CN108649236A - A kind of the air pole material and preparation method of intermediate temperature solid oxide fuel cell - Google Patents

A kind of the air pole material and preparation method of intermediate temperature solid oxide fuel cell Download PDF

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Publication number
CN108649236A
CN108649236A CN201810327177.0A CN201810327177A CN108649236A CN 108649236 A CN108649236 A CN 108649236A CN 201810327177 A CN201810327177 A CN 201810327177A CN 108649236 A CN108649236 A CN 108649236A
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air pole
powder
pole material
solid oxide
oxide fuel
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凌意瀚
郭阳阳
郭天民
陈辉
郭立童
冯培忠
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China University of Mining and Technology CUMT
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China University of Mining and Technology CUMT
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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
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
    • H01M4/9025—Oxides specially used in fuel cell operating at high temperature, e.g. SOFC
    • H01M4/9033—Complex oxides, optionally doped, of the type M1MeO3, M1 being an alkaline earth metal or a rare earth, Me being a metal, e.g. perovskites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Nickelates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M2008/1293—Fuel cells with solid oxide electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Abstract

A kind of the air pole material and preparation method of intermediate temperature solid oxide fuel cell, belong to field of solid oxide fuel.Material：Select the Sr of perovskite-like oxide3Fe2O7‑δMatrix, the A La using trivalent replace, and further increase the structural stability of material, and B, using transition metal Ni part substitution Fe, further increase the conductivity and catalytic activity of material；Method is：Suitable complexing agent ethylenediamine tetra-acetic acid is added in traditional combustion method of citric acid using improved combustion method of citric acid powder), according to La:Sr:Fe:Ni=0.25:2.75:1:1 molar ratio weighs the chemical raw material corresponding to each element, and citric acid, two kinds of complexing agents of ethylenediamine tetra-acetic acid (EDTA) are added, nitric acid and ammonia solvent are added, it is 78 to adjust PH, is evaporated and sinters powder into, again in 1200 DEG C of pre-burning 3h, air pole material powder is obtained.Advantage：The present invention has good ion and Electronic Transport of Two Benzene, good chemical property, is that a kind of comprehensive performance is good and air pole material suitable for middle low temperature.

Description

A kind of the air pole material and preparation method of intermediate temperature solid oxide fuel cell
Technical field
The present invention relates to field of solid oxide fuel, especially a kind of intermediate temperature solid oxide fuel cell Perovskite-like oxide air pole material.
Background technology
Solid oxide fuel cell (SOFC), can be in direct fuel as a kind of energy conversion apparatus of high-efficiency cleaning Chemical energy convert electric energy, do not limited by Carnot cycle.The operation temperature for reducing SOFC, helps speed up the business of SOFC Change process has wider range of material selection.However, with the reduction of SOFC operation temperatures, the Ohmic resistance and polarization electricity of battery Resistance greatly increases, and wherein polarization resistance accounts for the overwhelming majority.According to hydrogen reduction process, hybrid ionic electronic conductor can have The extension three-phase reaction interface of effect, the effective process for accelerating hydrogen reduction, therefore, in searching under low temperature high catalytic activity it is mixed The air pole material for closing ion-electron conduction is particularly critical.
Ruddlesden-Popper (RP) types layered oxide (general skeleton symbol An+1BnO3n+1) it is by the rock salt of two layers of AO Layer is intermediate to press from both sides n ABO3Perovskite composition sandwich structure, belong to simple tetragonal crystal.Relative to simple perovskite oxygen Compound, RP type layered oxides have orderly BO6The oxygen of octahedral structure, the anisotropy of oxonium ion diffusion and high concentration Defect species so that oxygen ion conduction activation energy reduces, oxygen surface exchange and transmittability are improved.Sr3Fe2O7-δOxygen passes Defeated performance has anisotropy, presents excellent hybrid ionic electronic conduction characteristic, is equally presented not as electrode material Wrong chemical property, but Sr3Fe2O7-δStructural stability it is to be improved.
Invention content
The invention aims to provide a kind of perovskite-like oxide air of intermediate temperature solid oxide fuel cell Pole material improves the cryogenic property and long-time stability of solid oxide fuel cell.
The object of the present invention is achieved like this：The present invention includes the preparation side of air pole material and its air pole material Method；
The air pole material：Select the Sr of perovskite-like oxide3Fe2O7-δMatrix, A are taken using the La of trivalent In generation, further increases the structural stability of material, and B, using transition metal Ni part substitution Fe, further increase the electricity of material Conductance and catalytic activity.
The preparation method of the air pole material is：Using improved combustion method of citric acid powder, the improved lemon Lemon acid burning legal system powder is that suitable complexing agent ethylenediamine tetra-acetic acid is added in traditional combustion method of citric acid, according to La: Sr:Fe:Ni=0.25:2.75:1:1 molar ratio weighs the chemical raw material corresponding to each element, and citric acid, second is added Two kinds of complexing agents of ethylenediamine tetraacetic acid (EDTA) (EDTA) add nitric acid and ammonia solvent, and adjusting PH is 7-8, is evaporated and sinters powder into, Again in 1200 DEG C of pre-burning 3h, air pole material powder is obtained.
Specific preparation process：
(1) required raw material is calculated according to the molal weight of each element first：La(NO3)3·6H2O、Sr(NO3)2、 Fe (NO3)3·9H2O、Ni(NO3)3·6H2The quality of O, and four kinds of raw material weighings are put into well in a clean beaker, then press Complexing agent, wherein citric acid is added in molar ratio：Ethylenediamine tetra-acetic acid：Metal ion, the metal ion are La+Sr+Fe + Ni, molar ratio 1:0.8:1, add 50-100ml distilled water after complexing agent to be put into the beaker for preparing raw material, adds 15- 20ml nitric acid, stirring, ultrasound add ammonium hydroxide, and adjusting PH is 7-8, obtains clear solution；
(2) clear solution that step (1) prepares is put into evaporating dish and is heated, stirred when solution is evaporated soon, to prevent Only uneven heating causes liquid splash or evaporating dish to crack, and stirring is sticky to solution and violent combustion reaction occurs, and obtains just Beginning powder；Initial powder is collected after cooling and is put into high temperature alumina crucible, and crucible is put into 1200 DEG C of -3h of Muffle furnace pre-burning, Obtain air pole material powder.
Advantageous effect, using the above scheme, the present invention is based on the Sr of high catalytic activity3Fe2O7-δMatrix passes through high price La The parts the Ni substitution Fe of part substitution Sr and divalent, increase coupling between the transition metal of layered oxide, adjust stratiform oxygen The defect and band structure of compound improve ion and electronic conduction ability, increase stable structure.
La0.25Sr2.75FeNiO7-δWith excellent chemical stability, high urges chemical property, is presented under middle low temperature The air pole material of a kind of novel ion and electron mixed conductor type of excellent combination property.La0.25Sr2.75FeNiO7-δ300 DEG C electronic conductivity reach 221S/cm, polarization impedance of the air pole material as proton conductor SOFC at 700 DEG C is 0.21Ω/cm2, maximum power density reaches 517.81mWcm-2。
The cryogenic property and long-time stability for improving solid oxide fuel cell, have reached the purpose of the present invention.
Advantage：The air pole material of the present invention has ion-electron hybrid conductive performance, and middle low temperature comprehensive performance is good, By the parts the Ni substitution Fe of high price La part substitution Sr and divalent, ion and electronic conduction ability are improved, in middle low temperature item There is higher catalytic activity under part.
The present invention has good ion and Electronic Transport of Two Benzene simultaneously, has good chemical property, is a kind of comprehensive Close air pole material functional and suitable for middle low temperature.
Description of the drawings：
Description of the drawings：
Fig. 1 be the present invention pretreatment after powder XRD diagram.
Fig. 2 is the conductivity and temperature relation figure of the present invention.
Fig. 3 is the battery performance figure of the proton conductor solid oxide fuel cell of the present invention.
Fig. 4 is that the electrochemical impedance of the proton conductor solid oxide fuel cell of the present invention varies with temperature relational graph.
Fig. 5 is the ohmage Ro of the present invention, the relational graph between polarization impedance Rp and total impedance Rt.
Specific implementation mode
The embodiment of the present invention is further described below in conjunction with the accompanying drawings：
The present invention includes the preparation method of air pole material and its air pole material；
The air pole material：Select the Sr of perovskite-like oxide3Fe2O7-δMatrix, A are taken using the La of trivalent In generation, further increases the structural stability of material, and B, using transition metal Ni part substitution Fe, further increase the electricity of material Conductance and catalytic activity.
The preparation method of the air pole material is：Using improved combustion method of citric acid powder, the improved lemon Lemon acid burning legal system powder is that suitable complexing agent ethylenediamine tetra-acetic acid is added in traditional combustion method of citric acid, according to La: Sr:Fe:Ni=0.25:2.75:1:1 molar ratio weighs the chemical raw material corresponding to each element, and citric acid, second is added Two kinds of complexing agents of ethylenediamine tetraacetic acid (EDTA) (EDTA) add nitric acid and ammonia solvent, and adjusting PH is 7-8, is evaporated and sinters powder into, Again in 1200 DEG C of pre-burning 3h, air pole material powder is obtained.
Specific preparation process：
(1) required raw material is calculated according to the molal weight of each element first：La(NO3)3·6H2O、Sr(NO3)2、 Fe (NO3)3·9H2O、Ni(NO3)3·6H2The quality of O, and four kinds of raw material weighings are put into well in a clean beaker, then press Complexing agent, wherein citric acid is added in molar ratio：Ethylenediamine tetra-acetic acid：Metal ion, the metal ion are La+Sr+Fe + Ni, molar ratio 1:0.8:1, add 50-100ml distilled water after complexing agent to be put into the beaker for preparing raw material, adds 15- 20ml nitric acid, stirring, ultrasound add ammonium hydroxide, and adjusting PH is 7-8, obtains clear solution；
(2) clear solution that step (1) prepares is put into evaporating dish and is heated, stirred when solution is evaporated soon, to prevent Only uneven heating causes liquid splash or evaporating dish to crack, and stirring is sticky to solution and violent combustion reaction occurs, and obtains just Beginning powder；Initial powder is collected after cooling and is put into high temperature alumina crucible, and crucible is put into 1200 DEG C of -3h of Muffle furnace pre-burning, Obtain air pole material powder.
Embodiment 1：Weigh La (NO3)3·6H2O、Sr(NO3)2、Fe(NO3)3·9H2O、Ni(NO3)3·6H2O is raw material, Complexing agent citric acid, ethylenediamine tetra-acetic acid, wherein citric acid are weighed again：Ethylenediamine tetra-acetic acid：Metal ion (La+Sr+Fe+Ni) Molar ratio is 1:0.8:1.It is put into clean beaker, adds 50-100ml distilled water, adds 15-20ml nitric acid, is stirred, Ultrasound dissolves citric acid and EDTA as possible, adds ammonium hydroxide, and adjusting PH is 7-8, at the uniform velocity stirs, obtains clear solution.
The clear solution prepared is put into evaporating dish and is heated, concentration is burnt until being evaporated and starting, and stops heating, Powder is obtained, is put into 1200 DEG C of -3h of Muffle furnace pre-burning later, organic matter is removed, obtains La0.25Sr2.75FeNiO7-δPowder.
By La0.25Sr2.75FeNiO7-δSuitable terpinol for containing 10% ethyl cellulose is added in powder, wherein La0.25Sr2.75FeNiO7-δThe mass ratio of powder and terpinol-ethyl cellulose is 1:1.5, it grinds two hours, obtains cathode slurry Material.Use quality ratio is 6:4=NiO:BaZr0.1Ce0.7Y0.2O3-δAdd 30% starch as anode, BaZr0.1Ce0.7Y0.2O3-δ As electrolyte, NiO-BaZr0.1Ce0.7Y0.2O3-δAs functional layer, the method for pressing anode-supported altogether using three layers makes half electricity Pond is put into 1400 DEG C of sintering 5h of Muffle furnace, three times cathode slurries is painted after taking-up, often brushes one times and dries 10-20 in drying box Minute, 1000 DEG C of sintering 3h of Muffle furnace are finally putting into, full battery to be measured is obtained.
Weigh the La of prior milled0.25Sr2.75FeNiO7-δCathode powder 1.5g or so is placed in clean mortar.Xiang Fen A small amount of PVAC polyvinylalcohol (two drops) is added in body to increase the viscosity and plasticity of powder, powder is mixed to mill altogether with PVA It 20 minutes, after powder densification, is put into compression bar mold, pays attention to paving, however hand forcing press, it is pressurized to 4MPa or so, Pressurize 30 seconds, takes out the cathode strip being pressed into, is put into high temperature furnace, is taken out after being sintered 5 hours at 1350 DEG C, is made and is used for Test the strip of cathode conductivity.
Use X-ray diffractometer（Shimadzu 7000S/L types）Structural analysis is carried out to the LSFN cathode powders after pre-burning, obtains figure 1, Fig. 1 La0.25Sr2.75FeNiO7-δThe XRD diagram of powder after pretreatment.It can be seen that sample LSFN phases are pure, do not find other Dephasign.
Use digital multimeter（Keithley 2000）The conductivity for testing cathode powder sintering item, obtains Fig. 2, Fig. 2 is La0.25Sr2.75FeNiO7-δConductivity and temperature relation figure, therefrom can be observed cathode conductivity increased gradually with temperature under Drop.
Use electronic load（This IT8511 of Edk）Monocell working curve is tested, obtains Fig. 3, Fig. 3 is La0.25Sr2.75FeNiO7-δThe proton conductor solid oxide fuel cell as air pole battery performance figure, anodic gas For 3% H2O-97%H2, cathode gas is air.700 DEG C of open-circuit voltage is about 1V, maximum power density 517.81mWcm-2。
Use electrochemical workstation（Shanghai Chen Hua）The impedance for testing monocell, obtains Fig. 4, Fig. 4 is La0.25Sr2.75FeNiO7-δThe electrochemical impedance of the proton conductor solid oxide fuel cell as air pole become with temperature Change relational graph, and a step calculates the relationship between Ohmic resistance, polarization resistance and all-in resistance, sees that Fig. 5, Fig. 5 are La0.25Sr2.75FeNiO7-δThe proton conductor solid oxide fuel cell as air pole ohmage Ro, polarization impedance Relational graph between Rp and total impedance Rt, it is seen that battery polarization impedance is 0.21 Ω cm at 700 DEG C-2。

Claims (3)

1. a kind of air pole material of intermediate temperature solid oxide fuel cell, it is characterized in that：Air pole material：Select class calcium titanium The Sr of mine oxide3Fe2O7-δMatrix, the A La using trivalent replace, and further increase the structural stability of material, B utilizations Transition metal Ni part substitution Fe, further increase the conductivity and catalytic activity of material.
2. the preparation method of the air pole material of intermediate temperature solid oxide fuel cell described in claim 1, it is characterized in that： The preparation method of the air pole material is：Using improved combustion method of citric acid powder, according to La: Sr: Fe: Ni= 0.25:2.75:1:1 molar ratio weighs the chemical raw material corresponding to each element, and citric acid, ethylenediamine tetra-acetic acid is added （EDTA）Two kinds of complexing agents add nitric acid and ammonia solvent, and adjusting PH is 7-8, is evaporated and sinters powder into, then pre- at 1200 DEG C 3h is burnt, air pole material powder is obtained.
3. the preparation method of the air pole material of intermediate temperature solid oxide fuel cell described in claim 1, it is characterized in that： Specific preparation process：
（1）Required raw material is calculated according to the molal weight of each element first：La(NO3)3·6H2O、Sr(NO3)2、Fe(NO3)3· 9H2O、Ni(NO3)3·6H2The quality of O, and four kinds of raw material weighings are put into well in a clean beaker, then example in molar ratio Complexing agent is added,
Citric acid：Ethylenediamine tetra-acetic acid：Metal ion, the metal ion are La+Sr+Fe+Ni, molar ratio 1:0.8:1, Add 50-100ml distilled water after complexing agent to be put into the beaker for preparing raw material, add 15-20ml nitric acid, stirs, ultrasound, then add Enter ammonium hydroxide, adjusting PH is 7-8, obtains clear solution；
（2）By step（1）The clear solution prepared, which is put into evaporating dish, to be heated, and is stirred when solution is evaporated soon, with prevent by Hot unevenness causes liquid splash or evaporating dish to crack, and stirring is sticky to solution and violent combustion reaction occurs, and obtains initial powder Body；Initial powder is collected after cooling and is put into high temperature alumina crucible, and crucible is put into 1200 DEG C of -3h of Muffle furnace pre-burning, is obtained Air pole material powder.
CN201810327177.0A 2018-04-12 2018-04-12 A kind of the air pole material and preparation method of intermediate temperature solid oxide fuel cell Pending CN108649236A (en)

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CN110931809A (en) * 2019-11-27 2020-03-27 武汉工程大学 Doped medium-low temperature SOFC cathode material, preparation method and application thereof, and SOFC cathode material
CN111129517A (en) * 2019-12-30 2020-05-08 黑龙江大学 Preparation method of Ruddlesden-Popper layered structure iron-based cathode catalyst
CN111747383A (en) * 2020-05-23 2020-10-09 北京工业大学 Ruddlesden-Popper layered perovskite structure single-phase ferroelectric photovoltaic material
CN111916763A (en) * 2020-09-02 2020-11-10 厦门理工学院 Graphene-based catalyst for air electrode and preparation method thereof
CN112164808A (en) * 2020-09-24 2021-01-01 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of oxygen reduction reaction electrocatalyst for fluorine-doped praseodymium, strontium and cobalt solid oxide fuel cell and product thereof
CN112221506A (en) * 2020-09-29 2021-01-15 广州大学 Catalyst, preparation method and application thereof
CN112952171A (en) * 2021-01-29 2021-06-11 中国矿业大学 Barium cerate substrate sub-conductor-based integrated fully-symmetrical solid oxide fuel cell electrode material and preparation and application thereof
CN114349059A (en) * 2021-12-22 2022-04-15 南华大学 Preparation and application of novel uranium-fixed solid oxide fuel cell cathode material
CN114520356A (en) * 2020-11-19 2022-05-20 中国科学院上海硅酸盐研究所 One-step low-temperature co-fired proton conductor type reversible solid oxide battery and preparation method thereof
CN114538912A (en) * 2022-01-07 2022-05-27 中国科学技术大学 Layered perovskite-like structure oxide and preparation method and application thereof

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110931809A (en) * 2019-11-27 2020-03-27 武汉工程大学 Doped medium-low temperature SOFC cathode material, preparation method and application thereof, and SOFC cathode material
CN111129517A (en) * 2019-12-30 2020-05-08 黑龙江大学 Preparation method of Ruddlesden-Popper layered structure iron-based cathode catalyst
CN111747383A (en) * 2020-05-23 2020-10-09 北京工业大学 Ruddlesden-Popper layered perovskite structure single-phase ferroelectric photovoltaic material
CN111747383B (en) * 2020-05-23 2022-09-23 北京工业大学 Ruddlesden-Popper layered perovskite structure single-phase ferroelectric photovoltaic material
CN111916763A (en) * 2020-09-02 2020-11-10 厦门理工学院 Graphene-based catalyst for air electrode and preparation method thereof
CN111916763B (en) * 2020-09-02 2021-11-02 厦门理工学院 Graphene-based catalyst for air electrode and preparation method thereof
CN112164808A (en) * 2020-09-24 2021-01-01 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of oxygen reduction reaction electrocatalyst for fluorine-doped praseodymium, strontium and cobalt solid oxide fuel cell and product thereof
CN112221506A (en) * 2020-09-29 2021-01-15 广州大学 Catalyst, preparation method and application thereof
CN114520356A (en) * 2020-11-19 2022-05-20 中国科学院上海硅酸盐研究所 One-step low-temperature co-fired proton conductor type reversible solid oxide battery and preparation method thereof
CN114520356B (en) * 2020-11-19 2024-02-06 中国科学院上海硅酸盐研究所 Proton conductor type reversible solid oxide battery co-fired at one step at low temperature and preparation method thereof
CN112952171A (en) * 2021-01-29 2021-06-11 中国矿业大学 Barium cerate substrate sub-conductor-based integrated fully-symmetrical solid oxide fuel cell electrode material and preparation and application thereof
CN112952171B (en) * 2021-01-29 2022-03-22 中国矿业大学 Barium cerate substrate sub-conductor-based integrated fully-symmetrical solid oxide fuel cell electrode material and preparation and application thereof
CN114349059A (en) * 2021-12-22 2022-04-15 南华大学 Preparation and application of novel uranium-fixed solid oxide fuel cell cathode material
CN114349059B (en) * 2021-12-22 2023-10-20 南华大学 Preparation and application of novel uranium-fixed solid oxide fuel cell cathode material
CN114538912A (en) * 2022-01-07 2022-05-27 中国科学技术大学 Layered perovskite-like structure oxide and preparation method and application thereof

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Application publication date: 20181012