CN100409478C - Method for reducing deformation of solid oxide fuel cell electrolyte film - Google Patents
Method for reducing deformation of solid oxide fuel cell electrolyte film Download PDFInfo
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- CN100409478C CN100409478C CNB2006100102392A CN200610010239A CN100409478C CN 100409478 C CN100409478 C CN 100409478C CN B2006100102392 A CNB2006100102392 A CN B2006100102392A CN 200610010239 A CN200610010239 A CN 200610010239A CN 100409478 C CN100409478 C CN 100409478C
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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 a method for reducing the deformation of a solid oxide fuel battery electrolyte film, which relates to a method for reducing the deformation of the electrolyte film. The procedures of the method are as following: step 1, an anode supporting body is prepared; step 2, YSZ electrolyte slurry is prepared, step 3, a YSZ electrolyte film is printed, step 4, a YSZ sheet is prepared; step 5, the YSZ electrolyte film is sintered. Thus, the YSZ electrolyte film in an anode supporting type of the solid oxide fuel battery is obtained, and also has the thickness of 0.44mm. The thickness of the electrolyte film in the prior art after the sintering operation with the anode is 1.28mm. The thickness of the electrolyte film according to the method of the present invention after the sintering operation with the anode is 0.44mm. The electrolyte film prepared according to the method of the present invention has the advantages of smooth surface, no deformation, and providence of helpful condition for the preparation of a battery cathode and easy package for the battery. The sintering process of the electrolyte film in the method of the present invention increases the pressure from the YSZ sheet and reduces deformation. Thus, the electrolyte film is dense. The voltage of the battery prepared by the method of the present invention can stably obtain 1.0 V.
Description
Technical field
The present invention relates to a kind of method that reduces dielectric film deformation.
Background technology
Solid Oxide Fuel Cell (Solid Oxide Fuel Cell, be called for short SOFC) being a kind of fuel gas and oxidant gas by ionic conduction, electrochemistry takes place in conjunction with all solid state energy conversion device that produces electric energy in soild oxide (electrolyte), is an emerging technology that develops rapidly the 1980s.Electrolytical filming can reduce the working temperature of SOFC, improves the combination property of battery, but current electrolysis plasma membrane and anode burn the serious deformation of generation altogether, are unfavorable for the preparation of cell cathode and the encapsulation of battery.Though people such as S.H.Lee are at Key.Eng.Mat.321[8] people such as 264-268 (2004) this piece document and P.Z.Cai are at J.Am.Ceram.Soc.80[8] point out to cause that the reason that serious deformation takes place for dielectric film and anode high temperature co-firing knot back mainly includes the viscosity of anode substrate thickness, slurry and mechanical pressure of the hot matching between flowability, anode and dielectric film and each interlayer of dielectric film or the like in the document of 1929-39 (1997).People such as Paul VonDollen are at J.Am.Ceram.Soc.88[12] mentioned the deformation that behind dielectric film and anode co-sintering, causes among the 3361-3368 (2005), and specialized in some factors that anode calcined temperature, anode substrate thickness and wet end furnish etc. influence dielectric film deformation.But do not solve dielectric film and anode all the time and burn the problem that serious deformation takes place altogether.
Summary of the invention
The objective of the invention is to burn the problem that serious deformation takes place altogether in order to solve dielectric film and anode, and a kind of method that reduces deformation of solid oxide fuel cell electrolyte film that provides.The method that reduces deformation of solid oxide fuel cell electrolyte film realizes according to the following steps: (one) prepares anode support: 5: 1: 3 by weight: 5 ratio is with the NiO powder, starch, absolute ethyl alcohol is put into the planetary ball mill that abrading-ball is an agate with the YSZ powder that contains the 8mol% yittrium oxide, the weight ratio of agate ball and mixture is 2～5: 1, at rotational speed of ball-mill ball milling 4～10h under the condition of 150～250r/min, dry back is pressed into the anode strip that thickness is 0.4～0.5mm under the condition of 250～350MPa, anode strip is put into environment sintering 1.8～2.2h of 950～1050 ℃ then, is anode support; (2) preparation of YSZ electrolyte slurry: the YSZ powder that will contain 8mol% yittrium oxide, particle diameter and be 0.05～1.0 μ m is put into the grinding in ball grinder that abrading-ball is an agate, will put into agate mortar by 4: 5 weight ratio through the YSZ fine powder of ball milling and organic binder bond then and be mixed into uniform and stable YSZ electrolyte slurry; (3) printing of YSZ dielectric film: the YSZ electrolyte slurry that step (two) is made with 400～440 purpose nylon mesh printing machines is printed on the upper surface of the anode support of step () preparation uniformly, treat to print one deck electrolyte slurry down again after one deck electrolyte slurry drying, YSZ dielectric film thickness is 10～50 μ m; (4) preparation YSZ sheet: the YSZ powder that will contain the 3mol% yittrium oxide carries out compressing tablet, puts into environment sintering 3.5～4.5h of 1500～1700 ℃ then, and the cross-sectional area of the YSZ sheet that obtains through oversintering is greater than the area of dielectric film; (5) sintering YSZ dielectric film: the one side that anode support is printed on dielectric film is upwards put into muffle furnace and place the YSZ sheet of step (four) preparation on dielectric film, the pressure that makes the electrolyte face is 650～1310Pa, muffle furnace is warming up to 300～500 ℃ with 3h, be warming up to 500～900 ℃ with 4h again, be warming up to 900～1400 ℃ with 2h then, 1400 ℃ are incubated 2h afterwards, be cooled to 900～1399 ℃ with 2h again, be cooled to room temperature at last and remove the YSZ sheet that step on the dielectric film (four) prepares, promptly obtain anode of solid oxide fuel cell support type YSZ dielectric film.The same thick dielectric film of 0.44mm, thickness is 1.28mm behind existing method dielectric film and the anode sintering; By dielectric film thickness behind the inventive method dielectric film and the anode sintering is 0.44mm, and deformation does not take place its surface smoothing, for the preparation of cell cathode provides advantageous conditions, also makes the easier encapsulation of battery.Battery voltage in the open test process that existing solid oxide fuel cell electrolyte film preparation method produces is up to 0.6V, and test begins soon that voltage just drops near the 0V; And the cell electrolyte film sintering process has increased the pressure that comes from the YSZ sheet in the inventive method, and the deformation that has produced when having reduced dielectric film and anode sintering simultaneously makes dielectric film become more fine and close.That adopts battery that the inventive method prepares voltage can be highly stable in the open test process reaches 1.0V, has improved the performance of Solid Oxide Fuel Cell.The inventive method can be applied in the film sintering process of different electrolytes and go, also can combine with multiple dielectric film preparation technology (using electrolyte slurry), make the preparation process of battery convenient, promote dielectric film preparation technology's popularization and the commercialization process of SOFC.
Embodiment
Embodiment one: the method that present embodiment reduces deformation of solid oxide fuel cell electrolyte film realizes according to the following steps: (one) prepares anode support: 5: 1: 3 by weight: 5 ratio is with the NiO powder, starch, absolute ethyl alcohol is put into the planetary ball mill that abrading-ball is an agate with the YSZ powder that contains the 8mol% yittrium oxide, the weight ratio of agate ball and mixture is 2～5: 1, at rotational speed of ball-mill ball milling 4～10h under the condition of 150～250r/min, dry back is pressed into the anode strip that thickness is 0.4～0.5mm under the condition of 250～350MPa, anode strip is put into environment sintering 1.8～2.2h of 950～1050 ℃ then, is anode support; (2) preparation of YSZ electrolyte slurry: the YSZ powder that will contain 8mol% yittrium oxide, particle diameter and be 0.05～1.0 μ m is put into the grinding in ball grinder that abrading-ball is an agate, will put into agate mortar by 4: 5 weight ratio through the YSZ fine powder of ball milling and organic binder bond then and be mixed into uniform and stable YSZ electrolyte slurry; (3) printing of YSZ dielectric film: the YSZ electrolyte slurry that step (two) is made with 400～440 purpose nylon mesh printing machines is printed on the upper surface of the anode support of step () preparation uniformly, treat to print one deck electrolyte slurry down again after one deck electrolyte slurry drying, YSZ dielectric film thickness is 10～50 μ m; (4) preparation YSZ sheet: the YSZ powder that will contain the 3mol% yittrium oxide carries out compressing tablet, puts into environment sintering 3.5～4.5h of 1500～1700 ℃ then, and the cross-sectional area of the YSZ sheet that obtains through oversintering is greater than the area of dielectric film; (5) sintering YSZ dielectric film: the one side that anode support is printed on dielectric film is upwards put into muffle furnace and place the YSZ sheet of step (four) preparation on dielectric film, the pressure that makes the electrolyte face is 650～1310Pa, muffle furnace is warming up to 300～500 ℃ with 3h, be warming up to 500～900 ℃ with 4h again, be warming up to 900～1400 ℃ with 2h then, 1400 ℃ are incubated 2h afterwards, be cooled to 900～1399 ℃ with 2h again, be cooled to room temperature at last and remove the YSZ sheet that step on the dielectric film (four) prepares, promptly obtain anode of solid oxide fuel cell support type YSZ dielectric film.
Other parts of present embodiment Solid Oxide Fuel Cell all can be made by existing technology, can obtain high-performance, cheap, the simply easy Solid Oxide Fuel Cell of assembly unit.Present embodiment adopts the YSZ sheet of step (four) preparation to increase the pressure of YSZ electrolyte face, can avoid the introducing of other impurity.
Embodiment two: the difference of present embodiment and execution mode one is: the particle diameter that contains the YSZ powder of 8mol% yittrium oxide in the step () is 0.5～2.0 μ m.Other step is identical with execution mode one.
The YSZ powder that present embodiment is selected for use has bigger particle diameter can guarantee that anode support forms good YSZ skeleton in sintering process, avoid the agglomeration of NiO.
Embodiment three: the difference of present embodiment and execution mode one is: organic binder bond is the mixed liquor of ethyl cellulose and terpinol in the step (two), wherein ethyl cellulose accounts for 4～6% of mixeding liquid volume, and terpinol accounts for 94～96% of mixeding liquid volume.Other step is identical with execution mode one.
Embodiment four: the difference of present embodiment and execution mode one is: organic binder bond is the mixed liquor of ethyl cellulose and terpinol in the step (two), wherein ethyl cellulose accounts for 5% of mixeding liquid volume, and terpinol accounts for 95% of mixeding liquid volume.Other step is identical with execution mode one.
Embodiment five: the difference of present embodiment and execution mode one is: the weight ratio of agate ball and YSZ powder is 2～5: 1 in the step (two), and drum's speed of rotation is 150～250r/min, and the ball milling time is 4～10h.Other step is identical with execution mode one.
Embodiment six: the difference of present embodiment and execution mode one is: the weight ratio of agate ball and YSZ powder is 3～4: 1 in the step (two), and drum's speed of rotation is 180～220r/min, and the ball milling time is 5～9h.Other step is identical with execution mode one.
Embodiment seven: the difference of present embodiment and execution mode one is: the weight ratio of agate ball and YSZ powder is 3.5: 1 in the step (two), and drum's speed of rotation is 200r/min, and the ball milling time is 7h.Other step is identical with execution mode one.
Embodiment eight: the difference of present embodiment and execution mode one is: be pressed into the anode strip that thickness is 0.41～0.49mm in the step ().Other step is identical with execution mode one.
Embodiment nine: the difference of present embodiment and execution mode one is: be pressed into the anode strip that thickness is 0.42～0.48mm in the step ().Other step is identical with execution mode one.
Embodiment ten: the difference of present embodiment and execution mode one is: be pressed into the anode strip that thickness is 0.45mm in the step ().Other step is identical with execution mode one.
Embodiment 11: the difference of present embodiment and execution mode one is: anode strip is put into environment sintering 1.9～2.1h of 960～1040 ℃ in the step ().Other step is identical with execution mode one.
Present embodiment can be removed desizing, and the formation porosity is 10～60% anode support, and strengthens the mechanical strength of anode support.
Embodiment 12: the difference of present embodiment and execution mode one is: anode strip is put into 1000 ℃ environment sintering 2h in the step ().Other step is identical with execution mode one.
Embodiment 13: the difference of present embodiment and execution mode one is: the YSZ electrolyte slurry that with 410～430 purpose nylon mesh printing machines step (two) is made in the step (three) is printed on the upper surface of the anode support of step () preparation uniformly.Other step is identical with execution mode one.
Embodiment 14: the difference of present embodiment and execution mode one is: the YSZ electrolyte slurry that with 420 purpose nylon mesh printing machines step (two) is made in the step (three) is printed on the upper surface of the anode support of step () preparation uniformly.Other step is identical with execution mode one.
Embodiment 15: the difference of present embodiment and execution mode one is: YSZ dielectric film thickness is 15～45 μ m in the step (three).Other step is identical with execution mode one.
Embodiment 16: the difference of present embodiment and execution mode one is: YSZ dielectric film thickness is 20～40 μ m in the step (three).Other step is identical with execution mode one.
Embodiment 17: the difference of present embodiment and execution mode one is: YSZ dielectric film thickness is 31 μ m in the step (three).Other step is identical with execution mode one.
Embodiment 18: the difference of present embodiment and execution mode one is: the YSZ pressed powder is put into 1600 ℃ environment sintering 4h in the step (four).Other step is identical with execution mode one.
Embodiment 19: the difference of present embodiment and execution mode one is: the pressure of electrolyte face is 660～1300Pa in step (five).Other step is identical with execution mode one.
Embodiment 20: the difference of present embodiment and execution mode one is: the pressure of electrolyte face is 700～1200Pa in step (five).Other step is identical with execution mode one.
Embodiment 21: the difference of present embodiment and execution mode one is: the pressure of electrolyte face is 800～1100Pa in step (five).Other step is identical with execution mode one.
Embodiment 22: the difference of present embodiment and execution mode one is: the weight ratio of agate ball and mixture is 3～4: 1 in the step (), and drum's speed of rotation is 180～220r/min, and the ball milling time is 5～9h.Other step is identical with execution mode one.
Embodiment 23: the difference of present embodiment and execution mode one is: the weight ratio of agate ball and mixture is 3.5: 1 in the step (), and drum's speed of rotation is 190～210r/min, and the ball milling time is 6～8h.Other step is identical with execution mode one.
Embodiment 24: the difference of present embodiment and execution mode one is: the weight ratio of agate ball and mixture is 4: 1 in the step (), and drum's speed of rotation is 200r/min, and the ball milling time is 7h.Other step is identical with execution mode one.
Claims (10)
1. method that reduces deformation of solid oxide fuel cell electrolyte film, it is characterized in that the method that reduces deformation of solid oxide fuel cell electrolyte film realizes according to the following steps: one, the preparation anode support: 5: 1: 3 by weight: 5 ratio was with the NiO powder, starch, absolute ethyl alcohol is put into the planetary ball mill that abrading-ball is an agate with the YSZ powder that contains the 8mol% yittrium oxide, the weight ratio of agate ball and mixture is 2～5: 1, at rotational speed of ball-mill ball milling 4～10h under the condition of 150～250r/min, dry back is pressed into the anode strip that thickness is 0.4～0.5mm under the condition of 250～350MPa, anode strip is put into environment sintering 1.8～2.2h of 950～1050 ℃ then, is anode support; Two, the preparation of YSZ electrolyte slurry: the YSZ powder that will contain 8mol% yittrium oxide, particle diameter and be 0.05～1.0 μ m is put into the grinding in ball grinder that abrading-ball is an agate, will put into agate mortar by 4: 5 weight ratio through the YSZ fine powder of ball milling and organic binder bond then and be mixed into uniform and stable YSZ electrolyte slurry; Three, the printing of YSZ dielectric film: the YSZ electrolyte slurry that step 2 is made with 400～440 purpose nylon mesh printing machines is printed on the upper surface of the anode support of step 1 preparation uniformly, treat to print one deck electrolyte slurry down again after one deck electrolyte slurry drying, YSZ dielectric film thickness is 10～50 μ m; Four, preparation YSZ sheet: the YSZ powder that will contain the 3mol% yittrium oxide carries out compressing tablet, puts into environment sintering 3.5～4.5h of 1500～1700 ℃ then, and the cross-sectional area of the YSZ sheet that obtains through oversintering is greater than the area of dielectric film; Five, sintering YSZ dielectric film: the one side that anode support is printed on dielectric film is upwards put into muffle furnace and place the YSZ sheet of step 4 preparation on dielectric film, the pressure that makes the electrolyte face is 650～1310Pa, muffle furnace is warming up to 300～500 ℃ with 3h, be warming up to 500～900 ℃ with 4h again, be warming up to 900～1400 ℃ with 2h then, 1400 ℃ are incubated 2h afterwards, be cooled to 900～1399 ℃ with 2h again, be cooled to room temperature at last and remove the YSZ sheet that step 4 prepares on the dielectric film, promptly obtain anode of solid oxide fuel cell support type YSZ dielectric film.
2. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1, the particle diameter that it is characterized in that containing in the step 1 YSZ powder of 8mol% yittrium oxide is 0.5～2.0 μ m.
3. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1, it is characterized in that organic binder bond is the mixed liquor of ethyl cellulose and terpinol in the step 2, wherein ethyl cellulose accounts for 4～6% of mixeding liquid volume, and terpinol accounts for 94～96% of mixeding liquid volume.
4. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1, it is characterized in that the weight ratio of agate ball and YSZ powder is 2～5: 1 in the step 2, drum's speed of rotation is 150～250r/min, and the ball milling time is 4～10h.
5. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1 is characterized in that being pressed in the step 1 anode strip that thickness is 0.41～0.49mm.
6. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1 is characterized in that anode strip is put into environment sintering 1.9～2.1h of 960～1040 ℃ in the step 1.
7. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1 is characterized in that the YSZ electrolyte slurry that with 410～430 purpose nylon mesh printing machines step 2 is made in the step 3 is printed on the upper surface of the anode support of step 1 preparation uniformly.
8. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1 is characterized in that YSZ dielectric film thickness is 15～45 μ m in the step 3.
9. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1 is characterized in that the YSZ pressed powder is put into 1600 ℃ environment sintering 4h in the step 4.
10. a kind of method that reduces deformation of solid oxide fuel cell electrolyte film according to claim 1, the pressure that it is characterized in that electrolyte face in the step 5 is 660～1300Pa.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101635364B (en) * | 2009-07-15 | 2011-11-30 | 哈尔滨工业大学 | Method for preparing anode support electrolyte complex film |
| CN102584223A (en) * | 2012-01-18 | 2012-07-18 | 苏州华清京昆新能源科技有限公司 | Casting slurry for preparing electrolyte layer in fuel cell |
| WO2013173981A1 (en) * | 2012-05-22 | 2013-11-28 | Yang Shaohua | Anode-supported solid oxide fuel cell and method for preparing same |
| CN104183860B (en) * | 2014-08-04 | 2016-08-17 | 景德镇陶瓷学院 | A kind of zirconium oxide plate burnt for planar anode-supported type SOFC half-cell pressure and surface modification method thereof |
| CN113497266B (en) * | 2021-06-25 | 2022-12-09 | 华中科技大学 | Electrolyte layer, preparation method and application thereof |
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Patent Citations (6)
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| JPH06349503A (en) * | 1993-06-07 | 1994-12-22 | Mitsubishi Heavy Ind Ltd | Solid electrolyte type electrolytic cell |
| CN1271969A (en) * | 1999-04-22 | 2000-11-01 | 中国科学院大连化学物理研究所 | Anode load type solid electrolyte of yttrium oxide stabilized zirconium oxide and its preparing process |
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