CN103887520A - Method for preparing solid oxide fuel cell composite cathode through low-temperature sintering - Google Patents
Method for preparing solid oxide fuel cell composite cathode through low-temperature sintering Download PDFInfo
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- CN103887520A CN103887520A CN201210566367.0A CN201210566367A CN103887520A CN 103887520 A CN103887520 A CN 103887520A CN 201210566367 A CN201210566367 A CN 201210566367A CN 103887520 A CN103887520 A CN 103887520A
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- cathode
- perovskite
- composite cathode
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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
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
- H01M4/8885—Sintering or firing
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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
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/881—Electrolytic membranes
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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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
-
- 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
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
- H01M4/8885—Sintering or firing
- H01M4/8889—Cosintering or cofiring of a catalytic active layer with another type of layer
-
- 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
The invention provides a method for preparing a solid oxide fuel cell composite cathode through low-temperature sintering. The method comprises: employing a composite cathode material primary powder synthesized by employing an ammonium citrate process to prepare a slurry, coating an anode electrolyte two-in-one assembly, and sintering at a low temperature of 900-1000 DEG C for preparing the cell cathode. The composite cathode possesses perovskite phase and cubic fluorite phase at the same time, and is a mixed ionic electronic conductor. Particle size is uniform, specific surface area is large, many three-phase interfaces as electrochemical active sites exists and are uniformly distributed in the whole cathode body, cell performances are higher than those of a conventional mechanically mixed cathode, and a cell can stably run.
Description
Technical field
The present invention relates to compound cathode of solid oxide fuel battery, specifically a kind of low-temperature sintering is prepared the method for sending out of compound cathode of solid oxide fuel battery.
Background technology
Solid Oxide Fuel Cell is a kind of energy conversion device that chemical energy in fuel is converted into electric energy.A typical Solid Oxide Fuel Cell comprises anode, electrolyte and negative electrode three parts.For the anode-supported hull cell mainly adopting now, cathodic polarization loss is the principal element of restriction battery performance.At negative electrode, be mainly the electro-reduction process of oxygen, comprise that the oxygen in gas phase is diffused into cathode surface by mesopore, adsorb thereon, dissociate, and accept electron conduction and transmit mutually the electronics coming and change into oxonium ion and enter the several processes of electrolyte lattice.And said process is except gas diffusion, all need very high reaction activation, reaction rate slow (X.J.Chen et al./Journal of Power Sources123 (2003) 17 – 25), the polarization loss producing is high, thereby becomes the principal element of restriction solid-oxide fuel battery performance.Therefore study the negative electrode of high-performance and long-time stability, the method for developing new cathode material or new sintered cathode just seems particularly important.
And the acquisition of conventional composite negative electrode is the method by mechanical mixture, exist and mix uneven problem, and material to pass through powder and twice high temperature sintering of electrode (>=1100 ° of C), particle is grown up comparatively serious, specific surface and three phase boundary loss are seriously.Therefore this patent proposes a kind of simple and effective method of preparing compound cathode of solid oxide fuel battery, prepared negative electrode has Perovskite Phase and cubic fluorite phase simultaneously, and only need the low-temperature sintering of once≤1000 ° of C, granular size is equal, contact well with electrolyte interface, battery performance is higher.
Summary of the invention
The present invention proposes a kind of method that low-temperature sintering is prepared compound cathode of solid oxide fuel battery.
Low-temperature sintering is prepared a method for compound cathode of solid oxide fuel battery, specifically comprises the following steps,
1) first prepare needed powder: take the nitrate of stoichiometric proportion, add appropriate amount of deionized water, stir it is dissolved completely; Add wherein reaction reagent, reaction reagent and GOLD FROM PLATING SOLUTION belong to mol ratio >=0.5 of ion, and regulation system pH dissolves reaction reagent completely, and heating evaporation moisture obtains after vitreosol, move to heating on heating furnace and make it that self-propagating combustion occur, collect the first powder of gained;
2) by gained just powder in agate mortar, add absolute ethyl alcohol and be ground to system and be ink-like;
3) by after the powder drying after grinding, add 711 glue to be uniformly mixed to obtain cathode slurry;
4) gained cathode slurry is coated in the two-in-one substrate of anode, 900 ~ 1000 ° of C sintering 2 ~ 5h of low temperature, obtain composite cathode.This composite cathode has Perovskite Phase and cubic fluorite phase simultaneously, without other dephasign; Be hybrid ionic electronic conductor, particle is thin and evenly, specific area is large, and three phase boundary is many and be uniformly distributed in whole composite cathode body phase, is conducive to improve battery performance.
The method is applicable to prepare the zirconio material of Perovskite Phase and cubic fluorite phase or the composite cathode of cerium sill, and wherein the general formula of Perovskite Phase is (La
1-xz
x)
a(M
1-yn
y) O
3 ± d, wherein Z is that doping occupies Ca or the Sr element of perovskite A position, M, N occupy perovskite B position and are selected from one or two or more kinds in the element of Cr, Mn, Fe, Co, Ni, Cu, and the value of a is 0.8 ~ 1, and preferably 0.9 ~ 0.95; The value of x is 0 ~ 0.5, preferably 0.1 ~ 0.2; The value of y is 0 ~ 0.4,0≤d≤0.1764;
Fluorite is YSZ (Y mutually
2o
3stable ZrO
2), GDC (Gd
2o
3stable CeO
2), LDC (La
2o
3stable CeO
2), SDC (Sm
2o
3stable CeO
2) in one or two or more kinds.
The synthetic required raw material of composite cathode comprises the synthetic Perovskite Phase raw material mutually used with fluorite, Perovskite Phase raw material used are the above nitrate of two kinds in metallic element in perovskite, fluorite raw material mutually used be in the nitrate of Y, La, Zr, Gd, Sm, Ce more than two kinds;
The general formula of described perovskite is (La
1-xz
x)
a(M
1-yn
y) O
3 ± d, wherein Z is that doping occupies Ca or the Sr element of perovskite A, M, N occupy perovskite B position and are selected from one or two or more kinds in the element of Cr, Mn, Fe, Co, Ni, Cu, and the value of a is 0.8 ~ 1; The value of x is 0 ~ 0.5; The value of y is 0 ~ 0.4; 0≤d≤0.1764;
Described fluorite is the zirconia of YSZ(stabilized with yttrium oxide mutually); The cerium oxide of GDC(gadolinium oxide doping), the cerium oxide of LDC(lanthanum oxide doping), the cerium oxide of SDC(samarium oxide doping) in one or two or more kinds.
Perovskite is 40%:60% ~ 70%:30% with the mass ratio of fluorite phase, preferably 50%:50%, 55%:45%, 60%:40%, 65%:35%, 70%:30%.
Reaction reagent is the one in Triammonium citrate, EDTA+ citric acid, glycine, urea, optimization citric acid three ammoniums or glycine, and the mol ratio of the metal ion sum in reaction reagent and synthetic composite cathode needed raw material is generally 1.2 ~ 1.5.
Sintering temperature is 900 ~ 1000 ° of C, preferably 950 ° of C, and the programming rate of low temperature≤400 ° C is less than 1 ° of C/min.
Beneficial effect of the present invention:
The present invention adopts a low-temperature sintering to obtain perovskite fluorite composite cathode, and the particle that while having avoided conventional cathode to prepare, powder and twice high temperature sintering of cell cathode cause is grown up and the minimizing of three phase boundary electrochemical site.And the composite cathode average grain diameter of preparation only has tens nanometers; There is different size hole, be conducive to the diffusion of gas; Specific area is large, reaches 12.833m
2/ g; Two-phase interface contact is good, and three phase boundary is dispersed throughout whole cathode phase, and hydrogen reduction active sites increases greatly, and performance is increased to 1.957 ~ 2.194 times of traditional mechanical mixture negative electrode.
Brief description of the drawings
Fig. 1 is the (La that adopts ammonium citrate method to synthesize together
0.8sr
0.2)
0.9mnO
3 ± dxRD collection of illustrative plates after the first powder of composite cathode material and the 950 ° of C roasting 3h of/YSZ=60:40wt%.
Fig. 2 is the (La that adopts glycine method synthetic
0.8sr
0.2)
0.9mnO
3 ± dthe composite cathode material of/YSZ=60:40wt% is the SEM photo of powder just.
Fig. 3 is the (La that adopts glycine method synthetic
0.8sr
0.2)
0.9mnO
3 ± dthe composite cathode material of/YSZ=60:40wt% just powder with after 950 ° of C roasting 3h of sintering temperature identical with electrode, the SEM photo of powder
Fig. 4 is the (La that adopts ammonium citrate method synthetic
0.8sr
0.2)
0.9mnO
3 ± d/ YSZ just powder is made into slurry, and low-temperature sintering becomes after cell cathode, Au afflux, the cell I-V curve of 800 ° of C tests and the comparison of traditional mechanical mixture composite cathode LSM afflux battery.Wherein (La
0.8sr
0.2)
0.9mnO
3 ± d/ YSZ=55:45,60:40,65:35,70:30wt%.
The real formula of concrete enforcement
Embodiment 1
Adopt the synthetic (La of Triammonium citrate method
0.8sr
0.2)
0.9mnO
3 ± d– YSZ=60:40wt%, composite cathode material, wherein (La
0.8sr
0.2)
0.9mnO
3+dfor 0.02mol, take 6.2361g La (NO
3)
36H
2o(analyzes pure), 0.7657g Sr (NO
3)
2(analyzing pure), 7.158g Mn (NO
3)
2(analyzing pure 50wt% solution), 8.7686gZr (NO
3)
45H
2o (analyzing pure), 1.3560g Y (NO
3)
36H
2o (analyzing pure), be dissolved in completely in 100ml deionized water, after according to Triammonium citrate: metal ion total mole number=1:1.2(mol ratio) ratio add 19.0406g Triammonium citrate (analyzing pure), and to reconcile the pH value of mixed liquor with nitric acid be 1 it to be dissolved completely, then heating makes to react in solution system, and transpiring moisture, solution becomes sticky thick gradually, be after vitreosol and move on heating furnace and heat, make it that self-propagating combustion occur, collect gained first powder, and at the beginning of getting part, powder adopts the heating schedule roasting (with sintering procedure in embodiment 3) identical with electrode, adopt XRD to characterize this two kinds of powders, Fig. 1 is the XRD spectra of gained.
Embodiment 2
Adopt glycine method synthetic (La together
0.8sr
0.2)
0.9mnO
3 ± d– YSZ=60:40wt% composite material, wherein (La
0.8sr
0.2)
0.9mnO
3+dfor 0.01mol, take 3.1181g La (NO
3)
36H
2o(analyzes pure), 0.3828gSr (NO
3)
2(analyzing pure), 3.579g Mn (NO
3)
2(analyzing pure 50wt% solution), 4.3804gZr (NO
3)
45H
2o (analyzing pure), 0.6797g Y (NO
3)
36H
2o (analyzing pure), be dissolved in completely in 100ml deionized water, according to glycine: metal ion total mole number=1:2.31(mol ratio) ratio add 3.8267g glycine (analyzing pure), heating complexing transpiring moisture after dissolving completely, solution becomes sticky gradually and moves on heating furnace and heat after thick, make its burning, collect gained first powder, and get just powder employing of the part heating schedule roasting (with sintering procedure in embodiment 3) identical with electrode, its SEM photo is as shown in Figures 2 and 3.
Embodiment 3
As preparation (La in embodiment 1
0.8sr
0.2)
0.9mnO
3 ± d– YSZ(mass ratio)=55:45%, 60:40%, 65:35%, the first powder of 70:30%, adds 711 glue to be made into cathode slurry after grinding evenly, applies 0.0100g two-in-one upper to anodolyte, temperature programming sintering.
Sintering procedure is: room temperature to 400 ° C, heats up by 1 ° of C/min; Be greater than 400 ° of C ~ 800 ° C, heat up by 5 ° of C/min; Be greater than 800 ~ 950 ° of C, heat up by 2 ° of C/min, 950 ° of C insulation 180min; Be down to 400 ° of C by 2 ° of C/min; After cooling with stove.
Cell evaluation carries out on the device of self assembly.Test I-V curve after 800 ° of C polarization 16h.Result as shown in Figure 4.
Claims (10)
1. low-temperature sintering is prepared a method for compound cathode of solid oxide fuel battery, it is characterized in that: specifically comprise the following steps,
1) first prepare needed powder: take the nitrate of metallic element in required Ca-Ti ore type and fluorite oxide according to stoichiometric proportion, add deionized water, stir it is dissolved completely; Add wherein reaction reagent, reaction reagent and GOLD FROM PLATING SOLUTION belong to mol ratio >=0.5 of ion, and regulation system pH dissolves reaction reagent completely, and heating evaporation moisture obtains after vitreosol, move to heating on heating furnace and make it that self-propagating combustion occur, collect the first powder of gained;
2) by gained just powder in agate mortar, add absolute ethyl alcohol and be ground to system and be ink-like;
3) by after the powder drying after grinding, add 711 glue to be uniformly mixed to obtain cathode slurry;
4) gained cathode slurry is coated in the two-in-one substrate of anodolyte or dielectric film substrate, from room temperature temperature programming to 900 ~ 1000 ° C, and in 900 ~ 1000 ° of C heat preservation sintering 2 ~ 5h, obtains composite cathode.
2. method according to claim 1, is characterized in that:
Prepared composite cathode is perovskite/fluorite phase composite cathode;
Wherein the general formula of perovskite is (La
1-xz
x)
a(M
1-yn
y) O
3 ± d, wherein Z is that doping occupies Ca or the Sr element of perovskite A position, M, N occupy perovskite B position and are selected from one or two or more kinds in the element of Cr, Mn, Fe, Co, Ni, Cu, and the value of a is 0.8 ~ 1; The value of x is 0 ~ 0.5; The value of y is 0 ~ 0.4; 0≤d≤0.1764; Fluorite is one or two or more kinds in YSZ, GDC, LDC, SDC mutually.
3. method according to claim 1 and 2, it is characterized in that: the synthetic required raw material of composite cathode material comprises the synthetic Perovskite Phase raw material mutually used with fluorite, Perovskite Phase raw material used are the above nitrate of two kinds in metallic element in perovskite, fluorite raw material mutually used be in the nitrate of Y, La, Zr, Gd, Sm, Ce more than two kinds.
4. method according to claim 2, is characterized in that: described a value preferably 0.9 ~ 0.95; X value preferably 0.1 ~ 0.2.
5. method according to claim 1, is characterized in that: in composite cathode, the mass ratio of perovskite oxide and fluorite phase oxide is 40%:60% ~ 70%:30%.
6. method according to claim 1, is characterized in that: reaction reagent is the one in Triammonium citrate, EDTA+ citric acid, glycine, urea.
7. method according to claim 1, is characterized in that: the mol ratio of the metal ion sum in reaction reagent and synthetic composite cathode material needed raw material preferably 1.2 ~ 1.5.
8. method according to claim 1, is characterized in that: sintering temperature is preferably 950 ° of C;
In composite cathode, the mass ratio of perovskite oxide and fluorite phase oxide is preferably 50%:50%, 55%:45%, 60%:40%, 65%:35%, or 70%:30%;
Reaction reagent is preferably Triammonium citrate or glycine.
9. method according to claim 1, is characterized in that: the heating rate of the low thermophase from room temperature temperature programming to≤400 ° of C is less than or equal to 1 ° of C/min.
10. method according to claim 1, is characterized in that:
In step 1) regulation system pH for be less than or equal to 2 or pH be 6-7;
The 40-100% that in step 1), 711 glue consumptions are powder quality.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104085926A (en) * | 2014-07-18 | 2014-10-08 | 渤海大学 | Preparation method of SLSTON (Sr, La, Sc, Ta, O and N) perovskite-type nitrogen oxide solid solution powder |
| CN105261765A (en) * | 2014-07-17 | 2016-01-20 | 中国科学院大连化学物理研究所 | Method for preparing LSM-YSZ nanocomposite electrode through high temperature phase separation |
| CN105789636A (en) * | 2016-03-22 | 2016-07-20 | 山西师范大学 | Method for one-step hydrothermal synthesis preparation of composite anode material of solid oxide fuel cell |
| CN106876720A (en) * | 2015-12-12 | 2017-06-20 | 中国科学院大连化学物理研究所 | A kind of modified high-temperature solid oxide electrolytic cell composite anode materials of bismuth oxide |
| CN106876755A (en) * | 2015-12-12 | 2017-06-20 | 中国科学院大连化学物理研究所 | A kind of method of low-firing composite cathode on cerium base electrolyte interlayer |
| CN106887631A (en) * | 2015-12-12 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of method for improving perovskite oxide cathodic stability |
| CN108091885A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of high-temperature fuel cell cathode and its application |
| CN108110262A (en) * | 2016-11-25 | 2018-06-01 | 中国科学院大连化学物理研究所 | A kind of method of high-temperature fuel cell cathode modification |
| CN109841845A (en) * | 2017-11-28 | 2019-06-04 | 中国科学院大连化学物理研究所 | A kind of method of LSM-YSZ cathode modification |
| CN114142101A (en) * | 2021-11-29 | 2022-03-04 | 福州大学 | Method for preparing LATP solid electrolyte with blocking electrode at low temperature in one step |
| US11439983B2 (en) * | 2019-03-29 | 2022-09-13 | Johnson Matthey Public Limited Company | Active perovskite-type catalysts stable to high temperature aging for gasoline exhaust gas applications |
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| CN105261765A (en) * | 2014-07-17 | 2016-01-20 | 中国科学院大连化学物理研究所 | Method for preparing LSM-YSZ nanocomposite electrode through high temperature phase separation |
| CN105261765B (en) * | 2014-07-17 | 2017-11-28 | 中国科学院大连化学物理研究所 | A kind of method that high temperature phase separation prepares LSM YSZ nanometer combined electrodes |
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| CN104085926A (en) * | 2014-07-18 | 2014-10-08 | 渤海大学 | Preparation method of SLSTON (Sr, La, Sc, Ta, O and N) perovskite-type nitrogen oxide solid solution powder |
| CN106876755B (en) * | 2015-12-12 | 2019-07-02 | 中国科学院大连化学物理研究所 | A kind of method of low-firing composite cathode on cerium base electrolyte interlayer |
| CN106876720A (en) * | 2015-12-12 | 2017-06-20 | 中国科学院大连化学物理研究所 | A kind of modified high-temperature solid oxide electrolytic cell composite anode materials of bismuth oxide |
| CN106876755A (en) * | 2015-12-12 | 2017-06-20 | 中国科学院大连化学物理研究所 | A kind of method of low-firing composite cathode on cerium base electrolyte interlayer |
| CN106887631A (en) * | 2015-12-12 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of method for improving perovskite oxide cathodic stability |
| CN105789636A (en) * | 2016-03-22 | 2016-07-20 | 山西师范大学 | Method for one-step hydrothermal synthesis preparation of composite anode material of solid oxide fuel cell |
| CN108091885A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of high-temperature fuel cell cathode and its application |
| CN108091885B (en) * | 2016-11-21 | 2020-08-04 | 中国科学院大连化学物理研究所 | High-temperature fuel cell cathode and application thereof |
| CN108110262A (en) * | 2016-11-25 | 2018-06-01 | 中国科学院大连化学物理研究所 | A kind of method of high-temperature fuel cell cathode modification |
| CN109841845A (en) * | 2017-11-28 | 2019-06-04 | 中国科学院大连化学物理研究所 | A kind of method of LSM-YSZ cathode modification |
| US11439983B2 (en) * | 2019-03-29 | 2022-09-13 | Johnson Matthey Public Limited Company | Active perovskite-type catalysts stable to high temperature aging for gasoline exhaust gas applications |
| CN114142101A (en) * | 2021-11-29 | 2022-03-04 | 福州大学 | Method for preparing LATP solid electrolyte with blocking electrode at low temperature in one step |
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