CN104103837B - The intermediate temperature solid oxide fuel cell cathode material of resistant to carbon dioxide and application - Google Patents
The intermediate temperature solid oxide fuel cell cathode material of resistant to carbon dioxide and application Download PDFInfo
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8652—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites as mixture
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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
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- Y02E60/50—Fuel cells
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Abstract
The invention discloses the intermediate temperature solid oxide fuel cell cathode material of a kind of resistant to carbon dioxide, consisting of La1‑xSrxCoyFe1‑yO3‑δ‑Ln0.8Sr0.2MnO3+d(Ln=La,Ce,Pr,Nd,Ga,Sm；0.1≤x≤0.5；0≤y≤1；0≤δ≤0.25；0≤d≤0.05).The cathode material of the present invention has good intermediate temperature solid oxide fuel cell (SOFC) cathode performance, illustrate the stability of excellent resistant to carbon dioxide, overcome conventional negative electrode shortcoming of deep fades in the oxidant containing carbon dioxide, be the intermediate temperature solid oxide fuel cell cathode material of a kind of excellent resistant to carbon dioxide.
Description
Technical field
The present invention relates to fuel cell field, be specifically related to the middle low-temperature solid oxidation of a kind of resistant to carbon dioxide
Thing fuel battery cathode material and preparation thereof and application.
Background technology
SOFC (Solid Oxide Fuel Cell is called for short SOFC) is that one is at high temperature passed through
The chemical energy being stored in fuel and oxidant directly efficiently, is environmentally friendly changed into electric energy by chemical reaction
All solid state TRT, be one of the most promising clean energy technology.Reducing cost is SOFC commercialization
Key issue.Therefore, reducing the running temperature of SOFC, development intermediate temperature solid oxide fuel cell is
Become the research and development focus of SOFC.SOFC is devoted to be applied to large-scale stationary distribution formula electricity
Standing, its business-like projected life is at least higher than 40000h.In long-term running, several factors
Cause the decay of SOFC.The stability of raising SOFC is one of major issue of its commercialization needs solution.
Cathode material conventional for SOFC is perovskite composite oxide, and these oxides are how first containing alkaline earth and rare earth
Element.When air is directly as the oxidant of SOFC, the carbon dioxide of the trace in air, sulfur dioxide,
The easily absorption such as steam forms carbonate, sulfate and hydroxide etc., sternly at cathode surface and with cathode reaction
Important place reduces the performance of SOFC.Therefore, the middle low-temperature solid oxide fuel electricity of a kind of resistant to carbon dioxide is researched and developed
Pool cathode is very important.
Ding et al. " Phys.Chem.Chem.Phys " (Phys.Chem.Chem.Phys.15,489-496,
2013) point out that SrO is at La1-xSrxCoyFe1-yO3-δThe enrichment on surface.Yokokawa et al. is at " Journal of
Alloys and Compounds " (Journal of Alloys and Compounds452,41-47,2008) calculate
(La,Sr)MO3-δThe activity of the SrO on (M=Mn, Fe, Co) surface, SrO activity reduces the most successively:
(La,Sr)CoO3>(La,Sr)FeO3>(La,Sr)MnO3.Under the conditions of cathodic polarization, La1-xSrxCoyFe1-yO3-δ
The Sr element of negative electrode can be enriched with to cathode surface further, and La0.8Sr0.2MnO3+dDo not have this Sr element
Surface enrichment phenomenon.The SrO of cathode surface enrichment is easy to react with carbon dioxide, sulfur dioxide, steam etc.,
Hinder oxygen in cathode surface exchange and oxygen species diffusion into the surface process.If able to suppression cathode surface SrO
Enrichment, may improve the stability that in the anti-air of negative electrode, impurity gas poisons.La1-xSrxCoyFe1-yO3-δNegative electrode
In middle low temperature range, show excellent performance, but there will be surface Sr enrichment.And La0.8Sr0.2MnO3+dIt is
Typical high temperature sofc cathode, does not haves Sr Element surface enrichment phenomenon, but it is in the property of middle low temperature range
Can be the lowest.If the performance of the two and the advantage of stability well combined, one may be developed
The middle low temperature sofc cathode of resistant to carbon dioxide.The present invention is exactly by Ln0.8Sr0.2MnO3+d(Ln is La, Ce, Pr,
Nd,Ga,Sm;0≤d≤0.05) it is prepared into La1-xSrxCoyFe1-yO3-δSurface, the surface enrichment of suppression Sr element,
Improving the stability of the resistant to carbon dioxide of negative electrode, this invention has great practical value.
Summary of the invention
Present invention aim to overcome that what intermediate temperature solid oxide fuel cell negative electrode not resistant to carbon dioxide poisoned
Shortcoming, it is provided that the intermediate temperature solid oxide fuel cell cathode material of a kind of resistant to carbon dioxide.
The present invention is by Ln0.8Sr0.2MnO3+d(Ln is La, Ce, Pr, Nd, Ga, Sm；0≤d≤0.05) it is prepared into
La1-xSrxCoyFe1-yO3-δIn, obtain composite cathode material.In middle low temperature range, this negative electrode shows good
Good chemical property, illustrates the stability of extraordinary resistant to carbon dioxide.
For reaching above-mentioned purpose, present invention employs following technical scheme:
A kind of intermediate temperature solid oxide fuel cell cathode material of resistant to carbon dioxide, consisting of
La1-xSrxCoyFe1-yO3-δ-Ln0.8Sr0.2MnO3+d, wherein, 0.1≤x≤0.5；0≤y≤1；0≤δ≤0.25；
0≤d≤0.05；Ln is La, one or more in Ce, Pr, Nd, Ga, Sm.Wherein,
Ln0.8Sr0.2MnO3+dParticle is evenly dispersed in La1-xSrxCoyFe1-yO3-δParticle surface.Wherein,
Ln0.8Sr0.2MnO3+dContent in cell cathode is 5-20%, by weight percentage.
La in the cathode material of this invention1-xSrxCoyFe1-yO3-δEmploying citric acid method (Mater.Lett.60,
261-265,2006), glycine method (Mater.Lett.10,6-12,1990) and coprecipitation (Daltron Trans..
19,3110-3115,2004) prepare.
The cathode material of this invention is prepared on cell interlayer and can use La1-xSrxCoyFe1-yO3-δWith
Ln0.8Sr0.2MnO3+dPowder is according to the mechanical mixing of certain mass ratio, Ln0.8Sr0.2MnO3+dForerunner's colloidal sol
It is impregnated into La1-xSrxCoyFe1-yO3-δ、Ln0.8Sr0.2MnO3+dForerunner's nitrate solution be impregnated into
La1-xSrxCoyFe1-yO3-δPrepare etc. method.
Ln in cathode material layer0.8Sr0.2MnO3+dParticle is evenly dispersed in La1-xSrxCoyFe1-yO3-δParticle table
Face.
It is an advantage of the current invention that:
(1) negative electrode prepared by the present invention, it is possible to resistant to carbon dioxide poisons.Possible reason is:
Ln0.8Sr0.2MnO3+dSelf having good chemical stability, Sr enrichment of element is inconspicuous, is covered
La1-xSrxCoyFe1-yO3-δSurface, it is suppressed that La1-xSrxCoyFe1-yO3-δMiddle Sr element show enrichment, resistance
Hinder the chemical reaction of itself and carbon dioxide, improve the stability of composite cathode.
(2) negative electrode prepared by the present invention, the good performance at middle low temperature display.Its reason is
Ln0.8Sr0.2MnO3+dThe catalytic oxidation-reduction activity having had, La1-xSrxCoyFe1-yO3-δThere is big oxonium ion
Conductivity, the two combination improves cathode reaction active region.
(3) composite cathode prepared by the present invention can be used for plate, cast, flat-tube type, honeycomb type etc. are multiple
In the SOFC of configuration；It is applicable to multiple intermediate temperature solid oxide fuel cell application neck
Territory, such as compact power, decentralized power s etc..
Below by embodiment, the invention will be further elaborated.
Detailed description of the invention
Comparative example 1
With Ni-YSZ (mass ratio 1:1) as anode, YSZ is electrolyte, and GDC is that interlayer is prepared as anode and props up
The battery component of support type.La is prepared respectively by citric acid method0.6Sr0.4CoO3-δ(LSC), La0.6Sr0.4FeO3-δ
And La (LSF)0.6Sr0.4Co0.2Fe0.8O3-δ(LSCF) at 1000 DEG C of roasting 2h, powder is obtained, respectively by powder
Body (1g) is fully ground and adds appropriate binding agent (n-butanol, 1g), is prepared as cathode slurry.It is coated with respectively
Cover 0.012g cathode slurry (area: 0.5cm2) on the interlayer of the battery component of anode support type, at 1050 DEG C
Roasting 3h, obtains the monocell of coin, is denoted as LSC battery, LSF battery and LSCF battery respectively.
In anode-side, the hydrogen of humidification is as fuel (volumetric concentration 3%H2O,100ml min-1), at negative electrode
Side, oxygen is as oxidant (100ml min-1).(0.15A cm under 600 DEG C and constant current density-2),
LSC cell voltage be 0.94V, LSCF cell voltage be 0.92V, LSF cell voltage be 0.89V.?
Oxygen stream introduces volumetric concentration 2.83%CO2And 2.64%H2After O, 48h, LSC cell voltage have dropped
About 26%, LSCF cell voltage have dropped about 20%, and LSF cell voltage have dropped about 15%.
Embodiment 1
La0.6Sr0.4CoO3-δ-La0.8Sr0.2MnO3+dNegative electrode
Citric acid method is used to prepare La0.6Sr0.4CoO3-δ, by La0.6Sr0.4CoO3-δStoichiometric proportion, will be each
The nitrate of element (La, Sr, Co) joins in water (100ml), after fully dissolving, adds suitable
Amount citric acid (citric acid: metal ion=1.5:1), before the pH value of regulation mixed liquor obtains clarification to 6
Driving solution, colloidal sol, to forming wine-colored colloidal sol, is contained in evaporating dish by heating evaporation moisture, and at electric furnace
In be heated to burning, obtain front axle shell.By La0.6Sr0.4CoO3-δFront axle shell, at 1000 DEG C of roasting 2h.Will
La after roasting0.6Sr0.4CoO3-δPowder (1g) grind and with some organic bonds (n-butanol, 1g), mixed
After conjunction, it is prepared as cathode slurry.Coating 0.012g cathode slurry (area: 0.5cm2) to anode support type
Battery component interlayer on, at 1050 DEG C of roasting 3h.By La0.8Sr0.2MnO3+dStoichiometric proportion, will
The nitrate of each element (La, Sr, Mn) joins in water (100ml), after fully dissolving, adds
Appropriate citric acid (organic acid: metal ion=1.5:1), the pH=1-2 of regulation mixed liquor.Immersion will be mixed
Stain is to La0.6Sr0.4CoO3-δIn, at 900 DEG C, roasting 2h.La0.8Sr0.2MnO3+δContaining in composite cathode
Amount is for 5%(by weight percentage), obtain battery and be denoted as LSC64-LSM5.
In addition to cathode material, the same comparative example of other assembly of battery, the most same comparative example of battery testing condition.
In anode-side, the hydrogen of humidification is as fuel (volumetric concentration 3%H2O,100ml min-1), at cathode side,
Oxygen is as oxidant (100ml min-1).(0.15A cm under 600 DEG C and constant current density-2),
LSC64-LSM5 cell voltage is 0.95V.Volumetric concentration 2.83%CO is introduced in oxygen stream2With 2.64%
H2After O, 48h, LSC64-LSM5 cell voltage have dropped about 7%, and the stability of battery is greatly improved.
La0.6Sr0.4CoO3-δ-La0.8Sr0.2MnO3+dThe stability of negative electrode resistant to carbon dioxide compares La0.6Sr0.4CoO3-δNegative electrode
Significantly improve.
Embodiment 2
La0.6Sr0.4Co0.2Fe0.8O3-δ-La0.8Sr0.2MnO3+dNegative electrode
Glycine method is used to prepare La0.6Sr0.4Co0.2Fe0.8O3-δ, by La0.6Sr0.4Co0.2Fe0.8O3-δChemistry meter
Amount ratio, joins the nitrate of each element (La, Sr, Co, Fe) in water (100ml), fully
After dissolving, adding appropriate glycine (glycine: metal ion=1.5:1), the pH value of regulation mixed liquor is extremely
8 precursor aqueous solutions obtaining clarification, colloidal sol, to forming wine-colored colloidal sol, is contained into evaporating dish by heating evaporation moisture
In, and in electric furnace, it is heated to burning, obtain front axle shell.By La0.6Sr0.4Co0.2Fe0.8O3-δFront axle shell,
1000 DEG C of roasting 2h.By the La after roasting0.6Sr0.4Co0.2Fe0.8O3-δPowder (1g) grinds and organic with some
After adhesive (n-butanol, 1g) mixing, it is prepared as cathode slurry.Coating 0.012g cathode slurry (area:
0.5cm2) on the interlayer of the battery component of anode support type, at 1050 DEG C of roasting 3h.By La0.8Sr0.2MnO3+d
Stoichiometric proportion, the nitrate of each element (La, Sr, Mn) is joined in water (100ml),
Fully dissolve.Nitrate solution is impregnated into La0.6Sr0.4Co0.2Fe0.8O3-δIn, at 900 DEG C, roasting 2h.
Control La0.8Sr0.2MnO3+dContent in composite cathode is respectively 2%, and 5%, 10% and 20%(by weight
Amount percentages), the battery obtained LSCF6428-LSM2, LSCF6428-LSM5 respectively,
LSCF6428-LSM10 and LSCF6428-LSM20.
In addition to cathode material, the same comparative example of other assembly of battery, the most same comparative example of battery testing condition.
In anode-side, the hydrogen of humidification is as fuel (volumetric concentration 3%H2O,100ml min-1), at cathode side,
Oxygen is as oxidant (100ml min-1).(0.15A cm under 600 DEG C and constant current density-2),
LSCF6428-LSM2, LSCF6428-LSM5, LSCF6428-LSM10 and LSCF6428-LSM20
Cell voltage is respectively 0.94, and 0.96,0.95 and 0.90V.Volumetric concentration 2.83%CO is introduced in oxygen stream2
And 2.64%H2After O, 48h, LSCF6428-LSM2, LSCF6428-LSM5, LSCF6428-LSM10
About 5.0%, 1.2%, 1.5% and 1.1% is have dropped with LSCF6428-LSM20 cell voltage.Composite cathode
Having the stability of good resistant to carbon dioxide, this is due to stable La0.8Sr0.2MnO3+dCover
La0.6Sr0.4Co0.2Fe0.8O3-δNot only promote the surface exchange process of oxygen, more inhibit Sr element diffusion and
Surface enrichment, improves negative electrode stability in carbon dioxide.
Embodiment 3
La0.6Sr0.4FeO3-δ-La0.8Sr0.2MnO3+dNegative electrode
Coprecipitation is used to prepare La0.6Sr0.4FeO3-δ, by La0.6Sr0.4FeO3-δStoichiometric proportion, Jiang Geyuan
The nitrate of element (La, Sr, Fe) joins in water (100ml), after fully dissolving, slowly to mixed
Close and liquid add ammoniacal liquor, to be precipitated completely after, by precipitation filtration and in high temperature furnace, 1000 DEG C of roasting 2h.
Coprecipitation is used to prepare La0.8Sr0.2MnO3+d, by La0.8Sr0.2MnO3+dStoichiometric proportion, Jiang Geyuan
The nitrate of (La, Sr, Mn) of element joins in water (100ml), after fully dissolving, slowly to
Mixed liquor adds ammoniacal liquor, to be precipitated completely after, by precipitation filtration and in high temperature furnace, 1100 DEG C of roasting 2h.
By La0.6Sr0.4FeO3-δPowder (0.9g) and La0.8Sr0.2MnO3+dAfter the grinding of powder (0.1g) mechanical mixture again
Mix with some organic bonds (n-butanol, 1g), obtain cathode slurry.Coating 0.012g cathode slurry (face
Long-pending: 0.5cm2) on the interlayer of the battery component of anode support type, at 1050 DEG C of roasting 3h.Control
La0.8Sr0.2MnO3+dContent in composite cathode is respectively 10%(by weight percentage), obtain battery
It is denoted as LSF64-LSM10.
In addition to cathode material, the same comparative example of other assembly of battery, the most same comparative example of battery testing condition.
In anode-side, the hydrogen of humidification is as fuel (volumetric concentration 3%H2O,100ml min-1), at cathode side,
Oxygen is as oxidant (100ml min-1).(0.15A cm under 600 DEG C and constant current density-2),
LSF64-LSM10 cell voltage is respectively 0.91V.Volumetric concentration 2.83%CO is introduced in oxygen stream2With
2.64%H2After O, 48h, LSF64-LSM10 cell voltage have dropped about 0.5%.Negative electrode illustrates very
The stability of good resistant to carbon dioxide.
Embodiment 4
La0.8Sr0.2FeO3-δ-Pr0.8Sr0.2MnO3+dNegative electrode
Citric acid method is used to prepare La0.8Sr0.2FeO3-δ, by La0.8Sr0.2FeO3-δStoichiometric proportion, Jiang Geyuan
The nitrate of element (La, Sr, Fe) joins in water (100ml), after fully dissolving, adds appropriate
Citric acid (citric acid: metal ion=1.5:1), the pH value of regulation mixed liquor is to 6 forerunners obtaining clarification
Solution, colloidal sol, to forming wine-colored colloidal sol, contained in evaporating dish by heating evaporation moisture, and in electric furnace
It is heated to burning, obtains front axle shell.By La0.8Sr0.2FeO3-δFront axle shell, at 1000 DEG C of roasting 2h.Will roasting
La after burning0.8Sr0.2FeO3-δPowder (1g) grinds and mixes with some organic bonds (n-butanol, 1g)
After, it is prepared as cathode slurry.Coating 0.012g cathode slurry (area: 0.5cm2) arrive anode support type
On the interlayer of battery component, at 1050 DEG C of roasting 3h.By Pr0.8Sr0.2MnO3+dStoichiometric proportion, will be each
The nitrate of element (Pr, Sr, Mn) joins in water (100ml), after fully dissolving, adds suitable
Amount citric acid (organic acid: metal ion=1.5:1), the pH=1-2 of regulation mixed liquor.Mixed liquor is impregnated
To La0.8Sr0.2FeO3-δIn, at 900 DEG C, roasting 2h.Control Pr0.8Sr0.2MnO3+dIn composite cathode
Content is respectively 5%(by weight percentage), the battery obtained is denoted as LSF82-PSM5.
In addition to cathode material, the same comparative example of other assembly of battery, the most same comparative example of battery testing condition.
In anode-side, the hydrogen of humidification is as fuel (volumetric concentration 3%H2O,100ml min-1), at cathode side,
Oxygen is as oxidant (100ml min-1).(0.15A cm under 600 DEG C and constant current density-2),
LSF82-PSM5 cell voltage is respectively 0.94V.Volumetric concentration 2.83%CO is introduced in oxygen stream2With
2.64%H2After O, 48h, LSF82-PSM5 cell voltage have dropped about 0.3%.Negative electrode illustrates the best
The stability of resistant to carbon dioxide.
Embodiment 5
La0.8Sr0.2Co0.2Fe0.8O3-δ-Nd0.8Sr0.2MnO3+dNegative electrode
Glycine method is used to prepare La0.8Sr0.2Co0.2Fe0.8O3-δ, by La0.8Sr0.2Co0.2Fe0.8O3-δChemistry meter
Amount ratio, joins the nitrate of each element (La, Sr, Co, Fe) in water (100ml), fully
After dissolving, adding appropriate glycine (glycine: metal ion=1.5:1), the pH value of regulation mixed liquor is extremely
6 precursor aqueous solutions obtaining clarification, colloidal sol, to forming wine-colored colloidal sol, is contained into evaporating dish by heating evaporation moisture
In, and in electric furnace, it is heated to burning, obtain front axle shell.By La0.8Sr0.2Co0.2Fe0.8O3-δFront axle shell,
1000 DEG C of roasting 2h.By the La after roasting0.8Sr0.2Co0.2Fe0.8O3-δPowder (1g) grinds and organic with some
After adhesive (n-butanol, 1g) mixing, it is prepared as cathode slurry.Coating 0.012g cathode slurry (area:
0.5cm2) on the interlayer of the battery component of anode support type, at 1050 DEG C of roasting 3h.Press
Nd0.8Sr0.2MnO3+dStoichiometric proportion, the nitrate of each element (Nd, Sr, Fe) is joined from
In water (100ml), after fully dissolving, add appropriate glycine (glycine: metal ion=1.5:1),
The pH=1-2 of regulation mixed liquor.Mixed liquor is impregnated into La0.8Sr0.2Co0.2Fe0.8O3-δIn, at 900 DEG C, roasting
Burn 2h.Control Nd0.8Sr0.2MnO3+dContent in composite cathode is respectively 5%(by weight percentage),
The battery obtained is denoted as LSCF8228-NSM5.
In addition to cathode material, the same comparative example of other assembly of battery, the most same comparative example of battery testing condition.
In anode-side, the hydrogen of humidification is as fuel (volumetric concentration 3%H2O,100ml min-1), at cathode side,
Oxygen is as oxidant (100ml min-1).(0.15A cm under 600 DEG C and constant current density-2),
LSCF8228-NSM5 cell voltage is respectively 0.92V.Volumetric concentration 2.83%CO is introduced in oxygen stream2
And 2.64%H2After O, 48h, LSCF8228-NSM5 cell voltage have dropped about 0.5%.Negative electrode illustrates
The stability of extraordinary resistant to carbon dioxide.
Claims (4)
1. an intermediate temperature solid oxide fuel cell cathode material for resistant to carbon dioxide, consisting of La1-xSrxCoyFe1-yO3-δ-Ln0.8Sr0.2MnO3+d, wherein, 0.1≤x≤0.5；0≤y≤1；0≤δ≤0.25；
0≤d≤0.05；Ln is one or more in La, Pr, Nd；
By weight percentage, Ln0.8Sr0.2MnO3+dContent in battery cathode material is 5-20%；
Ln0.8Sr0.2MnO3+dParticle is evenly dispersed in La1-xSrxCoyFe1-yO3-δParticle surface.
2. cathode material as claimed in claim 1, it is characterised in that: La1-xSrxCoyFe1-yO3-δ-Ln0.8
Sr0.2MnO3+dRepresent that cathode material is by La1-xSrxCoyFe1-yO3-δAnd Ln0.8Sr0.2MnO3+dPressed powder group
Conjunction forms.
3. the application of cathode material described in a claim 1, it is characterised in that:
Described cathode material is used to prepare cathode material layer on cell interlayer.
4. according to the application of cathode material described in claim 3, it is characterised in that:
Ln in cathode material layer0.8Sr0.2MnO3+dParticle is evenly dispersed in La1-xSrxCoyFe1-yO3-δParticle table
Face.
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| CN109742414A (en) * | 2019-01-09 | 2019-05-10 | 渤海大学 | A kind of intermediate temperature solid oxide fuel cell cathode material and the preparation method and application thereof |
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| Development of La0.6Sr0.4Co0.2Fe0.8O3Ld cathode with an improved stability via La0.8Sr0.2MnO3-film impregnation;Xingbao Zhu etal;《international journal of hydrogen energy》;20130317;第5375-5382页 * |
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