CN1256779C - Sealing material of solide oxide fuel cell and its sealing method - Google Patents

Sealing material of solide oxide fuel cell and its sealing method Download PDF

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Publication number
CN1256779C
CN1256779C CNB2004100438493A CN200410043849A CN1256779C CN 1256779 C CN1256779 C CN 1256779C CN B2004100438493 A CNB2004100438493 A CN B2004100438493A CN 200410043849 A CN200410043849 A CN 200410043849A CN 1256779 C CN1256779 C CN 1256779C
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China
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sealing
fuel cell
oxide fuel
seal
raw material
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CN1599092A (en
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吕喆
刘超前
苏文辉
刘志国
唐为民
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Harbin Institute of Technology
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Harbin Institute of Technology
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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

Abstract

The present invention discloses sealing material of a solid oxide fuel battery and a sealing method thereof, which relates to sealing material of a solid oxide fuel battery and a sealing method thereof. The sealing material of the present invention is prepared from raw material by the following mol percentage: 3 to 10% of Al2O3, 0 to 20% of BaCO3, 50 to 67% of SiO2, 0 to 15% of CaO, 0 to 15% of Na2CO, 2 to 9% of PbO2, 10 to 20% of B2O3 and 0 to 5% of ZnO. The sealing structure is realized in this way: (1) the raw material is weighed, and after being milled, the raw material is taken out and is dried; (2) the raw material is put in a porcelain crucible for calcining, quenching, pulverizing and screening; (3) after being milled again, the raw material is put in a porcelain crucible for baking, quenching, pulverizing and screening; (4) water is added, and after being milled and dried, the raw material is screened, and sealing material powder is prepared; (5) mud material is blended; (6) sealing strips are pressed; (7) the sealing strips are used; (8) encapsulation is carried out at high temperature, and a solid oxide fuel battery is obtained. The sealing material of the present invention has strong insulating property, and has the advantages of simple preparing and using method, strong adaptability to device shapes, etc.

Description

The seal, sealing materials of Solid Oxide Fuel Cell and method for sealing thereof
Technical field:
The present invention relates to the seal, sealing materials and the encapsulating method thereof of a kind of Solid Oxide Fuel Cell (SOFC).
Background technology:
A kind of " the high temperature seal, sealing materials and the sealing technology of Solid Oxide Fuel Cell " disclosed among the ZL99104482.7, this patent adopts pottery and vitreous material to form composite material, interior seal, sealing materials (ceramic layer) by high resistivity reduces the sealing-in electric leakage and stress and chemistry buffering is provided, and adopts manual smearing on the method for packing; " a kind of method of using metallic conductive glue to proceed solid oxide fuel cell fast sealing " disclosed in ZL02133049.2, this patent adopts metal material to carry out the sealing of SOFC, seal, sealing materials itself has very strong conductivity, and encapsulation operation also is manual smearing; ZL02147179.7 discloses " a kind of Solid Oxide Fuel Cell high temperature seal, sealing materials and method for sealing ", and it adopts rolling formation, strikes out the special shape that needs, and the material prescription system is CaO-MgO-SiO 2-Fe 2O 3-B 2O 3-ZrO 2-Y 2O 3
Summary of the invention:
The seal, sealing materials and the method for sealing thereof that the purpose of this invention is to provide a kind of Solid Oxide Fuel Cell, the high temp glass attitude material and the preformation method that adopt the present invention to propose are made flexible sealing-in parts, be used for the encapsulation of SOFC, have preparation simple with using method, to advantages such as device shape adaptability are strong.The seal, sealing materials of Solid Oxide Fuel Cell of the present invention (high temp glass attitude material) is made up of the raw material of following molar percentage: Al 2O 33～10%, BaCO 30～20%, SiO 250～67%, CaO0～15%, Na 2CO 30～15%, PbO 22～9%, B 2O 310～20%, ZnO0～5%, its physical function parameter sees Table 1.The method for sealing of Solid Oxide Fuel Cell is as follows: (1) is Al according to molar percentage 2O 33～10%, BaCO 30～20%, SiO 250～67%, CaO0～15%, Na 2CO 30～15%, PbO 22～9%, B 2O 310～20%, the ratio of ZnO0～5% takes by weighing above-mentioned raw materials, adds the ball grinder ball milling 2～24 hours of packing into behind the water, and wherein the mass ratio of raw material gross mass and water is 1: (1～3), take out oven dry; (2) during the powder behind the ball milling is packed porcelain crucible into, respectively calcined 2～6 hours at 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃ and 750 ℃ respectively, the crucible that powder is housed is directly taken out from stove, at quenching-in water, pulverize then, sieve; (3) the ball milling porcelain crucible of packing into after 2～24 hours again of the powder after will sieving 800～1000 ℃ of roastings 6～8 hours, directly takes out the crucible that powder is housed from stove, at quenching-in water, pulverizes then, sieves; (4) powder after will sieving adds the ball grinder ball milling 6～8h that packs into behind the water, sieves after the oven dry, makes the seal, sealing materials powder; (5) be 1 with cellulose and terpinol by mass ratio: the mixed of (10～25) is soaked 8～10h, form binder solution, add the seal, sealing materials powder then and mix, obtain pug, wherein the mass ratio of seal, sealing materials powder and binder solution is (1～4): 1; (6) pug was pressed between twin pressure roller, forming thickness is the slice of 1～5mm, and lining paper is pasted in the roll extrusion simultaneously of the two sides of slice, and slice is again by having two roller roll extrusion sliverings of emboss pit then; (7) cutting sealing bar is thrown off sealing strip protection lining paper bar simultaneously, is heated to 30～40 ℃, and the sealing strip that will throw off lining paper one side then is bonded at the zone of sealing-in, assembling fuel cell parts, pressurization at last; (8) battery of finishing assembling is placed in the stove in 80～100 ℃ of pre-burnings 0.5～1 hour, first speed by 2～5 ℃/min is warming up to 130～150 ℃ in high temperature furnace then, be incubated 0.5～1 hour, speed by 2～5 ℃/min is warmed up to 200～250 ℃ again, be incubated 0.5～1 hour, speed with 3 ℃/min directly is warmed up to 800～900 ℃ at last, be incubated 2～4 hours, cool to 750 ℃, 700 ℃ and 650 ℃ and be incubated 1 hour respectively with the speed of 1 ℃/min subsequently, cool to room temperature with 2 ℃/min speed at last, take out and obtain Solid Oxide Fuel Cell.The seal, sealing materials of SOFC must have and and the approaching thermal coefficient of expansion (8.0 * 10 of its contacted parts -6K -1～12.0 * 10 -6K -1).Glassy state can soften under higher temperature, viscosity descends and then fusing, under molten state, finish the sealing-in process, the fusing sealing temperature exceeds 50～100 ℃ of the working temperatures (500～1000 ℃) of SOFC, at the SOFC that works 500～800 ℃ middle temperature, its sealing temperature is near 850～900 ℃.The present invention has overcome used in the past seal, sealing materials and has had very strong conductivity, manual application efficient is low, encapsulant is in uneven thickness shortcoming.This method both had been suitable for the encapsulation of SOFC, also can be used for the repairing of SOFC parts crackle.In use, the shape of sealing strip can be arbitrarily crooked according to demand, so just can adapt to different needs, and need not redesign and process black box; This method is highly suitable for the trial production of laboratory research and small lot, also can be used as the replenishing of black box of large-scale production.
Table 1
Conversion temperature T g(K) softening temperature T s(K) fusion temperature T m＝T g(3/2) (K) thermal coefficient of expansion (50～500) ℃ (* 10 -6·K -1) 810～830 830～842 1210～1240 7.5～11
Description of drawings:
Fig. 1 is a SOFC sealing strip preparation process of the present invention, and Fig. 2 is the SOFC encapsulation process.
Embodiment:
Embodiment one: the seal, sealing materials of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 33～10%, BaCO 30～20%, SiO 250～67%, CaO0～15%, Na 2CO 30～15%, PbO 22～9%, B 2O 310～20%, ZnO0～5%.
Embodiment two: the seal, sealing materials of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 33～10%, BaCO 35～20%, SiO 250～67%, PbO 22～9%, B 2O 310～20%, ZnO0～5%.
Embodiment three: the seal, sealing materials of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 33～10%, SiO 250～67%, CaO5～15%, Na 2CO 30～15%, PbO 22～9%, B 2O 310～20%, ZnO0～5%.
Embodiment four: the seal, sealing materials of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 34～5%, BaCO 31～5%, SiO 258～64%, CaO8～14%, Na 2CO 37～13%, PbO 23～5%, B 2O 311～14%, ZnO1～2%.
Embodiment five: the seal, sealing materials of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 36～9%, BaCO 36～15%, SiO 251～56%, CaO1～6%, Na 2CO 31～6%, PbO 26～8%, B 2O 315～19%, ZnO3～4%, its physical function parameter sees Table 2.
Embodiment six: the seal, sealing materials AF1 of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 34%, BaCO 32%, SiO 259%, CaO12%, Na 2CO 38%, PbO 24%, B 2O 310%, ZnO1%, its physical function parameter sees Table 2.
Embodiment seven: the seal, sealing materials AF2 of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 37%, BaCO 38%, SiO 254%, CaO3%, Na 2CO 32%, PbO 27%, B 2O 316%, ZnO3%, its physical function parameter sees Table 2.
Embodiment eight: the seal, sealing materials AF3 of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 38%, BaCO 35%, SiO 262%, PbO 28%, B 2O 317%, its physical function parameter sees Table 2.
Embodiment nine: the seal, sealing materials AF4 of the Solid Oxide Fuel Cell of present embodiment is made up of the raw material of following molar percentage: Al 2O 39%, SiO 261%, CaO7%, Na 2CO 33%, PbO 24%, B 2O 313%, ZnO3%, its physical function parameter sees Table 2.
Table 2
Sample AF1 AF2 AF3 AF4
Conversion temperature T g(K) softening temperature T s(K) fusion temperature T m＝T g(3/2) (K) thermal coefficient of expansion (50～500 ℃) (* 10 -6·K -1) 816.5 841.0 1224.8 8.67 822.4 840.4 1233.6 8.88 816.0 839.5 1224.0 7.74 811.5 838.5 1217.3 8.58
Embodiment ten: the method for sealing of the Solid Oxide Fuel Cell of present embodiment carries out according to following step: (1) is Al according to molar percentage 2O 33～10%, BaCO 30～20%, SiO 250～67%, CaO0～15%, Na 2CO 30～15%, PbO 22～9%, B 2O 310～20%, the ratio of ZnO0～5% takes by weighing above-mentioned raw materials, adds the ball grinder ball milling 2～24 hours of packing into behind the water, and wherein the mass ratio of raw material gross mass and water is 1: (1～3), take out oven dry; (2) during the powder behind the ball milling is packed porcelain crucible into, respectively calcined 2～6 hours at 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃ and 750 ℃ respectively, the crucible that powder is housed is directly taken out from stove, at quenching-in water, pulverize then, sieve; (3) the ball milling porcelain crucible of packing into after 2～24 hours again of the powder after will sieving 800～1000 ℃ of roastings 6～8 hours, directly takes out the crucible that powder is housed from stove, at quenching-in water, pulverizes then, sieves; (4) powder after will sieving adds the ball grinder ball milling 6～8h that packs into behind the water, sieves after the oven dry, makes the seal, sealing materials powder; (5) be 1 with cellulose and terpinol by mass ratio: the mixed of (10～25) is soaked 8～10h, form binder solution, add the seal, sealing materials powder then and mix, obtain pug, wherein the mass ratio of seal, sealing materials powder and binder solution is (1～4): 1; (6) pressed between twin pressure roller practicing the pug that makes, forming thickness is the slice of 1～5mm, and lining paper is pasted in the roll extrusion simultaneously of the two sides of slice, and slice is again by having two roller roll extrusion sliverings of emboss pit then; (7) cutting sealing bar is thrown off sealing strip protection lining paper bar simultaneously, is heated to 30～40 ℃, then sealing strip is bonded at the zone of sealing-in, assembling fuel cell parts, pressurization at last; (8) battery of finishing assembling is placed in the stove in 80～100 ℃ of pre-burnings 0.5～1 hour, first speed by 2～5 ℃/min is warming up to 130～150 ℃ of insulations 0.5～1 hour in high temperature furnace then, speed by 2～5 ℃/min is warmed up to 200～250 ℃ of insulations 0.5～1 hour again, speed with 3 ℃/min directly is warmed up to 800～900 ℃ at last, be incubated 2～4 hours, cool to 750 ℃, 700 ℃ and 650 ℃ and be incubated 1 hour respectively with the speed of 1 ℃/min subsequently, cool to room temperature with 2 ℃/min speed at last, take out and obtain Solid Oxide Fuel Cell.
Embodiment 11: the method for sealing of the Solid Oxide Fuel Cell of present embodiment carries out according to following step: the preparation of (one) encapsulant powder AF8: (1) is Al according to molar percentage 2O 36%, SiO 255～65%, CaO7%, Na 2CO 30～3%, PbO 22～5%, B 2O 315～20%, ZnO 2～4% ratio takes by weighing above-mentioned raw materials, is that 1: 1 ratio adds aluminium oxide (or agate) the ball grinder ball milling 20 hours of packing into behind the water in mass ratio then, takes out oven dry; (2) porcelain crucible of packing into of the powder behind the ball milling, respectively calcined 4 hours at 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃ and 750 ℃ respectively, the crucible that powder is housed is directly taken out from stove, at quenching-in water, be broken into the particle of size with cylinder of steel and steel pestle, cross 40 mesh sieves less than 2mm; (3) the ball milling porcelain crucible of packing into after 15 hours again of the powder after will sieving 800 ℃ of roastings 8 hours, directly takes out the crucible that powder is housed from stove, at quenching-in water, is broken into the particle of size less than 2mm with cylinder of steel and steel pestle, crosses 40 mesh sieves; (4) powder after will sieving adds the ball grinder ball milling 8h that packs into behind the water, sieves after the oven dry, makes the seal, sealing materials powder; (2) mixing of pug: (5) are 1: 15 mixed immersion 10h formation binder solution by mass ratio with cellulose and terpinol, add seal, sealing materials powder furnishing then certain viscosity and plastic pug are arranged, wherein the mass ratio of seal, sealing materials powder and binder solution is 2: 1, the pug employing is rubbed by hand or vacuum deairing machine carries out pugging repeatedly, to eliminate the bubble of the inside; (3) compacting of sealing strip: pressed between twin pressure roller practicing the pug that makes (6), forming thickness is the slice of 3mm, lining paper is pasted in the roll extrusion simultaneously of the two sides of slice, slice is again by having two roller roll extrusion sliverings of emboss pit then, be with the sealing of protection lining paper bar to preserve, to prevent solvent evaporates drying (seeing accompanying drawing 1); (4) use of sealing strip: (7) are when using sealing strip, from airtight container, take out, measuring needs the sealing strip of length to cut, throw off the protection lining paper bar of one side, be heated to 35 ℃ and recover viscosity, carefully be bonded at the zone that needs sealing-in then, assembling needs the fuel cell component of sealing-in, pressurization at last make it to form the shape that needs and with the definite bonding realization sealing of parts; (5) high temperature encapsulation: the battery that (8) finish assembling is placed in the stove in 90 ℃ of pre-burnings 0.5 hour, first speed by 2～5 ℃/min is warming up to 150 ℃ of insulations 0.5 hour in high temperature furnace then, speed by 2～5 ℃/min is warmed up to 200 ℃ of insulations 0.5 hour again, speed with 3 ℃/min directly is warmed up to 800～900 ℃ at last, be incubated 2 hours, speed with 1 ℃/min cools to 750 ℃ subsequently, 700 ℃ and 650 ℃ also are incubated 1 hour respectively, at last with 2 ℃/min speed cool to room temperature (with circumstance of temperature difference less than 5 ℃), take out and to obtain Solid Oxide Fuel Cell (seeing accompanying drawing 2).
Embodiment 12: present embodiment is an electrolyte with the sheet yttria-stabilized zirconia (YSZ) of diameter 13mm, thick 0.5mm, with Ag is the negative electrode and the anode of fuel cell, utilize embodiment 11 described methods the end of electrolyte sheet sealing-in, form a Solid Oxide Fuel Cell (SOFC) monocell at alumina tube.The working gas of battery is hydrogen and oxygen, and its open circuit voltage sees Table 3.The result shows, the open circuit voltage of a SOFC monocell like this is near the theoretical electromotive force (1.1～1.2V) of hydrogen oxygen fuel cell, thereby proof this method can realize the sealing between fuel-cell electrolyte sheet and the stay pipe effectively, the gas leakage that do not react, and the open circuit voltage of having guaranteed battery is near theoretical value.In the sealing-in process of SOFC, when fusing takes place in seal, sealing materials will with by the wetting state of the parts surface retaining part of sealing-in, for flowing of the seal, sealing materials occurrence of large-area that prevents molten state, it soaks into the angle at device surfaces such as electrolyte can not be 0 °, its infiltration angle on YSZ solid electrolyte surface sees Table 4, obviously soaks into the angle and also can satisfy the SOFC demand well.
Table 3
Temperature 600℃ 650℃ 700℃ 750℃ 800℃ 850℃
E o 1.178V 1.180V 1.177V 1.164V 1.153V 1.139V
Above-mentioned fuel cell is carried out thermal cycling test, battery cooled to 200 ℃ from 750 ℃ in 1 hour, in 20 minutes, be warmed up to 750 ℃ again from 200 ℃, 3 times repeatedly, battery open circuit voltage 650 ℃ and 750 ℃ remains between 1.16～1.2V, take out to observe and do not see that crackle is arranged, thereby the thermal cycle of proof rapid take-off and landing temperature can not destroy the sealing effectiveness of battery, the fuel cell that encapsulates with this encapsulating method has good thermal circulation performance.
Embodiment 13: what present embodiment and embodiment 12 were different is, described electrolyte is samarium oxide doped cerium oxide (SDC), other process conditions are identical with embodiment 12 with parameter, infiltration angle on SDC solid electrolyte surface sees Table 4, obviously soaks into the angle and also can satisfy the SOFC demand well.
Table 4
Temperature (℃) 800 820 840 860 880 900 920 940 960 Sample
The infiltration angle (°) 38 12 25 20 30 19 15 14 16 AF8/YSZ
Temperature (℃) 800 850 900 - - - - - - -
The infiltration angle (°) 57 88 50 - - - - - - AF8/SDC

Claims (10)

1, the seal, sealing materials of Solid Oxide Fuel Cell is characterized in that it is made up of the raw material of following molar percentage: Al 2O 33～10%, BaCO 30～20%, SiO 250～67%, CaO 0～15%, Na 2CO 30～15%, PbO 22～9%, B 2O 310～20%, ZnO 0～5%.
2, the seal, sealing materials of Solid Oxide Fuel Cell according to claim 1 is characterized in that it is made up of the raw material of following molar percentage: Al 2O 34～5%, BaCO 31～5%, SiO 258～64%, CaO 8～14%, Na 2CO 37～13%, PbO 23～5%, B 2O 311～14%, ZnO 1～2%.
3, the seal, sealing materials of Solid Oxide Fuel Cell according to claim 1 is characterized in that it is made up of the raw material of following molar percentage: Al 2O 36～9%, BaCO 36～15%, SiO 251～56%, CaO 1～6%, Na 2CO 31～6%, PbO 26～8%, B 2O 315～19%, ZnO3～4%.
4, the seal, sealing materials of Solid Oxide Fuel Cell according to claim 1 is characterized in that it is made up of the raw material of following molar percentage: Al 2O 34%, BaCO 32%, SiO 259%, CaO 12%, Na 2CO 38%, PbO 24%, B 2O 310%, ZnO 1%.
5, the seal, sealing materials of Solid Oxide Fuel Cell according to claim 1 is characterized in that it is made up of the raw material of following molar percentage: Al 2O 37%, BaCO 38%, SiO 254%, CaO 3%, Na 2CO 32%, PbO 27%, B 2O 316%, ZnO 3%.
6, the seal, sealing materials of Solid Oxide Fuel Cell is characterized in that it is made up of the raw material of following molar percentage: Al 2O 33～10%, BaCO 35～20%, SiO 250～67%, PbO 22～9%, B 2O 310～20%, ZnO 0～5%.
7, the seal, sealing materials of Solid Oxide Fuel Cell according to claim 6 is characterized in that it is made up of the raw material of following molar percentage: Al 2O 38%, BaCO 35%, SiO 262%, PbO 28%, B 2O 317%.
8, the seal, sealing materials of Solid Oxide Fuel Cell is characterized in that it is made up of the raw material of following molar percentage: Al 2O 33～10%, SiO 250～67%, CaO 5～15%, Na 2CO 30～15%, PbO 22～9%, B 2O 310～20%, ZnO 0～5%.
9, the seal, sealing materials of Solid Oxide Fuel Cell according to claim 8 is characterized in that it is made up of the raw material of following molar percentage: Al 2O 36%, SiO 255～65%, CaO 7%, Na 2CO 30～3%, PbO 22～5%, B 2O 315～20%, ZnO 2～4%.
10, the method for sealing of Solid Oxide Fuel Cell, it is characterized in that it carries out according to following step: (1) is Al according to molar percentage 2O 33～10%, BaCO 30～20%, SiO 250～67%, CaO 0～15%, Na 2CO 30～15%, PbO 22～9%, B 2O 310～20%, the ratio of ZnO 0～5% takes by weighing above-mentioned raw materials, adds the ball grinder ball milling 2～24 hours of packing into behind the water, and wherein the mass ratio of raw material gross mass and water is 1: 1～3, takes out oven dry; (2) during the powder behind the ball milling is packed porcelain crucible into, respectively calcined 2～6 hours at 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃ and 750 ℃ respectively, the crucible that powder is housed is directly taken out from stove, at quenching-in water, pulverize then, sieve; (3) the ball milling porcelain crucible of packing into after 2～24 hours again of the powder after will sieving 800～1000 ℃ of roastings 6～8 hours, directly takes out the crucible that powder is housed from stove, at quenching-in water, pulverizes then, sieves; (4) powder after will sieving adds the ball grinder ball milling 6～8 hours of packing into behind the water, sieves after the oven dry, makes the seal, sealing materials powder; (5) be that 1: 10～25 mixed was soaked 8～10 hours with cellulose and terpinol by mass ratio, form binder solution, add the seal, sealing materials powder then and mix, obtain pug, wherein the mass ratio of seal, sealing materials powder and binder solution is 1～4: 1; (6) pug was pressed between twin pressure roller, forming thickness is the slice of 1～5mm, and lining paper is pasted in the roll extrusion simultaneously of the two sides of slice, and slice is again by having two roller roll extrusion sliverings of emboss pit then; (7) cutting sealing bar is thrown off sealing strip protection lining paper bar simultaneously, is heated to 30～40 ℃, and the sealing strip that will throw off lining paper one side then is bonded at the zone of sealing-in, assembling fuel cell parts, pressurization at last; (8) battery of finishing assembling is placed in the stove in 80～100 ℃ of pre-burnings 0.5～1 hour, first speed by 2～5 ℃/min is warming up to 130～150 ℃ of insulations 0.5～1 hour in high temperature furnace then, speed by 2～5 ℃/min is warmed up to 200～250 ℃ of insulations 0.5～1 hour again, speed with 3 ℃/min directly is warmed up to 800～900 ℃ at last, be incubated 2～4 hours, cool to 750 ℃, 700 ℃ and 650 ℃ and be incubated 1 hour respectively with the speed of 1 ℃/min subsequently, cool to room temperature with 2 ℃/min speed at last, take out and obtain Solid Oxide Fuel Cell.
CNB2004100438493A 2004-09-06 2004-09-06 Sealing material of solide oxide fuel cell and its sealing method Expired - Fee Related CN1256779C (en)

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