CN102479957A - Method for cosynthesis of solid oxide fuel cell composite cathode material - Google Patents
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Abstract
The invention provides a method for cosynthesis of a solid oxide fuel cell composite cathode material. According to the method, the required composite cathode precursor materials are dissolved to obtain a clear solution system; a reaction reagent is added to the system; the pH value is adjusted to completely dissolve the reaction reagent; a heating reaction is performed, and the water is evaporated to obtain the transparent sol; the sol is transferred to an electric furnace to carry out heating combustion to obtain compound primary powder; the powder is subjected to a high temperature baking treatment to obtain the powder material having perovskite and a cubic fluorite phase, wherein the powder material is the mixed ionic electronic conductor, and has characteristics of fine and uniform particles, and large specific surface area. According to the present invention, with adopting the solid oxide fuel cell composite cathode material of the present invention as the solid oxide fuel cell cathode, the three-phase interfaces adopted as the electrochemical active sites are more and are uniformly distributed on the whole cathode body phase so as to contribute to improvement of the cell performance.
Description
Technical field
The present invention relates to solid oxide fuel cell composite cathode material, specifically a kind of method of synthesis of solid oxide fuel cell composite cathode material altogether.
Background technology
SOFC is a kind of energy reforming unit that chemical energy in the fuel is converted into electric energy.Generally have anode, electrolyte and negative electrode three parts, the oxygen in the gas phase diffuses into negative electrode, adsorbs, dissociates and accept electron conduction to transmit the electronics that comes mutually and change into oxonium ion and get into the electrolyte lattice; While fuel gas discharges electric transmission in anode generation oxidation reaction and circulates to external circuit, produces electric current, and the chemical energy in the fuel has been changed into electric energy.The cathodic oxygen reduction reaction is because the reaction activity that needs is high, and reaction rate is slow, and the polarization loss of generation is high, becomes the principal element of restriction solid-oxide fuel battery performance.Therefore study the negative electrode of high-performance and long-time stability, the preparation method who develops new cathode material or new cathode material just seems particularly important.
Thank morning sunlight CN101020604A patented invention a kind of preparation have the method for the perovskite material of cloth, felt, net or foaming structure; CN1315920A has proposed a kind of controlled atmospher and has carried out the method that high energy milling prepares perovskite material; CN101172661A has proposed a kind of gel of stearic acid firing method method and has prepared ultra-fine perovskite type LaFeO
3, LaMnO
3, LaNiO
3; Leandro da Conceicao et al adopts urea and glycine to prepare La as propellant respectively
0.7Sr
0.3MnO
3Perovskite material.The factor that will control in the above procedure is various, and only prepares perovskite material; SOFC develops into now composite cathodes that adopt more; And the acquisition of conventional composite negative electrode is the method through mechanical mixture, exist to mix uneven problem, so this patent proposes a kind of simple and effective method for preparing solid oxide fuel cell composite cathode material; Prepared material have simultaneously perovskite mutually with cube fluorite mutually; Granular size is equal, contacts with electrolyte interface well, can prepare the composite material of polycalcium titanium ore and fluorite structure.
Summary of the invention
The present invention proposes a kind of method of synthesis of solid oxide fuel cell composite cathode material altogether.
A kind of method of synthesis of solid oxide fuel cell composite cathode material altogether specifically may further comprise the steps,
1) will synthesize the required raw material of composite cathode material and be dissolved in the same solution system, stirring is dissolved it fully;
At first water-fast metal oxide is dissolved in an amount of nitric acid or the hydrogen peroxide solution based on stoichiometric proportion; The dissolving back adds the deionized water dilution fully; The back adds required metal nitrate, stirs the settled solution that preparation comprises whole metal ions in the composite;
2) according to the needed reaction reagent of the various computing of synthesis mechanism; In this clarified solution, add reaction reagent; Regulation system pH dissolves reaction reagent fully, and heating is reacted then, simultaneously transpiring moisture; Get transparent gluey presoma, make mol ratio >=1 of the metal ion sum in reaction reagent and the synthetic composite cathode material needed raw material:
3) should heat by the glue presoma, burn until presoma;
4) will the burn first powder of gained promptly got after 950-1200 ℃ of roasting 1-5 hour and has perovskite simultaneously mutually and cube fluorite compound mutually, did not have other dephasign; Be the hybrid ionic electronic conductor, particle is thin and evenly, specific area is big.As cathode of solid oxide fuel cell, its three phase boundary as electrochemical site is many and be uniformly distributed in whole cathode phase, helps improving battery performance.
This method is applicable to preparation perovskite phase and cube fluorite zirconio material mutually or the composite granule 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 occupies the Ca or the Sr element of perovskite A position for mixing, and M, N occupy perovskite B position and are selected from a kind of in the element of Cr, Mn, Fe, Co, Ni, Cu or more than two kinds, and the value of a is 0.8～1, and preferred 0.9～0.95; The value of x is 0～0.5, preferred 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 a kind of or more than two kinds.
The synthetic required raw material of composite cathode comprises the raw material that synthetic perovskite is mutually used with fluorite mutually; The mutually used raw material of perovskite are the nitrate more than two kinds in the metallic element in the perovskite, the mutually used raw material of fluorite be in nitrate and Gd, Sm, the Ce oxide of Y, La, Zr more than two kinds;
The general formula of said perovskite is (La
1-xZ
x)
a(M
1-yN
y) O
3 ± d, wherein Z occupies Ca or the Sr element of perovskite A for mixing, and M, N occupy perovskite B position and are selected from a kind of in the element of Cr, Mn, Fe, Co, Ni, Cu or more than two kinds, 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;
Said fluorite is YSZ mutually; A kind of among GDC, LDC, the SDC or more than two kinds.
Reaction reagent is a kind of in Triammonium citrate, EDTA+ citric acid, glycine, the urea, optimization citric acid three ammoniums or glycine, and the mol ratio of the metal ion sum in reaction reagent and the synthetic composite cathode needed raw material is generally 1-3.
Beneficial effect of the present invention:
The conventional composite negative electrode is to adopt to become the perovskite material of phase and fluorite material to carry out the mechanical lapping mixing, not only labor intensive and time, and mix inhomogeneously, and two contact badly, and three phase boundary is few.And synthetic method of the present invention is simple, and synthetic powder is meticulous fluffy, and average grain diameter has only tens nanometers; Specific area is big, reaches 20m
2/ g has the different size hole, helps the diffusion of gas; And the two-phase interface contact is good, and three phase boundary is dispersed throughout whole cathode phase, and the hydrogen reduction active sites increases greatly, and performance is increased to 180% of mechanical mixture negative electrode.
Description of drawings
Fig. 1 is the (La that adopts the Triammonium citrate method synthetic together
0.8Sr
0.2)
0.9MnO
3 ± dThe composite cathode material of-YSZ just powder is composed at the XRD figure of 950 ℃, 1000 ℃, 1100 ℃, 1200 ℃ following roasting 2h gained respectively.
Fig. 2 is the (La that adopts the Triammonium citrate method synthetic
0.6Ca
0.4)
0.9MnO
3 ± d-YSZ composite cathode material just powder is composed at the XRD figure of 1100 ℃ of roasting 2h.
Fig. 3 adopts the synthetic LSF-GDC of the ammonium citrate method XRD figure spectrum of 1100 ℃ of roasting 2h of powder just
Fig. 4 is the (La that adopts glycine method synthetic
0.8Sr
0.2)
0.9Mn
0.6Fe
0.4O
3 ± d-YSZ composite cathode material just powder is composed at the XRD figure of 1100 ℃ of roasting 2h.
The real formula of practical implementation
Embodiment 1
Adopt the synthetic (La of Triammonium citrate method
0.8Sr
0.2)
0.9MnO
3 ± d-YSZ composite cathode material, wherein (La
0.8Sr
0.2)
0.9MnO
3+dBe 0.005mol, YSZ and its mass ratio are 1: 1.5, take by weighing the La (NO of stoichiometric proportion
3)
36H
2O (analyzing pure), Sr (NO
3)
2(analyzing pure), Mn (NO
3)
2(analyzing pure), Zr (NO
3)
45H
2O (analyzing pure), Y (NO
3)
36H
2O (analyzing pure) is dissolved in the 100ml deionized water fully, and back according to Triammonium citrate: the ratio of metal ion total mole number=1: 2 (mol ratio) adds Triammonium citrate (analyzing pure); And it is dissolved fully with the pH value that nitric acid is reconciled mixed liquor, heat to make in the solution system then and react, and transpiring moisture; Solution becomes sticky thick gradually, is to move on the heating furnace behind the vitreosol to heat, and makes its burning; The first powder of composite material, with the first powder of gained respectively different temperature roasting 2 hours, carry out XRD characterize perovskite and cube fluorite mutually; No dephasign, spectrogram is shown in 1.
Embodiment 2
The preparation process is to adopt the Triammonium citrate method to synthesize (La with embodiment 1 with embodiment 1 difference
0.6Ca
0.4)
0.9MnO
3 ± d-YSZ composite material, wherein (La
0.6Ca
0.4)
0.9MnO
3 ± dBe 0.02mol, YSZ and its mass ratio 1: 1 take by weighing the La (NO of stoichiometric proportion
3)
36H
2O (analyzing pure), Ca (NO
3)
24H
2O (analyzing pure), Mn (NO
3)
2(analyzing pure), Zr (NO
3)
45H
2O (analyzing pure), Y (NO
3)
36H
2O (analyzing pure) is dissolved in the 200ml deionized water; According to Triammonium citrate: the ratio of metal ion total mole number=1: 1.5 (mol ratio) adds Triammonium citrate (analyzing pure), and first powder is in 1100 ℃ of roasting 2h; Its XRD figure spectrum is as shown in Figure 2.
Embodiment 3
Adopt ammonium citrate as the synthetic La of complexing agent
0.6Sr
0.4Fe
0.6O
3 ± d(LSF)-Gd
0.1Ce
0.9O
1.95(GDC) composite cathode material, wherein La
0.6Sr
0.4Fe
0.6O
3 ± dBe 0.02mol, GDC and its mass ratio are 1: 1, take by weighing the CeO of stoichiometric proportion
2(analyzing pure) successively slowly adds an amount of nitric acid and hydrogen peroxide solution, stirs and makes CeO
2After the dissolving, in this solution, add the Gd that deionized water dilution back adds stoichiometric proportion fully
2O
3(analyzing pure) adds La (NO after the stirring and dissolving
3)
36H
2O (analyzing pure), Sr (NO
3)
2(analyzing pure), Fe (NO
3)
39H
2O (analyzing pure), be stirred to solution clarification after, according to Triammonium citrate: the ratio of metal ion total mole number=1: 1.2 (mol ratio) adds Triammonium citrate (analyzing pure); And adjusting pH is 2; Fully dissolving back heating carry out network with, move to when treating the solution becomes thickness be heated on the electric furnace burn first powder, this is 1100 ℃ of roasting 2h of powder just; Perovskite and fluorite mutually, as shown in Figure 3.
Embodiment 4
Adopt the synthetic (La of glycine method
0.8Sr
0.2)
0.9Mn
0.6Fe
0.4O
3 ± d-YSZ composite cathode material, wherein (La
0.8Sr
0.2)
0.9Mn
0.6Fe
0.4O
3 ± dBe 0.02mol, YSZ and its mass ratio are 1: 1.5, take by weighing the La (NO of stoichiometric proportion
3)
36H
2O (analyzing pure), Sr (NO
3)
2(analyzing pure), Mn (NO
3)
2(analyzing pure), Zr (NO
3)
45H
2O (analyzing pure), Y (NO
3)
36H
2O (analyzing pure) places beaker, adds the 200ml deionized water; Stirring is dissolved it fully, and then according to glycine: metal ion total mole number=1: 3 (mol) adds the glycine of stoichiometric proportion, dissolving; Reacting by heating is steamed water, moves to heating flame on the electric furnace, and first powder is at 1100 ℃ of roasting 2h; Carry out XRD and characterize, collection of illustrative plates is as shown in Figure 4.
Claims (6)
1. method of synthesis of solid oxide fuel cell composite cathode material altogether is characterized in that: specifically may further comprise the steps,
1) will synthesize the composite cathode perovskite and be dissolved in the same solution system with the mutually required raw material of cube fluorite, stirring is dissolved it fully;
2) in this clarified solution, add reaction reagent, make mol ratio >=1 of the metal ion sum in reaction reagent and the synthetic composite cathode material needed raw material, regulation system pH dissolves reaction reagent fully; Heating is reacted then; Transpiring moisture gets transparent gluey presoma simultaneously
3) should heat by the glue presoma, burn until presoma;
4) will the burn first powder of gained promptly got after 950-1200 ℃ of roasting 1-5 hour and has perovskite simultaneously mutually and cube fluorite compound mutually.
2. method according to claim 1 is characterized in that:
The general formula of perovskite is (La
1-xZ
x)
a(M
1-yN
y) O
3 ± d, wherein Z occupies the Ca or the Sr element of perovskite A position for mixing, and M, N occupy perovskite B position and are selected from a kind of in the element of Cr, Mn, Fe, Co, Ni, Cu or more than two kinds, 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; Fluorite is a kind of among YSZ, GDC, LDC, the SDC or more than two kinds mutually.
3. method according to claim 1; It is characterized in that: the synthetic required raw material of composite cathode material comprises the raw material that synthetic perovskite is mutually used with fluorite mutually; The mutually used raw material of perovskite are the nitrate more than two kinds in the metallic element in the perovskite, the mutually used raw material of fluorite be in nitrate and Gd, Sm, the Ce oxide of Y, La, Zr more than two kinds;
The general formula of said perovskite is (La
1-xZ
x)
a(M
1-yN
y) O
3 ± d, wherein Z occupies the Ca or the Sr element of perovskite A position for mixing, and M, N occupy perovskite B position and are selected from a kind of in the element of Cr, Mn, Fe, Co, Ni, Cu or more than two kinds, 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;
Said fluorite is YSZ mutually; A kind of among GDC, LDC, the SDC or more than two kinds.
4. according to claim 2 or 3 described methods, it is characterized in that: the value of said a is 0.9～0.95; The value of x is 0.1～0.2.
5. method according to claim 1 is characterized in that: reaction reagent is a kind of in Triammonium citrate, EDTA+ citric acid, glycine, the urea, and the mol ratio of the metal ion sum in reaction reagent and the synthetic composite cathode material needed raw material is 1-3.
6. method according to claim 1 is characterized in that: reaction reagent is Triammonium citrate or glycine.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103887520A (en) * | 2012-12-21 | 2014-06-25 | 中国科学院大连化学物理研究所 | Method for preparing solid oxide fuel cell composite cathode through low-temperature sintering |
| CN105870459A (en) * | 2016-04-09 | 2016-08-17 | 大连理工大学 | High-catalytic activity composite negative electrode material of intermediate-temperature solid oxide fuel cell and preparation method of composite negative electrode material |
| CN106856242A (en) * | 2017-01-12 | 2017-06-16 | 黑龙江大学 | A kind of method that colloid composite algorithm in situ prepares solid oxide fuel cell composite cathode material RBCO xCGO |
| 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 |
| CN109841840A (en) * | 2017-11-28 | 2019-06-04 | 中国科学院大连化学物理研究所 | A kind of high-temperature electrolysis pond hybrid fuel electrode and preparation method thereof |
| CN111244470A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Nano composite cathode and preparation and application thereof |
| CN114408986A (en) * | 2022-01-21 | 2022-04-29 | 陕西彩虹新材料有限公司 | Nanoscale single crystal ternary cathode material and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103887520A (en) * | 2012-12-21 | 2014-06-25 | 中国科学院大连化学物理研究所 | Method for preparing solid oxide fuel cell composite cathode through low-temperature sintering |
| 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 |
| 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 |
| CN105870459A (en) * | 2016-04-09 | 2016-08-17 | 大连理工大学 | High-catalytic activity composite negative electrode material of intermediate-temperature solid oxide fuel cell and preparation method of composite negative electrode material |
| CN105870459B (en) * | 2016-04-09 | 2018-08-14 | 大连理工大学 | A kind of high catalytic activity intermediate temperature solid oxide fuel cell composite cathode material and preparation method thereof |
| CN106856242A (en) * | 2017-01-12 | 2017-06-16 | 黑龙江大学 | A kind of method that colloid composite algorithm in situ prepares solid oxide fuel cell composite cathode material RBCO xCGO |
| CN106856242B (en) * | 2017-01-12 | 2019-08-09 | 黑龙江大学 | A kind of method that original position colloid composite algorithm prepares solid oxide fuel cell composite cathode material RBCO-xCGO |
| CN109841840A (en) * | 2017-11-28 | 2019-06-04 | 中国科学院大连化学物理研究所 | A kind of high-temperature electrolysis pond hybrid fuel electrode and preparation method thereof |
| CN111244470A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Nano composite cathode and preparation and application thereof |
| CN111244470B (en) * | 2018-11-29 | 2021-05-04 | 中国科学院大连化学物理研究所 | Nano composite cathode and preparation and application thereof |
| CN114408986A (en) * | 2022-01-21 | 2022-04-29 | 陕西彩虹新材料有限公司 | Nanoscale single crystal ternary cathode material and preparation method thereof |
| CN114408986B (en) * | 2022-01-21 | 2024-02-13 | 陕西彩虹新材料有限公司 | Nanoscale monocrystal ternary cathode material and preparation method thereof |
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Application publication date: 20120530 |