CN1560945A - 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 PDFInfo
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- CN1560945A CN1560945A CNA2004100285159A CN200410028515A CN1560945A CN 1560945 A CN1560945 A CN 1560945A CN A2004100285159 A CNA2004100285159 A CN A2004100285159A CN 200410028515 A CN200410028515 A CN 200410028515A CN 1560945 A CN1560945 A CN 1560945A
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- 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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- 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
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- 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
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Abstract
This invention relates to medium solid oxide fuel battery complex electrode material and its preparing method, in which, its component and content are electrode material and high oxygen ions electric conduction powders, the mass of which is 5%-60% to that of the complex electrode, the composition of the conduction material and structure are the same with the electrolyte material of fuel batteries or in a same series. The preparation steps are preparing conduction material powders to be mixed with electrode material, ground to be matched to polar slurry. The stability of oxygen ions conduction and electrode structure, its compatibility with electrolyte and its activity are increased by doping the materials in the same series with La gallate series electrolyte material in the same structure and high oxygen ions conduction.
Description
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, the The Nomenclature Composition and Structure of Complexes of hyperoxia ionic conductivity material or homologous series consistent with fuel battery electrolyte material.
Said electrode material itself can be high oxygen-ion conduction-electronic conductance mixed conductor material, the oxide of high electronic conductance, or nickel, cobalt, metal materials such as iron or copper.
The The Nomenclature Composition and Structure of Complexes of said hyperoxia ionic conductivity material or homologous series consistent with fuel battery electrolyte material can be selected from 1 at different electrolyte) lanthanum gallate series electrolyte; Or 2) the zirconia series electrolyte that mixes; Or 3) doping of cerium oxide series electrolyte.
Said lanthanum gallate series electrolyte can be selected from 1) with the lanthanum gallate of strontium, magnesium, 3 kinds of element dopings of cobalt; Or 2) with the lanthanum gallate of strontium, magnesium, 3 kinds of element dopings of nickel; Or 3) with the lanthanum gallate of strontium, magnesium, 3 kinds of element dopings of iron.
Said lanthanum gallate with strontium, magnesium, 3 kinds of element dopings of cobalt specifically consist of 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.
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
0.09O
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 (8)
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, the The Nomenclature Composition and Structure of Complexes of hyperoxia ionic conductivity material or homologous series consistent with fuel battery electrolyte material.
2, intermediate temperature solid oxide fuel cell combination electrode material as claimed in claim 1, it is characterized in that said electrode material is originally as hyperoxia ionic conductance-electronic conductance mixed conductor material, the oxide of high electronic conductance, or nickel, cobalt, metal materials such as iron or copper.
3, intermediate temperature solid oxide fuel cell combination electrode material as claimed in claim 1, it is characterized in that the The Nomenclature Composition and Structure of Complexes of said hyperoxia ionic conductivity material consistent with fuel battery electrolyte material or with the electrolyte homologous series.
4, intermediate temperature solid oxide fuel cell combination electrode material as claimed in claim 1 is characterized in that the composition of said hyperoxia ionic conductivity material is selected from 1) lanthanum gallate series electrolyte; Or 2) the zirconia series electrolyte that mixes; Or 3) doping of cerium oxide series electrolyte.
5, intermediate temperature solid oxide fuel cell combination electrode material as claimed in claim 4 is characterized in that said lanthanum gallate series electrolyte is selected from 1) with the lanthanum gallate of strontium, magnesium, 3 kinds of element dopings of cobalt; Or 2) with the lanthanum gallate of strontium, magnesium, 3 kinds of element dopings of nickel; Or 3) with the lanthanum gallate of strontium, magnesium, 3 kinds of element dopings of iron.
6, intermediate temperature solid oxide fuel cell combination electrode material as claimed in claim 5, what it is characterized in that said lanthanum gallate with strontium, magnesium, 3 kinds of element dopings of cobalt specifically consists of La
0.8Sr
0.2Ga
0.8Mg
0.2～xCo
xO
3, x=0～0.15.
7, the preparation method of intermediate temperature solid oxide fuel cell combination electrode material 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.
8, the preparation method of intermediate temperature solid oxide fuel cell combination electrode material as claimed in claim 7 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.
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|---|---|---|---|
| CNB2004100285159A CN1272864C (en) | 2004-03-05 | 2004-03-05 | Intermediate solid oxide fuel batter combination electrode material and its manufacturing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100285159A CN1272864C (en) | 2004-03-05 | 2004-03-05 | Intermediate solid oxide fuel batter combination electrode material and its manufacturing method |
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| Publication Number | Publication Date |
|---|---|
| CN1560945A true CN1560945A (en) | 2005-01-05 |
| CN1272864C CN1272864C (en) | 2006-08-30 |
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Cited By (2)
| 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 |
| CN106430289A (en) * | 2015-08-06 | 2017-02-22 | 中国科学院大连化学物理研究所 | Method for low temperature preparation of high specific surface area nanometer gallate spinel |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI442694B (en) | 2003-05-30 | 2014-06-21 | Asml Netherlands Bv | Lithographic apparatus and device manufacturing method |
-
2004
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Cited By (3)
| 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 |
| CN106430289A (en) * | 2015-08-06 | 2017-02-22 | 中国科学院大连化学物理研究所 | Method for low temperature preparation of high specific surface area nanometer gallate spinel |
| 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 |
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