CN102394307A - Preparation method for anode support layer of solid oxide fuel cell - Google Patents

Preparation method for anode support layer of solid oxide fuel cell Download PDF

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CN102394307A
CN102394307A CN2011103158649A CN201110315864A CN102394307A CN 102394307 A CN102394307 A CN 102394307A CN 2011103158649 A CN2011103158649 A CN 2011103158649A CN 201110315864 A CN201110315864 A CN 201110315864A CN 102394307 A CN102394307 A CN 102394307A
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anode
anode support
slurry
powder
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吴也凡
苏蕙
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Jingdezhen Ceramic Institute
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Jingdezhen Ceramic Institute
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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
    • 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
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Abstract

The invention relates to a preparation method for an anode support layer of an anode support type solid oxide fuel cell. According to the invention, the anode is in gradient design and divided into a functional layer and a support layer; the anode functional layer and an electrolyte layer both with about 20 microns in thickness are made through a tape casting method; in order to ensure the battery strength, a superfine A12O3 with less than 200nm particle diameter is made, and a Nio, a sintering assistant MgO and a needle-shaped A12O3 are added at the same time, so as to form an anode support layer powder body which is compressed together with the functional layer and the electrolyte layer, thereby obtaining an anode support type/film layer electrolyte composite material half cell. The method has a simple process and a low cost, and is suitable for industrialized production, and accordingly the mono-cell made through the method has high strength and favorable electrochemical property.

Description

A kind of preparation method of anode of solid oxide fuel cell supporting layer
Technical field
The present invention carries out gradient design with anode, is subdivided into functional layer and supporting layer, relates to a kind of preparation method of anode support, belongs to planar anode-supported type SOFC (SOFC) field.
Background technology
Along with the petrochemical industry resource reduce day by day and the cry of ecological environmental protection surging; Countries in the world have dropped into great amount of manpower and financial resources are studied novel energy; Wherein SOFC has the generating efficiency height, makes catalyst and pollute characteristics such as little and be considered to the electricity generation system of full blast without noble metal; Can be used for generating, cogeneration, traffic, space aerospace and other many fields, be called as the green energy resource of 21 century.The focus of research is the electrolyte thin film battery of anode-supported at present, can reduce battery operated temperature and the Ohmic resistance that reduces to be caused by electrolyte so effectively.
In anode support type SOFC, anode thickness is generally bigger, and for hundreds of microns arrive the millimeter level, because anode thickness is big, the diffusion ratio of gas in anode be difficulty, the path length of arrival three-phase reaction interface.Anode can be subdivided into anode support (ASL) and anode functional layer (AFL) again.Anode functional layer is the main region that reacts, and metallic catalyst should be evenly distributed, and has more phase reaction point and higher chemism.Anode support (ASL) mainly contains three effects: mechanical support, transmission charge, transport gas.So require anode support must have enough mechanical strengths to support top anode functional layer, electrolyte, negative electrode; The electric charge that reacts and discharge on the anode functional layer simultaneously needs to export to external circuit through supporting layer, so supporting layer needs the high conductivity of trying one's best; Fuel gas need get into functional layer through supporting layer, and the waste gas that reaction generates also need pass through supporting layer and derive, so supporting layer also needs the big porosity of trying one's best so that gas passage smoothly to be provided.
Method commonly used is through changing the content of YSZ and NiO; The content antianode of purity and particle diameter or pore creating material carries out graded; But the real effecting reaction zone of functional layer is in the position near tens of microns in electrolyte; The increase of functional layer thickness will cause the increase of interface contact resistance and gas phase diffusion impedance, and anode region does not in addition have too big related with anode-catalyzed reaction.If the anode and the electrolyte of preparation optimum thickness, then the intensity of battery is difficult to guarantee.
The aluminium oxide disperse phase of making structural material commonly used is to strengthen the character such as intensity, hardness and raising recrystallization temperature of basis material.Sintering is the process that surface energy reduces, and its motive force is mainly from the surface energy of particle.Alumina powder is thin more, and surface energy is high more, and the grain circle is many more, and the material migration distance is short more, thereby densification speed is fast more, effectively reduces the alumina sintering temperature.
The present invention is about a kind of preparation method of anode supporting type solid oxide fuel cell anode support, and antianode carries out gradient design, and it is subdivided into functional layer and supporting layer.Utilize The tape casting to make anode functional layer and dielectric substrate thin layer respectively; In order to guarantee the intensity of battery, adopt ultra-fine Al 2O 3, NiO, sintering aid MgO and have the needle-like Al that strengthens toughening effect 2O 3Make anode support; And obtain anode support type/thin layer electrolyte composite material half-cell after anode support and functional layer and dielectric substrate pressed altogether.Because Al 2O 3Price far below YSZ, adopt Al in anode support 2O 3Substitute YSZ, not only reduced preparation cost, also increased the shaking property of heat resistanceheat resistant of monocell.This preparation method's technology is simple, with low cost, be suitable for suitability for industrialized production, and the monocell that makes has high strength and good electrochemical.
Summary of the invention
In order to solve the problem of existing anode support type SOFC anode support and functional layer optimum thickness and monocell intensity, the present invention provides a kind of preparation method of anode support.The present invention is the basis with environment-friendly type water system The tape casting, and adopting NiO and YSZ etc. is feedstock production water system casting slurry, makes anode function layer film and electrolytic thin-membrane through curtain coating; Adopt aluminium carbonate ammonium thermolysis process to make the ultra-fine Al of average grain diameter below 200nm 2O 3, with NiO, MgO, needle-like Al 2O 3, ultra-fine Al 2O 3For primary raw material makes the anode support powder,, after pressing altogether, dielectric substrate obtains anode support type/thin layer electrolyte composite material half-cell with functional layer.This method technology is simple, with low cost, and the SOFC that makes has good electrocatalysis characteristic, and battery machine intensity is high.
Anode support of the present invention is by ultra-fine Al 2O 3, needle-like Al 2O 3, NiO, MgO and pore creating material constitute, and it is characterized in that said method is:
(1) with NH 4Al (SO 4) 2Aqueous solution atomizing joins the NH that contains polyethylene glycol 4HCO 3In the aqueous solution, carry out vigorous stirring, obtain NH 4Al (OH) 2CO 3Deposition;
(2) with NH 4Al (OH) 2CO 3Deposition is washed with distilled water, puts into the baking oven constant temperature drying.Sample after the oven dry is pulverized, and calcining makes ultra-fine Al in high temperature furnace 2O 3Powder;
The ultra-fine Al that (3) will make 2O 3, needle-like Al 2O 3, NiO, MgO and pore creating material evenly mix in the said ratio of claim 4; Add to be placed on behind an amount of dispersant and the water and shake 1～4 hour in the ultrasonic oscillator to be uniformly dispersed; Add binding agent then, place that ball milling obtained the anode support slurry in 15～24 hours on the planetary ball mill;
(4) take out the anode support slurry, place the baking oven constant temperature drying, and pulverize;
(5) Zirconium powder, pore creating material, dispersant, binding agent, the water with nickel oxide powder, stabilized with yttrium oxide is mixed with slurry, the ball mill mixing slurry, and degasification is processed anode functional layer biscuit diaphragm with the slurry flow casting molding;
(6) Zirconium powder, dispersant, binding agent, the water of stabilized with yttrium oxide are processed slurry, the ball mill mixing slurry, degasification is processed electrolyte biscuit diaphragm with the slurry flow casting molding;
(7) in press die, put electrolyte biscuit diaphragm successively, anode functional layer biscuit diaphragm, the anode support powder, suppress altogether the half-cell base substrate;
(8) with half-cell base substrate plastic removal, sintering obtains the composite anode half-cell.
Preferred plastic removal condition is 450～650 ℃, and programming rate is 0.5～1 ℃/minute.The preferred elevated temperature sintering condition is 1300～1450 ℃ of following sintering 2～4 hours.Preferred electrolyte biscuit film sheet curtain coating condition of molding is knife up 100～130 μ m, and preferred anode functional layer biscuit film sheet curtain coating condition of molding is knife up 100～130 μ m, and at room temperature dry 20～30 hours.
In an embodiment of the present invention, with starch be pore creating material;
With water is solvent;
With the polyvinylpyrrolidone is dispersant;
With polyacrylamide-B1070 is binding agent;
With polyethylene glycol (PEG400) is plasticizer.
The mass percent of each component specifically consists of in the slurry:
Anode support slurry: ultra-fine Al 2O 320～30, NiO 40～60, and MgO 1～5, starch 10～30, and polyvinylpyrrolidone 0.8～2, polyacrylamide-B107 3～5, polyethylene glycol (PEG400) 1～3, water 10～20;
Anode functional layer slurry: the zirconia of stabilized with yttrium oxide (YSZ) powder 35, nickel oxide powder 35, starch 10～20, polyvinylpyrrolidone 1～2.5, polyacrylamide-B107 8～10, polyethylene glycol (PEG400) 1～3, water 10～20.
To different powders, can take different proportioning modes.
The present invention utilizes plurality of raw materials to make a kind of novel anode support, and its advantage is:
(1) do not contain YSZ in the supporting layer, make reaction effectively concentrate in the functional layer, do not influence the carrying out of catalytic reaction;
(2) through adding ultra-fine Al 2O 3With needle-like Al 2O 3, the intensity of increase anode support reduces Al simultaneously 2O 3Sintering temperature;
(3) add light magnesium oxide as sintering aid, help reducing the sintering temperature of anode support;
(4) casting technique is easy to prepare the anode functional layer and the dielectric substrate of very thin thickness, and method is simple, with low cost, pollution-free;
(5) be divided into functional layer and supporting layer through the anode gradient, have to utilize to increase three-phase reaction interface, improve the monocell chemical property.
Description of drawings
Fig. 1 is for by the SOFC monocell of instance 9 preparation I-V and I-P indicatrix when 750 ℃ are fuel with hydrogen, and hydrogen flowing quantity is 25ml/min, oxidizing gas (O 2) flow is 25ml/min.
Specific embodiments
In order more to be expressly understood the present invention, explain that below in conjunction with specific embodiments the present invention makes progress and obvious improvement substantively, the application example that provides the inventor to be being further described the present invention, but not only is confined to embodiment.
Embodiment 1
Take by weighing 28.46g NH 4Al (SO 4) 2, add 1L distilled water and be made into the aqueous solution that concentration is 0.12mol/L, utilize spray gun to be injected to the 1.6mol/L NH that mass ratio is 2% polyethylene glycol that contains of vigorous stirring after stirring 4HCO 3In the aqueous solution, obtain NH 4Al (OH) 2CO 3Deposition.
Embodiment 2
With NH 4Al (OH) 2CO 3Deposition is repeatedly with the distilled water washing, and is centrifugal to remove foreign ion.Put into 100 ℃ of constant temperature dryings of baking oven to sediment at last.Sample after the oven dry is pulverized in agate mortar, and 1100 ℃ of calcinings make ultra-fine Al in high temperature furnace 2O 3Powder.
Embodiment 3
Accurate weighing 55gNiO, 5g MgO, 15g starch, the ultra-fine Al of 25g 2O 3Powder, 0.3g needle-like Al 2O 3, polyvinylpyrrolidone 2g and distilled water 20g are placed on and shake 2 hours in the ultrasonic oscillator to be uniformly dispersed; Add 5 gram polyacrylamide-B1070, polyethylene glycol (PEG400), 3 grams then, placed on the planetary ball mill ball milling 20 hours, the anode support slurry that obtains is placed 90 ℃ of constant temperature dryings of baking oven after, take out grind into powder and make the anode support powder.
Embodiment 4
Get zirconia (YSZ) powder 50 grams, nickel oxide powder 50 grams, starch 15 grams, polyvinylpyrrolidone 1.6 grams and water 20 grams of stabilized with yttrium oxide respectively, join in the polytetrafluoroethylene ball grinder, ball milling is 24 hours on planetary ball mill; Add polyacrylamide (mass ratio 50%)-B1070 (mass ratio 50%) 13 grams, polyethylene glycol (PEG400) 5 grams then, continued ball milling 12 hours, obtain the anode functional layer slurry.The anode functional layer slurry was vacuumized 10 minutes, on casting machine with knife up 120 μ m flow casting moldings, the demoulding after dry 24 hours under the room temperature.Make the anode functional layer biscuit film.
Embodiment 5
Get zirconia (YSZ) powder 50 grams, polyvinylpyrrolidone 2 grams and water 10 grams of stabilized with yttrium oxide respectively, join in the polytetrafluoroethylene ball grinder, ball milling is 24 hours on planetary ball mill; Add polyacrylamide (mass ratio 50%)-B1070 (mass ratio 50%) 3 grams, polyethylene glycol (PEG400) 2 grams then, continued ball milling 12 hours, obtain electrolyte slurry.Electrolyte slurry was vacuumized 10 minutes, on casting machine with knife up 100 μ m flow casting moldings, the demoulding after dry 24 hours under the room temperature.Make electrolyte biscuit diaphragm.
Embodiment 6
In mould, put into the anode support powder successively, anode functional layer biscuit film and electrolyte biscuit film are pressed under 20Mpa altogether, make thick about 1.5mm, the compound biscuit diaphragm of anode support-anode functional layer of the about 260mm of the length of side-thin layer electrolyte.With 1450 ℃ of following sintering of the compound biscuit diaphragm of the anode support-anode functional layer that makes-thin layer electrolyte 5 hours, programming rate was 2 ℃/minute.Behind sintering, process anode support-anode functional layer-thin layer electrolyte composite material half-cell.
Embodiment 7
Example 6 in accordance with the method of large-area anode support layer - an anode functional layer - thin half-cell electrolyte composite material of 13mm cut straight through the wafer, taking LSM1g, terpineol solution of 0.7g, the Ma Lao RESEARCH bowl sufficiently ground, and the resulting slurry was screen-printed on the composite cathode material of the electrolyte membrane side of the membrane, and then sintered at 1200 ℃ 2 hours at a heating rate of 1 ℃ / min.Finally make the coin shape monocell.
Embodiment 8
With the half-cell cut growth 4cm among the embodiment 6; The strip of wide 0.7cm; The WDW-10 type system controlled by computer electronics universal testing machine that adopts Lichuang Metering Instrument Co Ltd, Xi'an to produce is tested its intensity, and the result shows that the rupture strength of this half-cell is 320MPa.
Embodiment 9
Coin shape monocell anode one side in embodiment 7 preparations is coated the platinum grid with collected current, and draws Pt silk electricity at the two poles of the earth, seals with glass ring.Logical hydrogen reducing anode was a fuel with hydrogen after 2 hours in the time of 750 ℃, carried out generator experimental.The result shows that this monocell has good electrocatalysis characteristic, H 2Under maximum power density reached 0.79W/cm 2

Claims (7)

1. an anode support is characterized in that said supporting layer is by NiO, needle-like Al 2O 3, sintering aid MgO, ultra-fine Al 2O 3Form with pore creating material.
2. ultra-fine Al according to claim 1 2O 3, it is characterized in that its average grain diameter is below 200nm.
3. ultra-fine Al according to claim 1 2O 3, it is characterized in that it is by NH 4Al (SO 4) 2And NH 4HCO 3The aluminium carbonate ammonium thermal decomposition gained that makes for raw material.
4. supporting layer according to claim 1 is characterized in that its constitutive material proportion is ultra-fine Al 2O 3Account for 20～30% of material powder gross mass, NiO accounts for 40～60% of material powder gross mass, and MgO accounts for 1～5% of material powder gross mass, needle-like Al 2O 3Account for 0.3～1% of material powder gross mass, pore creating material accounts for 10～30% of material powder gross mass.
5. method of utilizing the flat SOFC anode support of the described supporting layer powder preparing of claim 1-4 is characterized in that said method is:
(1) with NH 4Al (SO 4) 2Aqueous solution atomizing joins the NH that contains polyethylene glycol 4HCO 3In the aqueous solution, carry out vigorous stirring, obtain NH 4Al (OH) 2CO 3Deposition;
(2) with NH 4Al (OH) 2CO 3Deposition is washed with distilled water, puts into the baking oven constant temperature drying.Sample after the oven dry is pulverized, and calcining makes ultra-fine Al in high temperature furnace 2O 3Powder;
The ultra-fine Al that (3) will make 2O 3, needle-like Al 2O 3, NiO, MgO and pore creating material evenly mix in the said ratio of claim 4; Add to be placed on behind an amount of dispersant and the water and shake 1～4 hour in the ultrasonic oscillator to be uniformly dispersed; Add binding agent then, place that ball milling obtained the anode support slurry in 15～24 hours on the planetary ball mill;
(4) take out the anode support slurry, place the baking oven constant temperature drying, and pulverize;
(5) Zirconium powder, pore creating material, dispersant, binding agent, the water with nickel oxide powder, stabilized with yttrium oxide is mixed with slurry, the ball mill mixing slurry, and degasification is processed anode functional layer biscuit diaphragm with the slurry flow casting molding;
(6) Zirconium powder, dispersant, binding agent, the water of stabilized with yttrium oxide are processed slurry, the ball mill mixing slurry, degasification is processed electrolyte biscuit diaphragm with the slurry flow casting molding;
(7) in press die, put electrolyte biscuit diaphragm successively, anode functional layer biscuit diaphragm, the anode support powder, suppress altogether the half-cell base substrate;
(8) with half-cell base substrate plastic removal, sintering obtains the composite anode half-cell.
6. by the method for the described anode support of claim 5, it is characterized in that the described plastic removal condition of step (8) is 450～650 ℃, programming rate is 0.5～1 ℃/minute.
7. by the method for the described anode support of claim 5, it is characterized in that the described sintering condition of step (8) is 1300～1450 ℃ of following sintering 2～4 hours.
CN2011103158649A 2011-10-12 2011-10-12 Preparation method for anode support layer of solid oxide fuel cell Pending CN102394307A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109216740A (en) * 2017-07-07 2019-01-15 中国科学院宁波材料技术与工程研究所 A kind of anode support and preparation method thereof of hollow symmetrical SOFC battery
CN111900449A (en) * 2020-08-04 2020-11-06 贝特瑞新材料集团股份有限公司 Solid oxide fuel cell, method for producing same and use thereof
CN111933956A (en) * 2020-07-13 2020-11-13 山东工业陶瓷研究设计院有限公司 Solid oxide fuel cell electrode material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10223243A (en) * 1997-02-04 1998-08-21 Mitsubishi Heavy Ind Ltd Base pipe for solid electrolyte fuel cell
US20110200910A1 (en) * 2008-10-14 2011-08-18 University Of Florida Research Foundation Inc. Advanced materials and design for low temperature sofcs
CN102185148A (en) * 2011-04-01 2011-09-14 景德镇陶瓷学院 NiO-based SOFC (Solid Oxide Fuel Cell) composite anode film material with nano-sheet microcellular structure and preparation method thereof
CN102208656A (en) * 2011-04-30 2011-10-05 景德镇陶瓷学院 Anode of fibrous nickel oxide-based SOFC (Solid Oxide Fuel Cell) and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10223243A (en) * 1997-02-04 1998-08-21 Mitsubishi Heavy Ind Ltd Base pipe for solid electrolyte fuel cell
US20110200910A1 (en) * 2008-10-14 2011-08-18 University Of Florida Research Foundation Inc. Advanced materials and design for low temperature sofcs
CN102185148A (en) * 2011-04-01 2011-09-14 景德镇陶瓷学院 NiO-based SOFC (Solid Oxide Fuel Cell) composite anode film material with nano-sheet microcellular structure and preparation method thereof
CN102208656A (en) * 2011-04-30 2011-10-05 景德镇陶瓷学院 Anode of fibrous nickel oxide-based SOFC (Solid Oxide Fuel Cell) and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109216740A (en) * 2017-07-07 2019-01-15 中国科学院宁波材料技术与工程研究所 A kind of anode support and preparation method thereof of hollow symmetrical SOFC battery
CN111933956A (en) * 2020-07-13 2020-11-13 山东工业陶瓷研究设计院有限公司 Solid oxide fuel cell electrode material and preparation method thereof
CN111933956B (en) * 2020-07-13 2021-10-08 山东工业陶瓷研究设计院有限公司 Solid oxide fuel cell electrode material and preparation method thereof
CN111900449A (en) * 2020-08-04 2020-11-06 贝特瑞新材料集团股份有限公司 Solid oxide fuel cell, method for producing same and use thereof
CN111900449B (en) * 2020-08-04 2021-09-14 贝特瑞新材料集团股份有限公司 Solid oxide fuel cell, method for producing same and use thereof

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Application publication date: 20120328