CN108649238A - A kind of Ca-Ti ore type cathode material for solid-oxide fuel cell and preparation method thereof - Google Patents
A kind of Ca-Ti ore type cathode material for solid-oxide fuel cell and preparation method thereof Download PDFInfo
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- CN108649238A CN108649238A CN201810446689.9A CN201810446689A CN108649238A CN 108649238 A CN108649238 A CN 108649238A CN 201810446689 A CN201810446689 A CN 201810446689A CN 108649238 A CN108649238 A CN 108649238A
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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
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M2008/1293—Fuel cells with solid oxide electrolytes
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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
Abstract
The invention discloses a kind of perovskite cathode material for solid-oxide fuel cell and preparation method thereof, and molecular formula is：(Pr0.9La0.1)2‑xNi0.74Cu0.21Al0.05O4+δ(0≤x≤0.15).The purpose of the present invention is develop the cathode material of novel no cobalt-based low thermal coefficient of expansion.By in A (Pr, La) the vacant chemical property for improving material with Cu and Al ionic compartmentations with B (Ni).Present invention obtains the novel cathode materials of a kind of function admirable：Coefficient of thermal expansion matches with common electrolyte material, and this kind of material has good stability and excellent electrochemical catalysis activity, is suitable for the working environment of intermediate temperature solid oxide fuel cell.
Description
Technical field
The present invention relates to the technical fields of solid oxide fuel cell, and in particular to arrives Ca-Ti ore type soild oxide
Fuel battery cathode material and its preparation and application.
Background technology
With economic and society high speed development, the deterioration of the ecological environment is to the sustainable of human society caused by fossil energy
Development is challenged, and exploitation new cleaning fuel is very urgent.Solid oxide fuel cell (Solid oxide fuel
Cells, SOFCs) it is a kind of energy resource system of clean and effective, it is referred to as the green energy resource of 21 century.In recent years, all exist both at home and abroad
SOFC technologies in research under low temperature, battery material play very crucial effect in SOFC evolutions.Studies have shown that cloudy
Pole material is the key component of SOFC, and ohmic loss thereon occupies sizable proportion in the ohmic loss of entire battery,
Therefore the cathode material of exploitation excellent performance develops SOFC significant.
The present invention passes through to (Pr0.9La0.1)2-xNi0.74Cu0.21Al0.05O4+δ(0≤x≤0.15) material (is abbreviated as
PLNCA it) is studied, by A (Pr, La) the vacant electrification for improving material with Cu and Al ionic compartmentations with B (Ni)
Performance is learned, material at high temperature stability is improved.The present invention provides a kind of methods obtaining excellent perovskite cathode material, obtain
The novel cathode material of a kind of function admirable provides Research Thinking for exploitation dependency structure cathode material.
Invention content
A Pr and La are proportionally carried out omission by the present invention, while B Ni ions being taken with part Cu and Al ion
In generation, obtain that a kind of electric conductivity is excellent and the active high sofc cathode material of electrochemical catalysis.
The present invention is to prepare perovskite sofc cathode material with sol-gal process.
The specific technical solution of the present invention is：A kind of perovskite sofc cathode material, composition general formula are
(Pr0.9La0.1)2-xNi0.74Cu0.21Al0.05O4+δThe best materials chemistry formula of (0≤x≤0.15) performance is (Pr0.9La0.1)2Ni0.74Cu0.21Al0.05O4+δ.
The perovskite cathode material of the present invention is prepared using sol-gal process, and steps are as follows：
Step 1: weighing：According to the stoichiometric ratio of above-mentioned material, Pr is weighed respectively6O11, Ni (NO3)2·3H2O, Cu
(NO3)2·3H2O, Al (NO3)3·9H2O and La2O3, according to metal ion: EDTA: citric acid=1: 1: 2, weigh EDTA and lemon
Lemon acid；
Step 2: preparing colloidal sol：By Ni (NO3)2·3H2O, Cu (NO3)2·3H2O, Al (NO3)3·9H2O pours into large beaker
In, then by Pr6O11It pours into small measuring cup, nitric acid is added stirs to solution and clarify, then by La2O3It pours into another small measuring cup,
It adds nitric acid to stir to solution clarification, finally the nitrate solution in two small measuring cups is poured into large beaker, opens magnetic force
Blender starts that EDTA is added when stirring is clarified to solution without black impurity, and ammonium hydroxide is added and adjusts pH (pH is required 6~8), so
After be added citric acid, then ammonium hydroxide is added to adjust pH to 6~8, until liquid jelly, stop stirring, take out magnon；
Step 3: drying：The colloidal liquid that step 2 obtains is put into bellows, dries 24 hours to glue with 180 DEG C
Object is dried；
Step 4: calcining：After the sample grinding that step 3 is obtained, it is put into Muffle furnace and calcines 10 hours at 600 DEG C, so
Regrinding is taken out afterwards, is calcined again at 1000 DEG C 5 hours, is finally added alcohol grinding again, obtain cathode powder, then choose
A part of tabletted, cylinder.
It will obtain the Ce for being coated in densification of cathode powder symmetrically by silk screen print method0.8Sm0.2O1.9(SDC) it is electrolysed
The both sides of matter piece calcine 2 hours Symmetrical cells obtained for testing impedance at 1000 DEG C.
Anode powder NiO-SDC is coated in the side of SDC by the same method, calcines 4 hours, will obtain at 1250 DEG C
Cathode powder is evenly coated in the other side of SDC electrolyte sheets by silk screen print method, calcines 2 hours, is used at 1000 DEG C
The monocell of measured power.
The disk that step 4 obtains uses the high-temperature conductivity of direct current four-end method test material, the cylinder that step 4 obtains to use
In the coefficient of thermal expansion of test material.
Advantages of the present invention：
The coefficient of thermal expansion that 1. cathode material of the present invention has and common electrolyte matches.
2. with good electric conductivity and higher electrochemical catalysis activity.
Description of the drawings
Fig. 1 is the XRD spectra of the PLNCA samples prepared；
Fig. 2 is PLNCA cathode materials 30 DEG C -1000 DEG C of thermal dilatometry in air atmosphere；
Fig. 3 is that PLNCA cathode materials vary with temperature curve in 100 DEG C -800 DEG C of conductivity；
Fig. 4 is PLNCA in the interfacial polarization impedance using SDC as the Symmetrical cells of electrolyte at different temperatures；
Fig. 5 is PLNCA using SDC as electrolyte, and NiO-SDC is the monocell output performance of anode.
Specific implementation mode
Embodiment 1：(Pr0.9La0.1)2Ni0.74Cu0.21Al0.05O4+δThe preparation of cathode, is thermally expanded and is surveyed heat stability testing
Examination, conductivity, impedance and cell output test.
According to the stoichiometric ratio of material, Pr is weighed respectively6O11, Ni (NO3)2·3H2O, Cu (NO3)2·3H2O, Al
(NO3)·9H2O and La2O3.First by Ni (NO3)2·3H2O, Cu (NO3)2·3H2O, Al (NO3)3·9H2O pours into large beaker
In, then respectively by Pr6O11And La2O3It is dissolved in nitric acid, obtains nitrate, obtained nitrate solution is also poured into large beaker
In, it opens magnetic stirring apparatus and starts to be mixed.EDTA is then added, ammonium hydroxide is added and adjusts pH (pH is required 6~8), then
Citric acid is added, then ammonium hydroxide is added to adjust pH, pH value is transferred to 6~8, after solution clarification, heating stirring to solution jelly.Finally will
Obtained colloidal liquid is put into bellows, is dried 24 hours with 180 DEG C and is dried to jelly, after obtained sample is ground, put
Enter in stove and calcined 10 hours at 600 DEG C, then take out regrinding, is next calcined 5 hours at 1000 DEG C, the powder after calcining
Body adds alcohol to grind, and it is pure phase to measure powder through XRD powder diffractometers, without other impurity, as shown in Figure 1.
Obtained cathode powder is pressed into disk and cylinder, is calcined 10 hours at 1100 DEG C, be respectively used to conductivity and
The measurement of thermal expansion.Fig. 2 is the thermal dilatometry measured, wherein (Pr0.9La0.1)2Ni0.74Cu0.21Al0.05O4+δCathode is in 30-
1000 DEG C of mean thermal expansion coefficients are 14.5 × 10-6K-1.High-temperature conductivity test is carried out to sample using direct current four-end method,
Fig. 3 is the conductivity map measured, (Pr0.9La0.1)2Ni0.74Cu0.21Al0.05O4+δHalf is embodied in 450 DEG C of temperature ranges below
Conductor transmission mechanism, 450 DEG C or more embody metal conduction mechanism, and it is 77Scm that conductivity is measured at 450 DEG C-1。
By (the Pr of preparation0.9La0.1)2Ni0.74Cu0.21Al0.05O4+δIt is equal by silk screen print method that cathode powder is made into slurry
The even both sides for being coated in fine and close SDC electrolyte calcine 2 hours Symmetrical cells obtained for testing impedance at 1000 DEG C.It is logical
It crosses electrochemical workstation and carries out impedance spectrum test, measure (Pr0.9La0.1)2Ni0.74Cu0.21Al0.05O4+δIt is different in air atmosphere
At a temperature of interfacial polarization impedance.Fig. 4 (a) is that interfacial polarization impedance varies with temperature curve, in 700 DEG C of interfacial polarization resistance
For 0.082 Ω cm2, fully meet the application requirement of sofc cathode material.
Electrolyte sheet is ground into the thickness of 0.3mm by diamond dust, by the same method by anode powder NiO-SDC
It is coated in the side of SDC, is calcined 4 hours at 1250 DEG C, (Pr will be obtained0.9La0.1)2Ni0.74Cu0.21Al0.05O4+δCathode slurry is logical
The other side that silk screen print method is evenly coated in SDC electrolyte sheets is crossed, is calcined 2 hours at 1000 DEG C, monocell is formed.After completion
One end of alumina tube is fixed in using silver paste, outwardly, anode is inwardly for cathode.Fig. 5 (a) be using SDC as electrolyte,
NiO-SDC is the monocell performance curve of anode, and the maximum power density of monocell is about 528mW cm at 800 DEG C-2。
Embodiment 2：(Pr0.9La0.1)1.95Ni0.74Cu0.21Al0.05O4+δPreparation, heat stability testing, the thermal expansion of cathode
Test, conductivity, impedance and cell output test.
The preparation of the sample and performance test step and embodiment 1 are almost the same, and required powder is measured through XRD powder diffractometers
End is pure phase, as shown in Figure 1.Fig. 2 is the thermal dilatometry measured, (Pr0.9La0.1)1.95Ni0.74Cu0.21Al0.05O4+δCathode
30-1000 DEG C of mean thermal expansion coefficients are 14.2 × 10-6K-1.Fig. 3 is the conductivity map measured, (Pr0.9La0.1)1.95Ni0.74Cu0.21Al0.05O4+δSemiconductor conductivity mechanism is embodied in 450 DEG C of temperature ranges below, 450 DEG C or more embody
Metal conduction mechanism, it is 63Scm that 450 DEG C, which measure conductivity,-1.Fig. 4 (b) is that interfacial polarization impedance varies with temperature curve,
700 DEG C of interfacial polarization resistance is 0.101 Ω cm2, fully meet the application requirement of sofc cathode material.Fig. 5 (b) is
(Pr0.9La0.1)1.95Ni0.74Cu0.21Al0.05O4+δUsing SDC as electrolyte, NiO-SDC is the monocell performance curve of anode,
The maximum power density of monocell is about 486mW cm at 800 DEG C-2。
Embodiment 3：(Pr0.9La0.1)1.9Ni0.74Cu0.21Al0.05O4+δThe preparation of cathode, is thermally expanded and is surveyed heat stability testing
It tries, the test of impedance and cell output.
The preparation of the sample and performance test step and embodiment 1 are almost the same, and required powder is measured through XRD powder diffractometers
End is pure phase, as shown in Figure 1.Fig. 2 is the thermal dilatometry measured, (Pr0.9La0.1)1.9Ni0.74Cu0.21Al0.05O4+δCathode 30-
1000 DEG C of mean thermal expansion coefficients are 14.1 × 10-6K-1.Fig. 3 is the conductivity map measured, 450 DEG C of humidity provinces below
Between embody semiconductor conductivity mechanism, 450 DEG C or more embody metal conduction mechanism, and it is 57Scm that 450 DEG C, which measure conductivity,-1。
Fig. 4 (c) is that interfacial polarization impedance varies with temperature curve, is 0.100 Ω cm in 700 DEG C of interfacial polarization resistance2, completely full
The application requirement of sufficient sofc cathode material.Fig. 5 (c) is (Pr0.9La0.1)1.9Ni0.74Cu0.21Al0.05O4+δIt is being electrolysis with SDC
Matter, NiO-SDC are the monocell performance curve of anode, and the maximum power density of monocell is about 477mW cm at 800 DEG C-2。
Claims (5)
1. a kind of Ca-Ti ore type cathode material for solid-oxide fuel cell and preparation method thereof, which is characterized in that the side
Method includes the following steps：
(1) it weighs：According to the stoichiometric ratio of above-mentioned material, Pr is weighed respectively6O11, Ni (NO3)2·3H2O, Cu (NO3)2·
3H2O, Al (NO3)3·9H2O and La2O3, according to metal ion: EDTA: citric acid=1: 1: 2, weigh EDTA and citric acid；
(2) colloidal sol is prepared：By Ni (NO3)2·3H2O, Cu (NO3)2·3H2O, Al (NO3)3·9H2O is poured into large beaker, then
By Pr6O11It pours into small measuring cup, nitric acid is added stirs to solution and clarify, then by La2O3It pours into another small measuring cup, adds
Nitric acid is stirred to solution and is clarified, and finally pours into the nitrate solution in two small measuring cups in large beaker, opens magnetic stirring apparatus
Start to stir, while EDTA is added, ammonium hydroxide is added and adjusts pH (pH is required 6~8), citric acid is then added, then add ammonium hydroxide tune
PH to 6~8 is saved, waits until liquid jelly, stops stirring, takes out magnon；
(3) it dries：The colloidal liquid that step (2) obtains is put into bellows, dries 24 hours to jelly exsiccation with 180 DEG C；
(4) it calcines：After the sample grinding that step (3) is obtained, it is put into Muffle furnace and is calcined 10 hours at 600 DEG C, then taken out
Regrinding calcines 5 hours at 1000 DEG C, finally adds alcohol grinding again, obtain cathode powder, then choose a part again
Tabletted and cylinder；
(5) prepared by Symmetrical cells：It is by silk screen print method being coated in symmetrically fine and close will to obtain cathode powder
Ce0.8Sm0.2O1.9(SDC) both sides of electrolyte sheet, and calcined 2 hours at 1000 DEG C；
(6) prepared by monocell：Anode powder NiO-SDC is coated in the side of SDC by the same method, 4 are calcined at 1250 DEG C
Hour, cathode powder will be obtained by silk screen print method and be evenly coated in the other side of SDC electrolyte sheets, it is small that 2 are calcined at 1000 DEG C
When, obtain the monocell for measured power；
(7) conductivity is tested with thermal expansion：The disk that step (4) is obtained uses the high-temperature electrical conductivity of direct current four-end method test material
Rate, the cylinder that step (4) is obtained are used for the coefficient of thermal expansion of test material.
2. a kind of perovskite cathode material for solid-oxide fuel cell and preparation method thereof as described in claim 1, feature
It is in step (1) that chemical composition used is：(Pr0.9La0.1)2Ni0.74Cu0.21Al0.05O4+δ, (Pr0.9La0.1)1.95Ni0.74Cu0.21Al0.05O4+δ, (Pr0.9La0.1)1.9Ni0.74Cu0.21Al0.05O4+δ。
3. a kind of perovskite cathode material for solid-oxide fuel cell and preparation method thereof as described in claim 1, feature
It is in step (4) that the synthesis temperature of disk and cylinder is calcined 10 hours for 1100 DEG C.
4. a kind of perovskite cathode material for solid-oxide fuel cell and preparation method thereof as described in claim 1, feature
It is that the electrolyte in step (5) is SDC, symmetry electrode preparation temperature is 1000 DEG C and calcines 2 hours.
5. a kind of perovskite cathode material for solid-oxide fuel cell and preparation method thereof as described in claim 1, feature
It is that the electrolyte in step (6) is SDC, anode powder NiO-SDC is coated in the side of SDC by the same method,
1250 DEG C are calcined 4 hours, will obtain cathode powder by silk screen print method and be evenly coated in the other side of SDC electrolyte sheets,
1000 DEG C are calcined 2 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110556542A (en) * | 2019-08-08 | 2019-12-10 | 黄山学院 | Cathode material of solid oxide fuel cell and preparation method thereof |
| CN111755671A (en) * | 2019-03-29 | 2020-10-09 | 宁德新能源科技有限公司 | Positive electrode material and lithium ion secondary battery |
| RU2749669C1 (en) * | 2020-12-24 | 2021-06-16 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Electrode material for electrochemical devices |
| RU2767036C1 (en) * | 2021-08-06 | 2022-03-16 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Method of producing complex oxides based on praseodymium nickelite doped with cobalt |
| RU2779630C1 (en) * | 2022-03-30 | 2022-09-12 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской академии наук (ИВТЭ УрО РАН) | Electrode material based on praseodymium nickelate for electrochemical devices |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111755671A (en) * | 2019-03-29 | 2020-10-09 | 宁德新能源科技有限公司 | Positive electrode material and lithium ion secondary battery |
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| RU2749669C1 (en) * | 2020-12-24 | 2021-06-16 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Electrode material for electrochemical devices |
| RU2767036C1 (en) * | 2021-08-06 | 2022-03-16 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Method of producing complex oxides based on praseodymium nickelite doped with cobalt |
| RU2779630C1 (en) * | 2022-03-30 | 2022-09-12 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской академии наук (ИВТЭ УрО РАН) | Electrode material based on praseodymium nickelate for electrochemical devices |
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