CN105895942A - Novel LSC catalyzed BCFZ negative electrode and preparation method thereof - Google Patents
Novel LSC catalyzed BCFZ negative electrode and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M8/10—Fuel cells with solid electrolytes
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/90—Selection of catalytic material
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- 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
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Abstract
The invention discloses a novel LSC catalyzed BaCo<0.4>Fe<0.4>Zr<0.2>O<3-Delta> negative electrode of a solid oxide fuel cell and a preparation method of the negative electrode. LSC is a novel La<1-x>Sr<x>CoO<3-Delta> catalyst, the polarization resistance of the BaCo<0.4>Fe<0.4>Zr<0.2>O<3-Delta> negative electrode of the solid oxide fuel cell, the polarization resistance is reduced by 62% when the BaCo<0.4>Fe<0.4>Zr<0.2>O<3-Delta> negative electrode is in a condition of a running temperature of 650 DEG C, and the degradation rate is reduced by two times.
Description
Technical field
The invention belongs to cell art, be specifically related to a kind of SOFC and protonic ceramic combustion
Material cell cathode catalyst and the preparation method of catalytic cathode.
Background technology
SOFC (SOFC) and protonic ceramic fuel cell (PCFC) are so far
One of energy conversion efficiency generation technology the highest, environmental protection, is also following most to be hopeful to replace thermal power generation
One of new technology of centralised or decentralised formula generating.Along with new material and the research of anode supported cells structure, fuel
The running temperature of battery drops to 600-800 DEG C from 800-1000 DEG C, and up-to-date research focus concentrates on
Running temperature is the low-temperature fuel cell of 450-650 DEG C.
The principal element of decision solid-oxide fuel battery performance and running temperature is electrolyte and negative electrode
Material, wherein the polarization resistance of negative electrode accounts for more than the 60% of battery drag overall.BCFZ negative electrode have one excellent
Different power density (150mW/cm2, 600 DEG C), be all middle low-temperature fuel cell cathode materials have most latent
One of material of power.
The present invention passes through BCFZ cathode dipping LSC nano particle, forms three-phase reduction at cathode particle surface
District, increases active reduction area, promotes the reduction of oxygen, improves hydrogen reduction speed, effectively reduces BCFZ
The polarization resistance of negative electrode and running temperature.
Summary of the invention
It is an object of the invention to provide the cathode catalysis of a kind of SOFC and proton fuel cell
Agent and the preparation method of catalytic cathode, solid oxidation prepared by the method current current material of solution and prior art
The problem that in thing fuel cell operation, running temperature is high and deterioration velocity is fast.Gained solid oxidation in the present invention
Thing fuel battery negative pole, compared with pure BCFZ negative electrode, LSC nanoparticle structure has high reduced nano effect
Answering and oxygen reduction activity, the BCFZ cathode surface of LSC dipping forms a kind of nanometer film and nano particle, effectively
Adding three-phase reaction interface and more reaction active site, the catalysis activity of LSC is high, and running temperature reduces,
The strongest to the reproducibility catalytic capability of BCFZ.The LSC that the method for the present invention prepares is catalyzed BCFZ negative electrode,
Its polarization resistance reduces by 62% than BCFZ negative electrode under the conditions of 650 DEG C, when running temperature is less than 650 DEG C,
Polarization resistance reduces by more than 62% than BCFZ, and negative electrode degradation ratio reduces than BCFZ negative electrode under the conditions of 650 DEG C
2 times, when the operating temperature less than 650 DEG C, degradation ratio can reduce by more than 2 times.
For realizing the purpose of the present invention, it is provided that following embodiment.
Term: BCFZ negative electrode represents by BaCo0.4Fe0.4Zr0.2O3-δThe cell cathode that material is made.
LSC catalyst represents by chemical formula La1-xSrxCoO3-δThe cell cathode catalyst of composition, BCFZ is cloudy
Pole surface impregnation (absorption) LSC catalyst is also referred to as cell catalyst negative electrode or LSC is catalyzed BCFZ negative electrode.
In one embodiment, the present invention provides a kind of cathode of solid oxide fuel cell LSC catalyst,
For La1-xSrxCoO3-δShown compound (being called for short LSC) is called for short, and wherein, X represents 0 < x < 1.
In another embodiment, the present invention provides one to prepare cathode of solid oxide fuel cell LSC to urge
The preparation method of agent, comprises the following steps:
1) by nitrate La (NO3)3·6H2O、Sr(NO3)2·6H2O and Co (NO3)2·6H2O joins shape in solvent
Becoming reaction system, add complexing agent citric acid, at room temperature, stirring makes nitrate dissolve, complexing;
2) solution after complexing is placed on electric hot plate heating, makes solution evaporate and burn, it is thus achieved that atrament warp
Grind and be put in batch-type furnace 600 DEG C after alms bowl grinds and calcine 2 hours, obtain chemical formula La1-xSrxCoO3-δCatalysis
Agent.
The method of the invention described above, step 1) described in solvent be absolute ethyl alcohol;Citric acid with
La(NO3)3·6H2O、Sr(NO3)2·6H2O and Co (NO3)2·6H2The metallic atom of all nitrate in O
Molecule mol ratio is 1:1, La (NO3)3·6H2O、Sr(NO3)2·6H2O and Co (NO3)2·6H2The rate of charge of O
According to La1-xSrxCoO3-δThe stoichiometric proportion of chemical formula calculates.
On the other hand, present invention also offers one and prepare SOFC LSC catalysis BCFZ
The method of negative electrode, comprises the following steps:
1) according to chemical formula La1-xSrxCoO3-δStoichiometric proportion configuration nitrate La (NO3)3·6H2O、
Sr(NO3)2·6H2O and Co (NO3)2·6H2The ethanol solution reaction system of O, the wherein scope of x in chemical formula
It is 0 < x < 1, adds complexing agent citric acid;
2) it is stirred at room temperature, makes nitrate be completely dissolved, be complexed, obtain LSC ethanol solution;
3) the LSC ethanol solution after complexing is impregnated in the hole of porous BCFZ negative electrode several times, is subsequently placed in
Calcine 2 hours under conditions of 800 DEG C, obtain the BCFZ negative electrode of LSC catalysis.
The method preparing LSC catalysis BCFZ negative electrode of the invention described above, described ethanol is absolute ethyl alcohol, lemon
Lemon acid with the concentration that mol ratio is 1:1, LSC solution of the metallic atom of all nitrate in reaction system is
0.15-0.25M;Step 3) in LSC dipping total amount be 1.3-1.9 μ L/mm2;Step 3) in leaching several times
Stain process has impregnated for 2 times for dividing, every time after dipping, and pre-burning 1-2 hour at 400 DEG C;LSC is immersed in
BCFZ particle surface forms a kind of nanometer film and nano particle.
The method of the preparation catalysis BCFZ negative electrode of the invention described above, described BCFZ negative electrode is to pass through silk process
Or prepared by the tape casting, and burn 2 hours under the conditions of air atmosphere under the conditions of 900-1100 DEG C, the hole of BCFZ
Gap rate is 20-40%.
The method of the invention described above, described LSC catalyst is a kind of Perovskite Phase structure.
The method preparing LSC catalysis BCFZ negative electrode of the invention described above, prepared LSC catalysis BCFZ is cloudy
Pole, its polarization resistance reduces by 62% than BCFZ negative electrode under the conditions of 650 DEG C, in running temperature less than 650 DEG C
Time, polarization resistance reduces by more than 62% than BCFZ, and negative electrode degradation ratio is ratio BCFZ negative electrode under the conditions of 650 DEG C
Reducing by 2 times, when the operating temperature less than 650 DEG C, degradation ratio can reduce by more than 2.0 times.
Present invention also offers a kind of SOFC BCFZ negative electrode containing LSC catalyst i.e.
SOFC LSC is catalyzed BCFZ negative electrode.
Present invention also offers a kind of SOFC, the BCFZ negative electrode containing LSC catalyst
(i.e. LSC is catalyzed BCFZ negative electrode).
A kind of SOFC of the present invention, is catalyzed BCFZ negative electrode, wherein LSC containing LSC
It is to be impregnated into BCFZ cathode particle surface one nanometer film and nano particle.
In a particular embodiment, the catalyst of a kind of SOFC BCFZ negative electrode of the present invention
La1-xSrxCoO3-δPreparation method, LSC catalyst realizes according to the following steps: one, according to chemical formula
La1-xSrxCoO3-δ, configure nitrate La (NO according to stoichiometric proportion3)3·6H2O、Sr(NO3)2·6H2O and
Co(NO3)2·6H2The ethanol solution of O, wherein in chemical formula x in the range of: 0 < x < 1, according to metal
Atom: citric acid molecule mol ratio is that the ratio of 1:1 adds citric acid;Two, at room temperature, by nitrate second
Alcoholic solution electromagnetic agitation 2 hours, makes nitrate be completely dissolved, is complexed;Three, the solution being complexed is placed
Electric hot plate heats, makes solution evaporate and burn, it is thus achieved that the ground alms bowl of atrament is put in batch-type furnace after grinding
In 800 DEG C burn 2 hours.
BCFZ catalytic cathode realizes according to the following steps: one, according to chemical formula La1-xSrxCoO3-δ, according to chemistry
Metering is than configuration nitrate La (NO3)3·6H2O、Sr(NO3)2·6H2O and Co (NO3)2·6H2The ethanol of O is molten
Liquid, wherein in chemical formula, x is in the range of 0 < x < 1, according to the metallic atom (La+Sr+Co) of nitrate: lemon
Lemon acid molecule mol ratio is that the ratio of 1:1 adds citric acid;Two, at room temperature, ethanolic nitrate solution is used
Electromagnetic agitation 2 hours, makes nitrate be completely dissolved, is complexed;Three, 2 times are divided by the LSC solution after complexing
Perfusion (dipping) is in the hole of porous BCFZ negative electrode, and after impregnating, at 400 DEG C, pre-burning 1-2 is little every time
Time, calcine 2 hours under conditions of being subsequently placed in 800 DEG C, after taking-up, both obtained the soild oxide combustion of LSC catalysis
Material battery BCFZ negative electrode.
Beneficial effect
The LSC catalyst of the SOFC BCFZ negative electrode that the present invention provides and LSC catalysis
The preparation method of BCFZ negative electrode.The catalytic cathode of this catalyst and the method gained is for reducing soild oxide
The running temperature of fuel cell and cost provide a kind of important solution.Can effectively reduce soild oxide
The polarization resistance of fuel battery negative pole and running temperature, reduce the cost of electricity-generating of SOFC.System
Uniform for catalysis BCFZ cathode construction, composition and the thickness gone out, there is good stability and repeatability.
Catalyst according to a kind of SOFC BCFZ negative electrode provided by the present invention
La1-xSrxCoO3-δThe BCFZ catalytic cathode that preparation method obtains, has excellent chemical property and relatively low
Degradation ratio.
Comparing compared with BCFZ negative electrode, the present invention uses dipping LSC method catalytic activation negative electrode, can obtain electricity
The catalytic cathode that chemical property is excellent.The LSC of the present invention is catalyzed BCFZ negative electrode, relative to uncatalyzed BCFZ
Negative electrode, polarization resistance reduces by 62% when 650 DEG C, and when less than 650 DEG C, it is possible to decrease more than 62%.Should
Result effectively reduces the running temperature of battery, to promoting the research of intermediate temperature solid oxide fuel cell and wide
General application has great importance.
In sum, gained LSC of the present invention catalysis BCFZ negative electrode can be applicable to low-temperature solid oxidation in preparation
The negative electrode of thing fuel cell, especially in positive electrode support solid oxidized fuel cell field, reduces fuel cell
Running temperature has bigger meaning, brings huge economic benefit to society.
Accompanying drawing explanation
Fig. 1 shows the BCFZ negative electrode pattern with LSC dipping.
Fig. 2 shows the chemical property of the BCFZ cathode half-cell with LSC dipping.
Detailed description of the invention
Embodiment 1 catalyst La1-xSrxCoO3-δ(LSC) and LSC catalysis BCFZ negative electrode preparation, wherein X=0.1
Preparation method realizes according to the following steps:
1) first according to the chemical formula La of impregnation of matters1-xSrxCoO3-δ(LSC), configure according to stoichiometric proportion
Nitrate La (NO3)3·6H2O、Sr(NO3)2·6H2O and Co (NO3)2·6H2The ethanol solution of O, Qi Zhonghua
In formula, x is 0.1, according to metallic atom (La+Sr+Co): material ratio (mol ratio) of citric acid molecule is
The ratio of 1:1 adds citric acid;
2) at room temperature, by ethanolic nitrate solution electromagnetic agitation 2 hours, make nitrate be completely dissolved,
Complexing, obtains LSC catalyst or referred to as LSC ethanol solution;
3) BCFZ slurry silk process is coated on electrolyte, is painted with and is placed on the drying of sample insulating box, instead
Multiple 4 times, it is subsequently placed in batch-type furnace and burns 2 hours in 900-1100 DEG C, obtain BCFZ negative electrode;
4) by step 2) complexing after LSC ethanol solution irrigate at twice (dipping) to porous BCFZ the moon
In the hole of pole, impregnate every time after at 400 DEG C elder generation's pre-burning 1-2 hour, make LSC be impregnated into BCFZ
On particle, total pickup is 1.35 μ L/mm2, calcine 2 hours under conditions of being subsequently placed in 800 DEG C, after taking-up
Both SOFC BCFZ negative electrode (the i.e. SOFC LSC of LSC catalysis had been obtained
Catalysis BCFZ negative electrode).
Embodiment 2 catalyst La1-xSrxCoO3-δ(LSC) and LSC catalysis BCFZ negative electrode preparation, wherein X=0.9.
Preparation method is same as in Example 1, is chemical formula La with embodiment difference1-xSrxCoO3-δ's
X is 0.9, and the configuration of nitrate matches with this chemical formula, step 4) in LSC pickup be
1.8μL/mm2, other steps are identical with tool embodiment 1 with parameter.
Embodiment 3 catalyst La1-xSrxCoO3-δ(LSC) and LSC catalysis BCFZ negative electrode preparation, wherein X=0.4.
Preparation method is same as in Example 1, and difference from Example 1 is chemical formula La1-xSrxCoO3-δX
Being 0.4, the configuration of nitrate matches with this chemical formula, step 4) in LSC pickup be 1.8 μ L/mm2,
Other steps are identical with tool embodiment 1 with parameter.
The preparation of embodiment 4LSC catalyst
Preparation technology comprises the following steps:
1) according to La1-xSrxCoO3-δThe stoichiometric proportion of chemical formula calculates consumption and the throwing of following nitrate
Expect ratio (being can to calculate and obtain according to the knowledge of this area), by nitrate La (NO3)3·6H2O、
Sr(NO3)2·6H2O and Co (NO3)2·6H2O joins formation reaction system in absolute ethyl alcohol, then presses nitrate
The mol ratio of all metallic atoms (i.e. La+Sr+Co) and citric acid be that 1:1 adds complexing agent citric acid,
At room temperature, stirring makes nitrate dissolve, complex reaction, obtains LSC ethanol solution.
2) the LSC ethanol solution after complexing is placed on electric hot plate heating, makes solution evaporate and burn, obtaining
The ground alms bowl of atrament grind after be put in batch-type furnace 800 DEG C and calcine 2 hours, obtain chemical formula
La1-xSrxCoO3-δCatalyst.
The preparation of embodiment 5BCFZ cathode slurry
1) BCFZ cathode slurry is prepared, according to chemical formula BaCo0.4Fe0.4Zr0.2O3-δStoichiometric proportion, join
Put Ba (NO3)2、Co(NO3)2·6H2O、Fe(NO3)3·9H2O and Zr (NO3)4·5H2O ethanolic nitrate solution
Reaction system;It is stirred at room temperature, makes nitrate be completely dissolved, be complexed, obtain BCFZ ethanol solution;
2) solution after complexing is placed on electric hot plate heating, makes solution evaporate and burn, it is thus achieved that atrament warp
Being put in batch-type furnace 600 DEG C after grinding to calcine 2 hours, obtaining chemical formula is BaCo0.4Fe0.4Zr0.2O3-δBCFZ
Powder.
3) 1:2.5 the most in mass ratio weighs and takes BCFZ powder and V006, and ground alms bowl grinds, mixes and get final product
BCFZ cathode slurry.
Embodiment 1-3 is obtained LSC catalysis BCFZ negative electrode and is arranged on SOFC, obtain
SOFC containing LSC catalysis BCFZ negative electrode.Survey through this area traditional test methods
Examination, obtains following result: the LSC of embodiment 1-3 is catalyzed BCFZ negative electrode, and its polarization resistance is at 650 DEG C of bars
62% is reduced than the BCFZ negative electrode not being catalyzed by LSC under part, when running temperature is less than 650 DEG C, polarization electricity
Resistance reduces by more than 62% than the BCFZ that is not catalyzed by LSC, negative electrode degradation ratio under the conditions of 650 DEG C than not by
The BCFZ negative electrode of LSC catalysis reduces by 2 times, and when the operating temperature less than 650 DEG C, degradation ratio can reduce by 2
More than Bei.
Pass through flexible under the Spirit Essence of the present invention or simply modify, under conditions of not changing essence of the present invention
Fall within the scope of the present invention.
Claims (16)
1. a cathode of solid oxide fuel cell catalyst is La1-xSrxCoO3-δ(LSC) compound shown in, its
In, X represents 0 < x < 1.
2. the method preparing catalyst described in claim 1, comprises the following steps:
1) by nitrate La (NO3)3·6H2O、Sr(NO3)2·6H2O and Co (NO3)2·6H2O joins shape in solvent
Becoming reaction system, add complexing agent citric acid, at room temperature, stirring makes nitrate dissolve, complexing;
2) solution after complexing is placed on electric hot plate heating, makes solution evaporate and burn, it is thus achieved that atrament warp
It is put in batch-type furnace 800 DEG C after grinding to calcine 2 hours, obtains chemical formula La1-xSrxCoO3-δCatalyst.
3. method as claimed in claim 2, step 1) described in solvent be absolute ethyl alcohol.
4. method as claimed in claim 2, citric acid and La (NO3)3·6H2O、Sr(NO3)2·6H2O and
Co(NO3)2·6H2The molecule mol ratio of all metallic atoms in O is 1:1.
5. the method preparing SOFC BCFZ negative electrode, comprises the following steps:
1) BCFZ cathode slurry is prepared, according to chemical formula BaCo0.4Fe0.4Zr0.2O3-δStoichiometric proportion, configuration
Ba(NO3)2、Co(NO3)2·6H2O、Fe(NO3)3·9H2O and Zr (NO3)4·5H2O ethanolic nitrate solution reaction
System;It is stirred at room temperature, makes nitrate be completely dissolved, be complexed, obtain BCFZ ethanol solution;
2) solution after complexing is placed on electric hot plate heating, makes solution evaporate and burn, it is thus achieved that atrament warp
Being put in batch-type furnace 600 DEG C after grinding to calcine 2 hours, obtaining chemical formula is BaCo0.4Fe0.4Zr0.2O3-δBCFZ
Powder.
6. method as claimed in claim 5, step 1) described in solvent be absolute ethyl alcohol.
7. method as claimed in claim 5, citric acid and Ba (NO3)2、Co(NO3)2·6H2O、Fe(NO3)3·9H2O
With Zr (NO3)4·5H2The molecule mol ratio of all metallic atoms in O is 1:1.
8. prepare a preparation method for the BCFZ negative electrode of fuel cell LSC catalysis, comprise the following steps:
1) configuration cathode filament wire mark slurry, 1:2.5 the most in mass ratio weighs and takes BCFZ and V006, ground alms bowl
Grind, mixing, prepare negative electrode by silk process, be put in subsequently in baking oven and be dried, in batch-type furnace 950-1100 DEG C
Burning 2 hours, the porosity of BCFZ negative electrode is 20-40%;
2) according to chemical formula La1-xSrxCoO3-δStoichiometric proportion configuration La (NO3)3·6H2O、Sr(NO3)2·6H2O
With Co (NO3)2·6H2The ethanolic nitrate solution reaction system of O, wherein in chemical formula x in the range of 0 < x < 1,
Add complexing agent citric acid;
3) it is stirred at room temperature, makes nitrate be completely dissolved, be complexed, obtain LSC ethanol solution;
4) the LSC ethanol solution after complexing is impregnated in the hole of porous BCFZ negative electrode several times, has impregnated every time
After one-tenth at 400 DEG C first pre-burning 1-2 hour, calcine 2 hours under conditions of being subsequently placed in 800 DEG C, obtain LSC
The BCFZ negative electrode of catalysis.
9. method as claimed in claim 8, described ethanol is absolute ethyl alcohol, citric acid and metal in reaction system
The mol ratio of atom be the concentration of 1:1, LSC solution be 0.15-0.25M.
10. method as claimed in claim 8, step 3) in LSC dipping total amount be 1.3-1.9 μ L/mm2。
11. methods as claimed in claim 8, step 3) in described dipping several times be point 2 dippings, often
After secondary dipping is complete, pre-burning 1-2 hour at 400 DEG C.
12. methods as claimed in claim 8, described LSC is a Perovskite Phase structure.
13. methods as claimed in claim 8, it is characterised in that LSC is immersed in BCFZ particle surface and forms one
Nanometer film and nano particle.
14. methods as claimed in claim 8, it is characterised in that LSC catalysis BCFZ negative electrode polarization resistance exist
Reducing by 62% than BCFZ negative electrode under the conditions of 650 DEG C, when running temperature is less than 650 DEG C, polarization resistance compares BCFZ
Reduce by more than 62%.
15. methods as claimed in claim 8, it is characterised in that the negative electrode degradation ratio of LSC catalysis BCFZ negative electrode exists
Reducing by 2 times than BCFZ negative electrode under the conditions of 650 DEG C, when the operating temperature less than 650 DEG C, degradation ratio can reduce
More than 2 times.
16. 1 kinds of SOFCs, the LSC prepared containing claim 8 is catalyzed BCFZ negative electrode.
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CN114744214A (en) * | 2022-02-21 | 2022-07-12 | 南京工业大学 | Triple-conductivity perovskite oxide, preparation method and application |
KR102678883B1 (en) * | 2018-08-09 | 2024-06-26 | 주식회사 엘지화학 | Cathode composition for solid oxide fuel cell, cathode, manufacturing method thereof and solid oxide fuel cell |
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