CN114765260B - Bismuth ion doped layered double perovskite cathode material and preparation method thereof - Google Patents
Bismuth ion doped layered double perovskite cathode material and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000010406 cathode material Substances 0.000 title claims description 6
- 229910001451 bismuth ion Inorganic materials 0.000 title description 2
- 239000000446 fuel Substances 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- 230000007935 neutral effect Effects 0.000 claims abstract description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000004471 Glycine Substances 0.000 claims description 8
- 239000003814 drug Substances 0.000 claims description 8
- 229940079593 drug Drugs 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Inorganic materials [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 25
- 238000000034 method Methods 0.000 abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- 238000005245 sintering Methods 0.000 abstract description 5
- XPFAJCSMHOQBQB-UHFFFAOYSA-N 2-aminoacetic acid;nitric acid Chemical compound O[N+]([O-])=O.NCC(O)=O XPFAJCSMHOQBQB-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 229910002651 NO3 Inorganic materials 0.000 description 18
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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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
-
- 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
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
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Abstract
The invention belongs to the field of solid oxide fuel cells, and particularly relates to an A-site doped Bi modified layered double perovskite material and a preparation method thereof. One material has the structural formula Ln 1‑ xBixBaCo2O5+δ, and delta is a value that keeps the compound of the chemical formula electrically neutral. The material is prepared by adopting a glycine nitrate method, has a simple process and does not need expensive experimental instruments. The material obtained by the invention has the characteristics of excellent oxygen exchange capacity, excellent catalytic activity, reduced sintering temperature, excellent stability and the like, can obtain a solid oxide fuel cell material with high electrochemical performance and stable long-time operation, and is beneficial to reducing the cell cost.
Description
Technical Field
The invention relates to the technical field of solid oxide fuel cells, in particular to a double perovskite structure medium temperature solid oxide fuel cell cathode material and a preparation method thereof.
Background
The solid oxide fuel cell is used as a new energy source with high efficiency and no pollution, and the electrode reacts with electrolyte at high temperature to reduce the performance of the cell, so that the long-term operation stability of the cell is poor, and the like, so that the solid oxide fuel cell has a longer path for commercial application.
As a new energy material, perovskite type rare earth composite oxide is used as a mixed ion and electron conductor, so that the perovskite type rare earth composite oxide still has good oxygen exchange capability at reduced temperature, and also has lower polarization resistance and better catalytic activity, so that the perovskite type rare earth composite oxide is widely researched, but the commercialization of the perovskite type rare earth composite oxide is hindered because of the problem of unbalanced performance, such as poor stability when the performance is better; the layered double perovskite has a certain improvement over the common perovskite in that the layered double perovskite is not commercially available. Therefore, some methods for improving electrochemical performance and improving battery stability by doping become current research hot spots, different doping modes have different effects, bi doping is widely applied to other material application fields as a doping mode, a great deal of researches show that Bi doping has good effect on improving material performance, bi doping finds that the effect of reducing sintering temperature and the high conductivity of Bi2O3 can improve material performance, and the method is a doping method for improving the performance of a layered double perovskite material with potential.
The introduction of aliovalent alkaline earth or transition metals at the a-site, the crystals need to create additional oxygen defects and/or raise the oxidation state of the transition metal to balance the lost charge, which can improve the oxygen hole concentration and reactivity of the perovskite material. The A-site Bi doping can improve the conductivity of the layered double perovskite material, because Bi is doped on the A-site to form Bi2O3 with high ion conductivity, the oxygen exchange performance is further improved, the polarization resistance at low temperature in the layered double perovskite material is further reduced, more oxygen vacancies are formed along with the increase of doping amount, the electrochemical performance of the layered double perovskite material is improved, the doped Bi can maintain good stability for a long time in a single cell test, good conditions are provided for commercial utilization, and besides, the Bi & lt3+ & gt melting point is lower, so that the A-site doped Bi can reduce the sintering temperature of a solid oxide fuel cell to be too high, energy is saved, and meanwhile, the cost is reduced.
Disclosure of Invention
In order to reduce the problems of the prior material, the invention designs the A-site doped Bi modified double perovskite material with good oxygen exchange performance, good stability, easily obtained raw materials and simple and efficient preparation process and the preparation method thereof.
The technical scheme is that the A-site doped Bi modified double perovskite material is prepared, the structural formula of the material is Ln 1-xBixBaCo2O5+δ, and delta is a value for keeping a compound of a chemical formula electrically neutral; the preparation method of the A-site doped Bi modified double perovskite material comprises the following steps:
(1) Weighing excessive rare earth oxides such as Ln 2O3 (Ln= La, nd, sm, gd, Y and Pr) and the like, preheating for 2 hours at 800 ℃, dripping a proper amount of nitric acid, heating and stirring at 100-150 ℃ to completely dissolve the rare earth oxides to form Ln (NO 3)3 solution;
(2) The Bi (NO 3)3,Ba(NO3)2,Co(NO3)2∙6H2 O other medicines are weighed according to the stoichiometric ratio of x to 1:2 and then added into a proper amount of deionized water for sealing and preservation;
(3) All medicines are formulated, the glycine amount is calculated according to the ratio of G/N=0.54, and the glycine amount is added and put into other solutions to form mixed solution;
9(1-x)Ln(NO3)3+9xBi(NO3)3+9Ba(NO3)2+18Co(NO3)2∙6H2O+44C2H5NO2=9Ln1- xBixBaCo2O5+δ+62.5N2+88CO2+218H2O
(4) And placing the mixed solution on a magnetic stirrer, heating and stirring at 120-180 ℃ until the moisture evaporates to form black gel, and continuing heating and starting combustion to obtain precursor powder.
The invention has the technical advantages that:
(1) Bi 2O3 with high ion conductivity is formed by doping Bi on the A site, so that the oxygen exchange performance is improved, the conductivity of the material is improved, and the polarization resistance of the material is reduced;
(2) Oxygen vacancies as a measure of ion transport capacity, increase with increasing Bi 3+ content, show good electrochemical performance;
(3) The doped Bi keeps good stability in a long time in practical test;
(4) The material prepared by the glycine nitrate method has simple process and lower natural burning temperature, can be prepared into uniform particle size distribution, has greatly improved performance compared with other methods, can reduce the sintering temperature by doping Bi 3+, reduces the cost, and can be used for commercial operation.
Drawings
Figure 1 is an XRD pattern of an example synthetic material.
Fig. 2 is an impedance diagram of example one and SDC, LSGM.
FIG. 3 is an SEM image of different sintering temperatures of an example material.
Detailed Description
The description is made with reference to the drawing of Nd 1-xBixBaCo2O5+δ.
The method and the preparation material of the invention are tested for performance to verify the effect, and the advantages are shown in a form or a picture.
Verification is performed in connection with the application in the actual field.
Embodiment one: nd 1-xBixBaCo2O5+δ (x=0.1, nbbc0.1) double perovskite powder preparation.
The preparation process comprises the following steps:
(1) Preheating 0.9mol of Nd 2O3 rare earth oxide for 2 hours at 800 ℃ according to the components, dripping a proper amount of nitric acid, heating and stirring at 100-150 ℃ to completely dissolve the weighed Nd 2O3 rare earth oxide to form Nd (NO 3)3 solution, weighing other medicines with 0.1molBi(NO3)33,1molBa(NO3)2,2molCo(NO3)2∙6H2O according to the stoichiometric ratio of 0.9:0.1:1:2, and adding a proper amount of deionized water for sealing and preserving;
(2) All medicines are formulated, the glycine amount is calculated according to the ratio of G/N=0.54, and the glycine amount is added and put into other solutions to form mixed solution;
8.1Nd(NO3)3+0.9Bi(NO3)3+9Ba(NO3)2+18Co(NO3)2∙6H2O+44C2H5NO2=9Nd0.9Bi0.1BaCo2O5+δ+62.5N2+88CO2+218H2O
(3) And placing the mixed solution on a magnetic stirrer, heating and stirring at 120-180 ℃ until the moisture evaporates to form black gel, and continuing heating and starting combustion to obtain precursor powder Nd 0.9Bi0.1BaCo2O5+δ.
FIG. 1 shows a synthesized Nd 0.9Bi0.1BaCo2O5+δ, which has no impurity phase generation, a tetragonal structure, and a SEM with a lower synthesis temperature than NdBaCo 2O5+δ (1150 or more); nd 0.9Bi0.1BaCo2O5+δ polarization resistance of fig. 2 shows lower than NdBaCo 2O5+δ.
Embodiment two: preparation of Nd 1-xBixBaCo2O5+δ (x=0.05, NBBC0.05) double perovskite powder
(1) Preheating 0.95mol of Nd 2O3 rare earth oxide for 2 hours at 800 ℃ according to the components, dripping a proper amount of nitric acid, heating and stirring at 100-150 ℃ to completely dissolve the weighed Nd 2O3 rare earth oxide to form Nd (NO 3)3 solution, weighing other medicines with 0.05molBi(NO3)33,1molBa(NO3)2,2molCo(NO3)2∙6H2O according to the stoichiometric ratio of 0.95:0.05:1:2, and then adding the weighed Nd 2O3 rare earth oxide into a proper amount of deionized water for sealing and preserving;
(2) All medicines are formulated, the glycine amount is calculated according to the ratio of G/N=0.54, and the glycine amount is added and put into other solutions to form mixed solution;
8.65Nd(NO3)3+0.45Bi(NO3)3+9Ba(NO3)2+18Co(NO3)2∙6H2O+44C2H5NO2=9Nd0.95Bi0.05BaCo2O5+δ+62.5N2+88CO2+218H2O
(3) And placing the mixed solution on a magnetic stirrer, heating and stirring at 120-180 ℃ until the moisture evaporates to form black gel, and continuing heating and starting combustion to obtain precursor powder Nd 0.95Bi0.05BaCo2O5+δ.
The invention is not limited to the above two examples, and all doping methods for the A-site Bi-doped layered double perovskite material are within the scope of protection.
Claims (1)
1. A preparation method of a double perovskite type medium temperature solid oxide fuel cell cathode material doped with Bi at A site is characterized in that the structural formula of the cathode material is thatDelta is a value that maintains the compound of formula (la) neutral, where Ln is La, nd, sm, gd, Y or Pr rare earth element; the structure of the cathode material is a tetragonal structure;
the preparation method comprises the following steps:
(1) According to Weighing excessive Ln 2O3 rare earth oxide, preheating for 2 hours at 800 ℃ to remove water, dripping a proper amount of nitric acid, heating and stirring at 100-150 ℃ to completely dissolve the Ln (NO 3)3 solution;
(2) Weighing the Bi (NO 3)3,Ba(NO3)2,Co(NO3)2∙6H2 O and other medicines according to the stoichiometric ratio of x to 1:2, adding the weighed Bi into a proper amount of deionized water, and sealing and preserving;
(3) All medicines are formulated, the glycine amount is calculated according to the ratio of G/N=0.54, and the glycine amount is added and put into other solutions to form mixed solution;
，
；
(4) And placing the mixed solution on a magnetic stirrer, heating and stirring at 120-180 ℃ until moisture is evaporated to form black gel, continuously heating and starting to burn, so as to obtain precursor powder, and calcining the precursor at 1000 ℃ for 10 hours to obtain the oxide with the required double perovskite structure.
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