CN108054408A - A kind of solid-oxide fuel cell stack compression sealing material and preparation method thereof - Google Patents
A kind of solid-oxide fuel cell stack compression sealing material and preparation method thereof Download PDFInfo
- Publication number
- CN108054408A CN108054408A CN201711351914.2A CN201711351914A CN108054408A CN 108054408 A CN108054408 A CN 108054408A CN 201711351914 A CN201711351914 A CN 201711351914A CN 108054408 A CN108054408 A CN 108054408A
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- Prior art keywords
- fuel cell
- sealing
- solid
- oxide fuel
- sealing material
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Classifications
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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
-
- 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
- H01M8/24—Grouping of fuel cells, e.g. stacking of fuel cells
- H01M8/2465—Details of groupings of fuel cells
-
- 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
Abstract
The invention discloses a kind of solid-oxide fuel cell stack compression sealing materials and preparation method thereof, and h BN base sealing materials are compounded to form by 80~100wt%h BN ceramics and 0~20wt% glass micro mists；The h BN base sealing materials thickness is 0.25~0.3mm；The h BN ceramics particle size is 5~8 μm, and coefficient of thermal expansion is 10.3 × 10 6K 1；The glass micro mist selects SiO2 Na2O K2O3 systems, and average grain diameter is 5 μm.The present invention adds the glass micro mist of different proportion using h BN bases sealing materials as matrix, realizes reliable sealing of the sealing material in pile, can effectively reduce the leak rate of sealing material, improves its mechanical behavior under high temperature, and then provides excellent sealing effect.
Description
Technical field
The invention belongs to energy technology fields, and in particular to a kind of solid-oxide fuel cell stack compression sealing material
Material and preparation method thereof.
Background technology
Solid oxide fuel cell is that the chemical energy in fuel is converted into a kind of power generator of electric energy, thermoelectricity
Alliance can improve transfer efficiency to 80%.In terms of domestic and international research tendency, middle low temperature flat solid oxide fuel cell
It is the mainstream of current research, advantage is mainly that monocell power density is high, production cost is low.Solid oxide fuel cell electricity
Heap is mainly in series by monocell and connector, and operating temperature is between 600 DEG C to 850 DEG C, by applying elevated-temperature seal material
Expect to realize sealing and the dual function to insulate between monocell and connector.Solid oxide fuel cell is in the process of running
Its monocell anode-side is passed through fuel gas, and cathode side is passed through air.To ensure the normal work of solid oxide fuel cell,
Sealing material must provide enough air-tightness, and with anode both sides gas infiltration does not occur for barrier cathode with mixing.In addition, sealing
Material also need to possess chemical compatibility between long-time stability, heat-resisting cyclicity, adjacent component and manufacture it is at low cost,
The features such as reliability height.
At present, the encapsulating method of flat solid oxide fuel cell is broadly divided into two kinds, compressive seal and hard close
Envelope.Compressive seal refers to fit closely sealing material and monocell/metal disjunctor by applying external pressure, so as to fulfill
Relative sliding can occur for dynamic sealing, seal interface without destroying air-tightness.This kind of sealing means are to sealing material with treating
Matched coefficients of thermal expansion between the component of sealing is of less demanding.Mainly there is mica using more compressive seal material at present
With ceramic base sealing material.Mica, which need to apply very huge pressing stress, could maintain good air-tightness, but pressure excessive in practical operation
Stress can cause monocell to rupture.In addition, in During Process of Long-term Operation, potassium element will volatilize pile in mica, and sink
Product is in cell cathode, so as to seriously affect solid-oxide fuel battery performance.For mica-based sealing material, curtain coating
Molding ceramic base sealing material is controllable with thickness, structural flexibility, the advantages that being easy to cut, in solid oxide fuel electricity
It is successfully applied in the pile of pond.However, ceramic base sealing material or the ceramic blankets impregnated of a large amount of fine solid particles
Enough sealings could be provided by also needing larger impressed pressure, at low pressures, the interfacial seal of ceramic base sealing material
Effect is undesirable, it is difficult to ensure that effective sealing in solid oxide fuel cell operational process.
Hard sealing refers to carry out hardwired mode between sealing material and sofc assemblies, work
Sealing material is not plastically deformed in the process, but the gap between adjacent component is filled by the hot mastication of glass.This
Class sealing material air-tightness is excellent, and most popular at present is glass and glass-ceramic seals.In glass sealing material
Glass belongs to thermodynamics metastable phase, and under the conditions of long term high temperature, thus the trend of oriented more stable crystal transition may be brought
The variations such as volume, coefficient of thermal expansion, internal stress, so as to shorten service life, it is impossible to solid oxide fuel cell be effectively ensured
Effective sealing in operational process.
The content of the invention
More than the deficiencies in the prior art are based on, technical problem solved by the invention is to provide a kind of soild oxide combustion
Expect battery pile compression sealing material and preparation method thereof, using h-BN bases sealing material as matrix, add different proportion
Glass micro mist realizes reliable sealing of the sealing material in pile, can effectively reduce the leak rate of sealing material, it is high to improve it
Warm mechanical property, and then excellent sealing effect is provided.
In order to solve the above-mentioned technical problem, the present invention is achieved through the following technical solutions：The present invention provides a kind of solid
Oxide fuel battery pile compression sealing material, by 80~100wt%h-BN ceramics and 0~20wt% glass micro mists
It is compounded to form h-BN base sealing materials.
Preferably, the h-BN bases sealing material is by 85~100wt%h-BN ceramics and 0~15wt% glass micro mists
It is compounded to form.
Further, the h-BN bases sealing material thickness is 0.25~0.3mm.
Further, the h-BN ceramics particle size is 5~8 μm, and coefficient of thermal expansion is 10.3 × 10-6K-1；
The glass micro mist selects SiO2-Na2O-K2O3System, average grain diameter are 5 μm.
Correspondingly, the present invention provides a kind of preparation sides of solid-oxide fuel cell stack compression sealing material
Method is prepared using solid-oxide fuel cell stack such as described in any one of the above embodiments compression sealing material, including walking as follows
Suddenly：
S1, mixed using absolute ethyl alcohol with dimethylbenzene as solvent, add in dispersant, binding agent is uniformly mixed；
S2, h-BN ceramics and glass micro mist are prepared into slurry progress as the mixed solvent in solute and step S1
Ball milling；
S3, the thin slice green body that the slurry after ball milling in step S2 is prepared to h-BN base sealing materials using moulding process.
Further, the moulding process for curtain coating, roll film or spraying in one kind.
Preferably, the moulding process uses casting molding processes.
Further, thin slice green body obtained by step S3 is placed in Sealing furnace, applies the pressure of 0.03~0.2Mpa, set
Temperature program carries out air tightness test.
Further, the step S3 comprises the following steps：
S31, by thin slice green body cut into needed for size sealing strip, in for solid-oxide fuel cell stack before
Precompressed is carried out to sealing strip；
S32, sealing strip is placed directly against to the region for needing to seal in battery pile.
Further, the step S32 comprises the following steps：
S321, the connector pedestal with gas passage is placed in first layer, sealing strip is sticked on connector pedestal both sides；
S322, monocell is placed on sealing strip, monocell surrounding is made to be pressed on this layer of sealing strip, again in monocell
Metal connector is placed on top, and pastes second layer sealing strip on metal connector periphery, then puts second layer monocell, according to this
Analogize, form battery pile；
S323, apply 70~500kPa on-load pressures in sealing surface direction in battery pile external vertical, be to slowly warm up to solid
The sealing of battery pile can be realized in oxide body temperature of fuel cell.
It is close containing h-BN bases described in any one of the above embodiments the present invention also provides a kind of solid-oxide fuel cell stack
Closure material.
Compared with prior art, the present invention has the advantages that：
Enhance its h-BN internal bond strength by adding in a certain amount of glass dust in the h-BN ceramics lamellas of the present invention；Solid
Oxide body temperature of fuel cell, with glass micro mist there are a degree of sintering, ideal state is h-BN ceramics
The glass micro mist of addition softens in operating temperature range to be tightly combined between ceramic, is made under the driving of thermal stress
The glass that must soften blocks leakage path to migration at leakage path；On the basis of sealing material body sealing performance is improved,
The deformability of sealing material is enhanced to a certain extent.
The present invention by the h-BN ceramic substrates of tape casting, as in solid-oxide fuel cell stack using possible
Sealing material in the operating condition, has ceramic layered main body and the composite construction of glass metal phase surface, can meet sealing material
The multiple requestings such as high-temperature insulating quality, structural stability and the interfacial seal of material；Further to reduce h-BN base sealing materials
Released gas rate can add in a small amount of glass ingredient to reduce the gas leakage path inside sealing material wherein；This is close
Closure material and encapsulating method are of low cost, prepare that simple, stable quality is reliable, are suitable for industrialized mass and prepare.
Description of the drawings
Fig. 1 is the structure diagram of the solid-oxide fuel battery stack sealing of the present invention；
Fig. 2 is the coefficient of thermal expansion variation with temperature curve of h-BN ceramics；
Fig. 3 is h-BN ceramics and the size distribution curve of glass micro mist；
Fig. 4 be h-BN base sealing materials at a temperature of different operating leak rate with venting pressure variation diagram；
The variation for the released gas rate that Fig. 5 is h-BN bases sealing material between 300 DEG C to 750 DEG C under thermal cycle conditions becomes
Gesture figure；
Fig. 6 is the interfacial seal mechanism schematic diagram that h-BN base sealing materials vary with temperature；
Fig. 7 is h-BN bases sealing material and monocell anode and the sealing state sectional view of metal connector.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further described.The specific embodiment of this description is only used for explaining the present invention, is not used to limit this hair
It is bright.In addition, as long as technical characteristic involved in the various embodiments of the present invention described below is not formed each other
Conflict can be mutually combined.
The preparation of example 1~4h-BN base sealing materials
According to the raw material proportioning in table 1,100g weighs required raw material respectively in an amount.300g oxidations are added in into ball grinder
Zirconium ball is mixed as solvent with xylene solution using ethyl alcohol as ball-milling medium, using herring oil as dispersant, adds in powder ball
After grinding 12h, with polyvinyl butyral (PVB) for binding agent, poly- alkyl glycol and butyl benzyl are plasticizer, and cyclohexanone is
Defrother is added in mixed slurry adds in a certain amount of solvent continuation ball milling for 24 hours again after ball milling 12h；In mechanical milling process with
ZrO2Ball is ball-milling medium, and ball milling pearl is about 3 with the ratio for adding in powder:1, vacuum is removed after ball milling becomes homogeneous slurry
Gas is cast the plain embryo to form that thickness is controllable, surface is smooth using accurate casting machine；Treat that organic matter volatilization is dried and can tested
With h-BN base sealing materials.
The biscuit that sealing material prepared by above-mentioned steps is cast is placed in Sealing furnace, applies certain on-load pressure, about
0.03-0.2MPa, sets temperature program to carry out air tightness test, and test result is as shown in Figure 4.
The raw material proportioning of 1 sealing material of table
Specifically, the implementation of solid-oxide fuel battery stack sealing
As shown in Figure 1, the h-BN base sealing materials prepared in example 4 are cut into the sealing strip of desired size；It will carry
The connector pedestal of gas passage is placed in first layer, is plated in first layer sealing strip in the position for being intended to placing battery monomer, puts electricity
Pond monomer, the periphery of battery cell is just pressed on this layer of sealing strip, then is plated in second layer sealing strip on the periphery of battery cell,
Then second layer metallic interconnection materials are put, repave deposited third layer sealing material, and so on, form battery pile.Outside battery pile
Portion applies 0.2MPa pressure perpendicular to sealing direction, works by heating rate to the solid oxide fuel cell of 1 DEG C/min warm
Degree, you can realize the sealing of battery pile.
As shown in Figure 2 and Figure 3, the raw material of the h-BN bases sealing material includes lamellar h-BN micro mists and glass micro mist,
Middle h-BN lamellas micro mist size is about 5~8 μm, and coefficient of thermal expansion (CTE) is about 10.3 × 10-6K-1.Glass micro mist selects
Coefficient of thermal expansion is matched with particle size, such as SiO2-Na2O-K2O3System.To maintain the high temperature of h-BN base sealing materials
The mass percent of mechanical property, wherein glass micro mist is less than 20wt%, as shown in Figure 1, being the soild oxide combustion of the present invention
Expect the structure diagram of battery pile sealing, the position of sealing material in the present invention is illustrated in Fig. 1.Wherein, 1 is " anode, electrolysis
The monocell of matter and cathode " triad, 2 be the position of sealing material in the present invention, and 3 be the metal connection for connecting monocell
Body, 4 be the pedestal of solid oxide fuel cell pile, and 5 be fuel inlet in solid oxide fuel cell pile, and 6 be combustion
Material outlet.
As shown in Figure 1, solid-oxide fuel cell stack is in series in vertical direction by monocell, in monocell
It is sealed between metal connector using the sealing material of the present invention, then applies appropriate pressure and pressurize to pile
Sealing.
In solid oxide fuel cell working condition, h-BN bases sealant surface can generate B2O3Liquid phase film, high viscosity
B2O3Liquid phase film can infiltrate metal connector or monocell surface, good interface connection and sealing be realized, so as to improve h-
The air-tightness of BN base sealing materials.In addition, glass ingredient melts and effectively can reduce or even disappear in the operating condition in sealing material
Except thermal stress, increase the combination power between sealing material and adjacent component, improve mechanical performance.
To obtain the material with said structure, since selected glass can be soft in solid oxide fuel cell operating temperature
Change, under impressed pressure effect, the liquid phase that h-BN ceramics generate mutually is combined closely with glass, improves the disconnected of sealing material
Split energy；On the other hand, there is diffusion with h-BN ceramics interface and even react in glass micro mist, improve glass and ceramics
Intergranular bond strength, so that the mechanical property of material is further promoted.If the excessive glass micro mist of addition, glass
The problem of glass state, can display, such as glass is easy to the characteristic of crystallization, is cracked in cold cycling；Thus select glass
Ratio of the quality of micro mist in h-BN ceramics and glass micro mist gross mass should be less than 15wt%, to maintain the skeleton of h-BN
Structure；The preferred proportion of h-BN ceramics-glass base composite sealing materials is 0~15wt%.
The B that h-BN bases sealant surface of the present invention is formed2O3Liquid phase film has adjacent monocell with metal connector good
Good immersional wetting；B2O3Fusing point be 577 DEG C, in solid oxide fuel cell operating temperature, h-BN base sealant surfaces
There are B2O3Liquid phase film；Below 1000 DEG C, B2O3Liquid film can prevent oxygen from being diffused to by air inside h-BN, so as to be formed with
The oxygen diffusion barrier layer of effect prevents the further oxidation inside h-BN ceramics；It will make B higher than 1000 DEG C2O3Saturated vapor pressure increase
Add, promote liquid B2O3Part is volatilized, and destroys the integrality of oxygen diffusion barrier layer；Due to h-BN high temperature can in air
Oxygen recurs chemical reaction, forms a large amount of B2O3Phase, in thermal analysis curve it can be seen that, when h-BN samples in air atmosphere
It is present with the phenomenon that drastically increases weight higher than 1000 DEG C, and corresponding exothermic peak occurs in DTA, this illustrates h-BN ceramics at this time due to oxygen
The destruction of diffusion barrier layer causes a large amount of B2O3Mutually it is formed continuously.Therefore, h-BN as sealing material in solid oxide fuel
Use should select suitable operating temperature in battery, avoid the B of h-BN oxidation generations2O3Volatilization ensures B2O3The structure of liquid film is complete
Whole property.Highly viscous B2O3 liquid phases film can effectively infiltrate metal connector and monocell surface, realize that reliable interface connects
It connects, improves the air-tightness of h-BN base sealing materials.
According between adjacent component in sealing material obtained in the embodiment of the present invention and solid-oxide fuel cell stack
With good matched coefficients of thermal expansion；As shown in Fig. 2, from room temperature to 750 DEG C, h-BN ceramics coefficient of thermal expansion is about 10.3
×10-6K-1, this and common metal connector Fe-16Cr alloys (12 × 10-6K-1) and single-celled electrolyte 8YSZ (10.5 ×
10-6K-1) similar thermal expansion coefficient, caused by can effectively alleviating the thermal expansion mismatch between adjacent component thermal stress concentrate,
And the interfacial gases leakage thus triggered.
The above is the preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, it is noted that for the professional technician of the art, without departing from the principle of the present invention, may be used also
To make several improvement and variation, these are improved and variation is also considered as protection scope of the present invention.
Claims (10)
1. a kind of solid-oxide fuel cell stack compression sealing material, which is characterized in that made pottery by 80~100wt%h-BN
Porcelain micro mist and 0~20wt% glass micro mists are compounded to form h-BN base sealing materials.
2. solid-oxide fuel cell stack as described in claim 1 compression sealing material, which is characterized in that the h-
BN bases sealing material is compounded to form by 85~100wt%h-BN ceramics and 0~15wt% glass micro mists.
3. solid-oxide fuel cell stack as claimed in claim 1 or 2 compression sealing material, which is characterized in that institute
H-BN base sealing materials thickness is stated as 0.25~0.3mm.
4. solid-oxide fuel cell stack as claimed in claim 1 or 2 compression sealing material, which is characterized in that institute
H-BN ceramics particle size is stated as 5~8 μm, coefficient of thermal expansion is 10.3 × 10-6K-1；The glass micro mist selection
SiO2-Na2O-K2O3System, average grain diameter are 5 μm.
5. a kind of preparation of the solid-oxide fuel cell stack compression sealing material as described in any in 1-4 such as claim
Method, which is characterized in that include the following steps：
S1, mixed using absolute ethyl alcohol with dimethylbenzene as solvent, add in dispersant, binding agent is uniformly mixed；
S2, h-BN ceramics and glass micro mist are prepared into slurry progress ball as the mixed solvent in solute and step S1
Mill；
S3, the thin slice green body that the slurry after ball milling in step S2 is prepared to h-BN base sealing materials using moulding process.
6. the solid-oxide fuel cell stack as claimed in claim 5 preparation method of compression sealing material, feature
Be, the moulding process for curtain coating, roll film or spraying in one kind.
7. the solid-oxide fuel cell stack as claimed in claim 6 preparation method of compression sealing material, feature
It is, thin slice green body obtained by step S3 is placed in Sealing furnace, apply the pressure of 0.03~0.2Mpa, temperature program is set to carry out
Air tightness test.
8. the solid-oxide fuel cell stack as claimed in claim 5 preparation method of compression sealing material, feature
It is, the step S3 comprises the following steps：
S31, by thin slice green body cut into needed for size sealing strip, in for solid-oxide fuel cell stack before to close
Strip of paper used for sealing carries out precompressed；
S32, sealing strip is placed directly against to the region for needing to seal in battery pile.
9. the solid-oxide fuel cell stack as claimed in claim 8 preparation method of compression sealing material, feature
It is, the step S32 comprises the following steps：
S321, the connector pedestal with gas passage is placed in first layer, sealing strip is sticked on connector pedestal both sides；
S322, monocell is placed on sealing strip, monocell surrounding is made to be pressed on this layer of sealing strip, again on monocell top
Metal connector is placed, and second layer sealing strip is pasted on metal connector periphery, then puts second layer monocell, according to this class
It pushes away, forms battery pile；
S323, apply 70~500kPa on-load pressures in sealing surface direction in battery pile external vertical, be to slowly warm up to solid oxygen
The sealing of battery pile can be realized in compound temperature of fuel cell.
10. a kind of solid-oxide fuel cell stack contains the h-BN base sealing materials described in claim 1 or 2.
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| CN201711351914.2A CN108054408A (en) | 2017-12-15 | 2017-12-15 | A kind of solid-oxide fuel cell stack compression sealing material and preparation method thereof |
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| CN201711351914.2A CN108054408A (en) | 2017-12-15 | 2017-12-15 | A kind of solid-oxide fuel cell stack compression sealing material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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|---|---|---|---|---|
| CN101079476A (en) * | 2007-06-20 | 2007-11-28 | 华中科技大学 | A sealing material of solid oxide fuel cell and its sealing method |
| CN102723448A (en) * | 2012-05-22 | 2012-10-10 | 华中科技大学 | Sealing material of medium temperature plate type solid-oxide fuel battery stack and sealing method |
| CN104505527A (en) * | 2014-11-14 | 2015-04-08 | 华中科技大学 | Medium temperature flat type solid oxide fuel cell pile sealing object and preparation method thereof |
| CN106699136A (en) * | 2016-12-27 | 2017-05-24 | 华中科技大学 | Method for manufacturing sealing material |
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2017
- 2017-12-15 CN CN201711351914.2A patent/CN108054408A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101079476A (en) * | 2007-06-20 | 2007-11-28 | 华中科技大学 | A sealing material of solid oxide fuel cell and its sealing method |
| CN102723448A (en) * | 2012-05-22 | 2012-10-10 | 华中科技大学 | Sealing material of medium temperature plate type solid-oxide fuel battery stack and sealing method |
| CN104505527A (en) * | 2014-11-14 | 2015-04-08 | 华中科技大学 | Medium temperature flat type solid oxide fuel cell pile sealing object and preparation method thereof |
| CN106699136A (en) * | 2016-12-27 | 2017-05-24 | 华中科技大学 | Method for manufacturing sealing material |
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| 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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