CN1272864C - Intermediate solid oxide fuel batter combination electrode material and its manufacturing method - Google Patents

Intermediate solid oxide fuel batter combination electrode material and its manufacturing method Download PDF

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CN1272864C
CN1272864C CNB2004100285159A CN200410028515A CN1272864C CN 1272864 C CN1272864 C CN 1272864C CN B2004100285159 A CNB2004100285159 A CN B2004100285159A CN 200410028515 A CN200410028515 A CN 200410028515A CN 1272864 C CN1272864 C CN 1272864C
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electrode
electrolyte
hyperoxia
ionic conductivity
conductance
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CN1560945A (en
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王世忠
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Xiamen University
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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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The present invention relates to an intermediate solid oxide fuel battery combination electrode material and a manufacturing method thereof. The ingredients of the electrode material are electrode material and high oxygen ionic conductance material powder, and the content is that the weight of the conductance material powders occupies 5%-60% of the combination electrode. The composition and the structure of the conductance material are consistent or homologous with those of a fuel-battery electrolyte material. The manufacturing method comprises the preparing steps of preparing the conductance material powder; mixing and grinding the conductance material powder and the electrode material to prepare electrode pulp. By mixing the homologous series material having the same structure and the high oxygen ionic conductance with a gallic acid la series electrolyte material in the electrode, the oxide ion conductance of the electrode, the stability of the electrode structure, the compatibility of the electrolyte, the activity and the stability of the electrode are raised. Series material having the same structure and the high oxygen ionic conductance with a gallic acid la series electrolyte material, the oxide ion conductance of the electrode, the stability of the electrode structure, the compatibility of the electrolyte, the activity and the stability of the electrode are raised. Due to the fact that the doped homologous series electrolyte powdered material has the similar structure with that of the electrolyte, the electrolyte powdered material has the similar thermal expansion coefficient with that of the electrolyte. The binding degree of the electrode and the electrolyte can be raised, and the stability of the electrode structure at high temperature is raised.

Description

Intermediate temperature solid oxide fuel cell combination electrode material and preparation method thereof
Technical field
The present invention relates to a kind of combination electrode material of fuel cell, especially a kind of general high activity, formation of high stability intermediate temperature solid oxide fuel cell combination electrode material and preparation method thereof.
Background technology
The lanthanum gallate series material (US 6586127 B1 patents) of Ishihara invention is a temperature oxygen ion conductor in the extraordinary class of performance, because this electrolytical invention time is shorter, lacks the development of corresponding electrode material.Be the activity and stability that guarantee electrode, the electrode of Solid Oxide Fuel Cell is combination electrode usually.For being electrolytical system with the lanthanum gallate series material, the alloy of combination electrode is generally doping of cerium oxide.(utilize the activity of samarium doped cerium oxide raising fuel cell, Acta PhySico-Chimica Sinica, 2003,19 (9): 844; Utilize samarium doping of cerium oxide interlayer to improve the activity of anode of fuel cell, Acta PhySico-Chimica Sinica, 2003,19 (9): 849) because cerium oxide and lanthanum gallate are differing far away aspect crystal phase structure and the various physical property, considering from life-span of battery long-time running, is that the electrode and the lanthanum gallate electrolyte of raw material may exist unmatched problem with the cerium oxide.If can utilize the feedstock production electrode close with lanthanum gallate character, may be favourable to the life-span of battery.
Summary of the invention
The object of the present invention is to provide a kind of general high activity, high stability intermediate temperature solid oxide fuel cell combination electrode material and preparation method thereof.
Technical scheme of the present invention is to form identical or isonomic hyperoxia ionic conductivity material powder by adding in electrode material with electrolyte, to improve the electro-chemical activity and the stability of battery.The preparation method of the combination electrode material that the present invention is given is equally applicable to other electrolyte system intermediate temperature solid oxide fuel cell.
The component of the said intermediate temperature solid oxide fuel cell combination electrode material of the present invention and be: electrode material itself and hyperoxia ionic conductivity material powder by the content of mass ratio, the quality of the hyperoxia ionic conductivity material powder that adds accounts for 5%～60% of combination electrode gross mass, hyperoxia ionic conductivity material The Nomenclature Composition and Structure of Complexes or homologous series consistent with fuel battery electrolyte material.
Electrode material is Sm 0.5Sr 0.5CoO 3", the hyperoxia ionic conductivity material is La 0.8Sr 0.2Ga 0.8Mg 0.2-xCo xO 3, x=0～0.15.
The preparation method of the said intermediate temperature solid oxide fuel cell combination electrode material of the present invention is:
1) preparation hyperoxia ionic conductivity material powder;
2) hyperoxia ionic conductivity material powder is mixed with electrode material, grind, and be made into electrode slurry, wherein the quality of hyperoxia ionic conductivity material accounts for 5%～60% of combination electrode gross mass.
Electrode material is Sm 0.5Sr 0.5CoO 3", the hyperoxia ionic conductivity material is La 0.8Sr 0.2Ga 0.8Mg 0.2-xCo xO 3, x=0～0.15.
Said hyperoxia ionic conductivity material powder can utilize solwution method or solid-phase synthesis to make.
The step of said hyperoxia ionic conductivity material powder solid-phase synthesis is:
1, with the La of purity 〉=99.95% 2O 3, Ga 2O 3, SrCO 3, MgO, CoO raw material mix and to be incorporated in ball milling 12～24h in the alcohol medium;
2, dry back is at 1100～1500 ℃ of roasting 2～24h;
3, after the roasting, in the alcohol medium ball milling to granularity less than 10 μ m.
The combination electrode material for preparing is made into electrode slurry, utilize method for printing screen with electrode preparation in electrolytical surface, the thickness of electrode is at 10～100 μ m; According to the difference of type of electrodes with electrode at 800～1300 ℃ of roasting 0.5～10h.
Utilization in electrode, mix oxygen-ion conduction that the homologous series material that has same structure and a high oxygen-ion conduction with lanthanum gallate series electrolyte improves electrode, electrode structure stability and with electrolytical compatibility, thereby improve the activity and stability of electrode.Thereby have close thermal coefficient of expansion owing to the homology electrolyte powder powder material that mixes is close with electrolyte structure, can improve electrode and electrolytical combination degree; The electrolyte powder has the characteristic of high temperature resistant sintering usually, can improve the stability of electrode structure at high temperature after mixing electrode; Thereby electrolyte powder has high oxygen-ion conduction makes oxonium ion can transfer to electrode interior, makes to be reflected at electrode interior and to carry out, and enlarges the zone of reaction.
Description of drawings
Fig. 1 is the micro-structure diagram of 900 ℃ of roasting electrode surfaces.(1) .70wt%Sm wherein 0.5Sr 0.5CoO 3～30wt%La 0.8Sr 0.2Ga 0.8Mg 0.11Co 0.09O 3(2) .70wt%Sm 0.5Sr 0.5CoO 3-30wt%La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3(3) .Sm 0.5Sr 0.5CoO 3
Fig. 2 is in 800 ℃ of air, 70wt%Sm 0.5Sr 0.5CoO 3-30wt%La 0.8Sr 0.2Ga 0.8Mg 0.11Co 0.09O 3, Sm 0.5Sr 0.5CoO 3The comparison diagram of electrode polarization curve.■ Sm 0.5Sr 0.5CoO 3▲ 70wt%Sm 0.5Sr 0.5CoO 3-30wt%La 0.8Sr 0.2Ga 0.8Mg 0.11Co 0.09O 3, wherein abscissa is overpotential (η c/V), ordinate is polarization current (J/Acm -2).
Fig. 3 is polarization front and back 70wt%Sm in the following 800 ℃ of air of Open Circuit Potential 0.5Sr 0.5CoO 3-30wt%La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3, Sm 0.5Sr 0.5CoO 3The AC impedance of electrode.■ Sm 0.5Sr 0.5CoO 3Before the polarization; Sm 0.5Sr 0.5CoO 3After the polarization; ● 70wt%Sm 0.5Sr 0.5CoO 3-30wt%La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3Before the polarization; Zero 70wt%Sm 0.5Sr 0.5CoO 3-30wt%La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3After the polarization, wherein abscissa is real part of impedance (Zre/ Ω cm -2), ordinate is imaginary part (the Zim/ Ω cm of impedance -2).
Fig. 4 is Sm 0.5Sr 0.5CoO 3/ La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3/ Ni or 90wt%Ni～10wt%LSGMC5 monocell is at 800 ℃ power curve of output.■ Sm 0.5Sr 0.5CoO 3/ La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3The power density curve of/90wt%Ni～10wt%LSGMC5; Sm 0.5Sr 0.5CoO 3/ La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3The volt-ampere curve of/90wt%Ni～10wt%LSGMC5; ● Sm 0.5Sr 0.5CoO 3/ La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3The power density curve of/Ni; Zero Sm 0.5Sr 0.5CoO 3/ La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3The volt-ampere curve of/Ni.Wherein abscissa is current density Currentdensity (Acm -2), left and right sides ordinate is respectively the terminal voltage Terminal voltage (mV) and the power density Power density (Wcm of battery -2).
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
Embodiment 1
Embodiment 1 has prepared Sm 0.5Sr 0.5CoO 3-La 0.8Sr 0.2Ga 0.8Mg 0.11Co 0.09O 3(SSC-LSGMC9), Sm 0.5Sr 0.5CoO 3-La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3(SSC-LSGMC5) combination electrode material is investigated LSGMC9, the LSGMC5 facilitation to SSC electrode structure stability.Electrolyte is for adopting the La of foregoing solid-phase synthesis preparation 0.9Sr 0.1Ga 0.8Mg 0.2O 3
The SSC powder adopts solid phase method synthetic, and raw material is Sm 2O 3(99.99%), SrCO 3(99.99%), Co (CH 3COO) 2.4H 2O (99.99%).After raw material adds alcohol and grinds 0.5h with mortar, at 650～750 ℃ of pre-burning 2h.After sample after the pre-burning adds alcohol grinding 0.5h, at 1000～1200 ℃ of roasting 6～12h.Sample after the pre-burning adds alcohol and grinds behind the 0.5h standby.
La 0.8Sr 0.2Ga 0.8Mg 0.11Co 0.99O 3, La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3Adopt solid-phase synthesis.La with high-purity (99.99%) 2O 3, Ga 2O 3, SrCO 3, MgO, CoO raw material mix and be incorporated in ball milling 12-24h in the alcohol medium, dry back is at 1200～1400 ℃ of roasting 2-24h.After the roasting, ball milling 6～12h in the alcohol medium, the granularity of electrolyte powder is less than 10 μ m.
Being prepared as directly of combination electrode, ball milling 2～12h in the alcohol medium then with electrolyte powder and SSC powder.Combination electrode material is made into slurry, utilizes method for printing screen to be printed onto La 0.9Sr 0.1Ga 0.8Mg 0.2O 3Bath surface, and at 800～1000 ℃ of roasting 2～4h.
Fig. 1 is two kinds of combination electrode surface microstructures and the comparison of the SSC negative electrode of preparation under the same conditions.The result shows that pure SSC electrode has tangible sintering phenomenon, electrolyte powder mix the sintering that has suppressed electrode particle significantly, show that method of the present invention can improve the stability of electrode structure.The improvement of high temperature sintering electrolyte powder foot couple electrode structure stability is more obvious.
Embodiment 2
Embodiment 2 has tested the Sm with method for preparing 0.5Sr 0.5CoO 3-La 0.8Sr 0.2Ga 0.8Mg 0.11Co 0.09O 3(SSC-LSGMC9) electro-chemical activity of combination electrode material is investigated the facilitation of LSGMC9 to electrode activity.Known three-electrode system is adopted in the test of electrode polarization curve, utilizes potentiostatic method to carry out.Test condition is in 800 ℃ of air, the results are shown in Fig. 2.Shown that by Fig. 2 LSGMC9 mixes the activity that has significantly improved electrode, under identical overpotential, SSC-LSGMC9 has far above pure SSC polarization of electrode electric current.
Embodiment 3
Embodiment 3 utilizes the AC impedance method to test Sm with the preparation of the method for embodiment 1 0.5Sr 0.5CoO 3-La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3(SSC-LSGMC5) electro-chemical activity of combination electrode material is investigated the facilitation of LSGMC5 to electrode activity and stability.Known three-electrode system in the document is adopted in the test of AC impedance experiment, utilizes the constant potential mode to carry out.Test condition is in 800 ℃ of air.AC impedance after the polarization was for carrying out 600～800 ℃, behind the polarization experiment in+0.8～0.8 interval, and the experiment that stable 24h carries out.The results are shown in Fig. 3.
Fig. 3 shows, LSGMC5 mixes the activity that has improved electrode, has reduced SSC polarization of electrode resistance.After the strong in addition polarization, the impedance spectrum of SSC-LSGMC5 does not have obvious variation, and SSC polarization of electrode resistance significantly increases, and shows that LSGMC5 has significantly improved the activity and stability of electrode.
Embodiment 4
Embodiment 4 has prepared Sm 0.5Sr 0.5CoO 3/ La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3/ Ni or 90wt%Ni～10wt%LSGMC5 monocell.Sm 0.5Sr 0.5CoO 3And La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3Preparation adopt known method, Ni is commercial nickel oxide powder (purity 99.99%, granularity 1 μ m).The preparation of 90wt%Ni～10wt%LSGMC5 combination electrode is adopted above-mentioned nickel oxide powder is mixed with the LSGMC5 powder, and the method with mortar grinding 0.5h obtains in alcohol then.1 method preparation among the LSGMC5 employing embodiment.
Reaction temperature is 800 ℃, and the reaction gas that feeds Ni or 90wt%Ni～10wt%LSGMC5 electrode is the hydrogen that contains saturated steam under the room temperature, feeds Sm 0.5Sr 0.5CoO 3The gas of negative electrode is pure oxygen.With Ni and 90wt%Ni～10wt%LSGMC5 is that the power out-put characteristic of the monocell of anode is shown in Fig. 4.The result of Fig. 4 shows, be that the activity of the battery of anode is significantly higher than with the pure nickel with 90wt%Ni～10wt%LSGMC5 is the battery of anode.
Embodiment 5
With Sm 0.5Sr 0.5CoO 3(SSC) be example, simply introduce the preparation of electrode material.Sm 0.5Sr 0.5CoO 3(SSC) powder adopts solid phase method synthetic.Raw material is Sm 2O 3(99.99%), SrCO 3(99.99%), Co (CH 3COO) 2.4H 2O (99.99%).After raw material adds alcohol and grinds 0.5-2h with mortar, at 600～800 ℃ of pre-burning 2h.After sample after the pre-burning adds alcohol grinding 0.5h, at 900～1300 ℃ of roasting 12h.It is standby that sample after the roasting grinds the back.Being prepared as directly of combination electrode mixes electrolyte powder with the SSC cathode powder, then ball milling 2～12h in the alcohol medium.Can adopt commercial nickel powder (granularity 1～10 μ m) for the pure nickel electrode.
The preparation of combination electrode can also be adopted infusion process, and the electrolyte powder impregnation that will synthesize is in the nitrate or other salting liquid of electrode material, after the drying, in suitable temperature roasting.With Ni～La 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3Be example, its preparation method is with the La for preparing 0.8Sr 0.2Ga 0.8Mg 0.15Co 0.05O 3Powder impregnation boils in nickel nitrate solution and evaporate to dryness, and pre-burning 2～5h between 500～800 ℃ is behind ball milling 2～12h, at 1000～1400 ℃ of roasting 2-24h.

Claims (3)

1, intermediate temperature solid oxide fuel cell combination electrode material, it is characterized in that its component and be: electrode material itself and hyperoxia ionic conductivity material powder by the content of mass ratio, the quality of hyperoxia ionic conductivity material powder accounts for 5%～60% of combination electrode gross mass, and the The Nomenclature Composition and Structure of Complexes of hyperoxia ionic conductivity material is consistent with fuel battery electrolyte material; Said electrode material is Sm 0.5Sr 0.5CoO 3The hyperoxia ionic conductivity material is La 0.8Sr 0.2Ga 0.8Mg 0.2-xCo xO 3, x=0.05～0.09.
2, the preparation method of intermediate temperature solid oxide fuel cell combination electrode material as claimed in claim 1 is characterized in that its step is
1) preparation hyperoxia ionic conductivity material powder;
2) hyperoxia ionic conductivity material powder is mixed with electrode material, grind, and be made into electrode slurry, wherein the quality of hyperoxia ionic conductivity material accounts for 5%～60% of combination electrode gross mass;
Said hyperoxia ionic conductivity material is La 0.8Sr 0.2Ga 0.8Mg 0.2-xCo xO 3, x=0～0.15, electrode material is Sm 0.5Sr 0.5CoO 3
3, the preparation method of intermediate temperature solid oxide fuel cell combination electrode material as claimed in claim 2 is characterized in that said hyperoxia ionic conductivity material powder utilizes solid-phase synthesis to make, and the steps include:
1), with the La of purity 〉=99.95% 2O 3, Ga 2O 3, SrCO 3, MgO, CoO raw material mix and to be incorporated in ball milling 12～24h in the alcohol medium;
2), dry back is at 1100～1500 ℃ of roasting 2～24h;
3), after the roasting, in the alcohol medium ball milling to granularity less than 10 μ m.
CNB2004100285159A 2004-03-05 2004-03-05 Intermediate solid oxide fuel batter combination electrode material and its manufacturing method Expired - Fee Related CN1272864C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7804574B2 (en) 2003-05-30 2010-09-28 Asml Netherlands B.V. Lithographic apparatus and device manufacturing method using acidic liquid

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1324740C (en) * 2005-08-19 2007-07-04 黑龙江大学 Solid oxide fuel cell cathode material
CN106430289B (en) * 2015-08-06 2018-03-20 中国科学院大连化学物理研究所 A kind of method of low temperature preparation high-specific area nano gallate spinel

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7804574B2 (en) 2003-05-30 2010-09-28 Asml Netherlands B.V. Lithographic apparatus and device manufacturing method using acidic liquid
US7808611B2 (en) 2003-05-30 2010-10-05 Asml Netherlands B.V. Lithographic apparatus and device manufacturing method using acidic liquid
US8416385B2 (en) 2003-05-30 2013-04-09 Asml Netherlands B.V. Lithographic apparatus and device manufacturing method

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