to be sealed
Position, is warming up to more than the softening temperature of glass to realize sealing in electric furnace.The gasket can composite enhancement and battery unit
Chemical compatibility between part reduces the thermal stress at seal interface in Thermal Cycling, so as to improve sealing effect.
The content of the invention
It is an object of the present invention to for the deficiency of existing sealing technique, overcome chemical between sealing material and adjacent component
The problems such as serious is reacted, a kind of preparation method of solid oxide fuel cell seal pad is provided.
Technical scheme is as follows：
A kind of preparation method of solid oxide fuel cell seal pad, comprises the following steps：
Step 1, glass powder is mixed and ground with solvent, binding agent, dispersant and plasticizer；Wherein, solvent content
For 10~40wt%, binder content is 1~10wt%, and dispersant is 1~10wt%, plasticizer loading for 1~
10wt%；It is 30~40wt% to preferably constitute as solvent content, and binder content is 2~5wt%, dispersant for 2~
5wt%, plasticizer loading are 2~5wt%；
Step 2, the slurry that step 1 is obtained crosses 100~200 mesh sieves, takes the component by sieve, vacuum defoamation；
Step 3, step 2 treated slurry curtain coating and drying and moulding, are made gasket biscuit；
Step 4, coating material powder mixes with solvent and grinds obtained coating paste；
Step 5, coating paste is coated in gasket biscuit upper and lower surface and drying；
Step 6, gasket is placed in the position to be sealed between two components to be sealed, glass is warming up in electric furnace
It more than softening temperature is sealed with realizing.
Glass is silicate glass, borate glass, borosilicate glass, one or both of alumina silicate glass with
On；According to the position of sealing, coating material is respectively NiO, YSZ, LSM, (Mn, Co)3O4One kind in.
Glass powder is mixed and ground with solvent, binding agent, dispersant and plasticizer；Solvent for use is volume ratio 1：1
Ethanol-acetone, volume ratio 1：1 ethanol-toluene or volume ratio 1：Any one in 1 isopropanol-xylene mixture,
Binding agent is polyvinyl butyral (PVB), and dispersant is fish oil, and plasticizer is dioctyl phthalate (DOP).
Coating paste uses volume ratio 1：1 ethylene glycol-polyethylene glycol is solvent；It is coated using the method brushed or sprayed
Coating.
The thickness of glass biscuit is in 0.2~0.8mm scopes, and the thickness of both sides coating material is in 5~20 μ ms.
Glass powder particle size is in 5~20 μ ms；Coating material powder particle size is in 0.1~1 μ m.
More than the softening temperature of glass refer to the softening temperature of glass between+300 degrees Celsius of the softening temperature of glass.
The softening temperature of glass is usually 600-800 degrees Celsius.
Advantage of the invention is that：Using above-mentioned gasket, the stability of sealing material can be improved, is reduced due to thermal expansion
Thermal stress caused by coefficient mismatches, so as to improve the stability at interface.The use of coating enhances sealing material and sealing
Chemical compatibility between part, so as to improve sealing effect.Since gasket material is simple, it is convenient to prepare, can be used in it is plate,
The sealing of the solid oxide fuel cell of a variety of configurations such as cast, flat-tube type.
Specific embodiment
The invention will be further elaborated by the following examples：
Embodiment 1
Step 1, weigh silicate glass powder (constituent content is listed in table 1) 100g, add in 20g ethyl alcohol, 10g acetone,
5gPVB, 5g fish oil, 3gDOP, in being mixed on horizontal ball mill and grind 100h.
Step 2, the slurry that step 1 is uniformly mixed is crossed into 80 mesh sieves, vacuum defoamation 1h is carried out on agitator.
Step 3, treated, and slurry is cast on casting machine and the drying and moulding at 60 DEG C, and it is close for 0.3mm that thickness is made
Packing biscuit.
Step 4,10g NiO and 10g (Mn, Co)3O4Powder is added separately in 5g ethylene glycol-polyethylene glycol solvent, sleeping
It is mixed on formula ball mill and grinds 25h and coating paste is made.
Step 5, slurry is respectively coated on to the both sides of gasket biscuit by the way of brushing, the dry 25h at 60 DEG C.
Step 6, gasket is placed between galvanic anode and connector, 850 DEG C is warming up in electric furnace, is realized to battery
The sealing of anode and connector.
Glass ingredient content (molar content) in 1 each embodiment of table
| SiO2 | B2O3 | Al2O3 | Na2O | MgO | CaO | SrO | BaO | La2O3 | |
| Embodiment 1 | 50 | 0 | 2 | 13 | 0 | 30 | 0 | 0 | 5 |
| Embodiment 2 | 25 | 30 | 2 | 0 | 0 | 0 | 40 | 0 | 3 |
| Embodiment 3 | 45 | 0 | 15 | 0 | 20 | 16.5 | 0 | 0 | 3.5 |
| Embodiment 4 | 43.5 | 0 | 11.9 | 0 | 10 | 0 | 0 | 30 | 4.6 |
Embodiment 2
Step 1, weigh borosilicate glass powder (constituent content is listed in table 1) 100g, add in 18g ethyl alcohol, 12g toluene,
6gPVB, 6g fish oil, 5gDOP, in being mixed on horizontal ball mill and grind 100h.
Step 2, the slurry that step 1 is uniformly mixed is crossed into 80 mesh sieves, vacuum defoamation 1h is carried out on agitator.
Step 3, treated, and slurry is cast on casting machine and the drying and moulding at 60 DEG C, and it is close for 0.3mm that thickness is made
Packing biscuit.
Step 4,10g YSZ and 10g (Mn, Co)3O4Powder is added separately in 6g ethylene glycol-polyethylene glycol solvent, sleeping
It is mixed on formula ball mill and grinds 25h and coating paste is made.
Step 5, slurry is respectively coated on to the both sides of gasket biscuit by the way of brushing, the dry 25h at 60 DEG C.
Step 6, gasket is placed between cell electrolyte and connector, 750 DEG C is warming up in electric furnace, is realized to electricity
The sealing of pond electrolyte and connector.
Embodiment 3
Step 1, weigh sillico aluminate glass powder (constituent content is listed in table 1) 100g, add in 22g ethyl alcohol, 12g acetone,
6gPVB, 6g fish oil, 3gDOP, in being mixed on horizontal ball mill and grind 100h.
Step 2, the slurry that step 1 is uniformly mixed is crossed into 80 mesh sieves, vacuum defoamation 1h is carried out on agitator.
Step 3, treated, and slurry is cast on casting machine and the drying and moulding at 60 DEG C, and it is close for 0.5mm that thickness is made
Packing biscuit.
Step 4,20g (Mn, Co)3O4Powder is added in 15g ethylene glycol-polyethylene glycol solvent, is mixed on horizontal ball mill
Merge grinding 25h and coating paste is made.
Step 5, slurry is coated in the both sides of gasket biscuit by the way of brushing, the dry 25h at 60 DEG C.
Step 6, between gasket being placed in two connectors, 875 DEG C is warming up in electric furnace, is realized to battery connecting structure
Sealing.
Embodiment 4
Step 1, weigh sillico aluminate glass powder (constituent content is listed in table 1) 100g, add in 25g ethyl alcohol, 15g toluene,
6gPVB, 6g fish oil, 5gDOP, in being mixed on horizontal ball mill and grind 100h.
Step 2, the slurry that step 1 is uniformly mixed is crossed into 80 mesh sieves, vacuum defoamation 1h is carried out on agitator.
Step 3, treated, and slurry is cast on casting machine and the drying and moulding at 60 DEG C, and it is close for 0.8mm that thickness is made
Packing biscuit.
Step 4,10g LSM powder and 10g (Mn, Co)3O4Powder is added in 6g ethylene glycol-polyethylene glycol solvent, sleeping
It is mixed on formula ball mill and grinds 25h and coating paste is made.
Step 5, slurry is respectively coated on to the both sides of gasket biscuit by the way of brushing, the dry 25h at 60 DEG C.
Step 6, gasket is placed between cathode and connector, 900 DEG C is warming up in electric furnace, is realized to cell cathode
With the sealing of connector.
Claims (8)
1. a kind of preparation method of solid oxide fuel cell seal pad, which is characterized in that comprise the following steps：
Step 1, glass powder is mixed and ground with solvent, binding agent, dispersant and plasticizer；Wherein, solvent content 10
~40wt%, binder content are 1~10wt%, and dispersant is 1~10wt%, and plasticizer loading is 1~10wt%；It is excellent
Choosing composition be that solvent content is 30~40wt%, and binder content is 2~5wt%, and dispersant is 2~5wt%, plasticizer
Content is 2~5wt%；
Step 2, the slurry that step 1 is obtained crosses 100~200 mesh sieves, takes the component by sieve, vacuum defoamation；
Step 3, step 2 treated slurry curtain coating and drying and moulding, are made gasket biscuit；
Step 4, coating material powder mixes with solvent and grinds obtained coating paste；
Step 5, coating paste is coated in gasket biscuit upper and lower surface and drying；
Step 6, gasket is placed in the position to be sealed between two components to be sealed, the softening of glass is warming up in electric furnace
It more than temperature is sealed with realizing.
2. preparation method as described in claim 1, which is characterized in that glass is silicate glass, borate glass, borosilicic acid
It is more than one or both of salt glass, alumina silicate glass；According to the position of sealing, coating material be respectively NiO, YSZ,
LSM、Mn3O4、Co3O4One or two or more kinds in.
3. preparation method as described in claim 1, which is characterized in that by glass powder and solvent, binding agent, dispersant and increasing
Modeling agent is mixed and ground；Solvent for use is volume ratio 1：1 ethanol-acetone, volume ratio 1：1 ethanol-toluene or volume ratio 1：1
Isopropanol-xylene mixture in any one, binding agent be polyvinyl butyral (PVB), dispersant is fish oil, increase
Modeling agent is dioctyl phthalate (DOP).
4. preparation method as described in claim 1, which is characterized in that coating paste uses volume ratio 1：1 ethylene glycol-poly- second
Glycol is solvent；Using the method applying coating brushed or sprayed.
5. preparation method as described in claim 1, which is characterized in that the thickness of glass biscuit is in 0.2~0.8mm scopes, and two
The thickness of side coating material is in 5~20 μ ms.
6. preparation method as described in claim 1, which is characterized in that glass powder particle size is in 5~20 μ ms；Coating
Material powder particle size is in 0.1~1 μ m.
7. preparation method as described in claim 1, which is characterized in that more than the softening temperature of glass refer to the softening temperature of glass
Degree is between+300 degrees Celsius of the softening temperature of glass.
8. the preparation method as described in claim 1 or 7, which is characterized in that the softening temperature of glass is usually 600-800 Celsius
Degree.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233340A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Glass surface waterproof coating and preparation and application thereof |
| EP3985767A1 (en) * | 2020-10-13 | 2022-04-20 | Instytut Energetyki - Instytut Badawczy | Method of preparation of an intermediate product, intermediate product, and method of manufacturing a gasket |
| CN115000449A (en) * | 2022-06-24 | 2022-09-02 | 西安石油大学 | Method for preparing SOFC (solid oxide Fuel cell) galvanic pile sealing coating by spraying-casting process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233340A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Glass surface waterproof coating and preparation and application thereof |
| EP3985767A1 (en) * | 2020-10-13 | 2022-04-20 | Instytut Energetyki - Instytut Badawczy | Method of preparation of an intermediate product, intermediate product, and method of manufacturing a gasket |
| CN115000449A (en) * | 2022-06-24 | 2022-09-02 | 西安石油大学 | Method for preparing SOFC (solid oxide Fuel cell) galvanic pile sealing coating by spraying-casting process |
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Application publication date: 20180601 |