CN111129517A - Preparation method of Ruddlesden-Popper layered structure iron-based cathode catalyst - Google Patents
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Abstract
A preparation method of an iron-based cathode catalyst with Ruddlesden-Popper layered structure belongs to the field of chemical power source solid oxide fuel cell materials. The method comprises the following steps: firstly, adding glycine into a mixed solution of strontium nitrate, rare earth nitrate and ferric nitrate to prepare black powder; secondly, preparing cathode catalyst powder; thirdly, preparing a solid CGO electrolyte substrate; fourthly, uniformly mixing the electrode adhesive and the cathode catalyst powder, and symmetrically coating the mixture on a substrate to form a symmetrical electrode; and fifthly, sintering. The cathode catalyst prepared by the invention has high ion-electron mixed conductivity, high oxygen ion transmission speed and lower interfacial polarization resistance, and the universal iron base of the solid oxide fuel cell with high catalytic activity is obtainedSr3‑xLnxFe2O7‑δAn electrode catalyst. The preparation raw materials are easy to obtain, the thermal matching with the solid electrolyte is good, and the durability and the high-temperature chemical stability are high. The method is suitable for preparing the cathode catalyst of the solid oxide fuel cell.
Description
Technical Field
The invention belongs to the field of chemical power source solid oxide fuel cell materials.
Background
A solid oxide fuel cell is an all solid state form energy conversion device that converts chemical energy of a fuel into electrical energy through an electrochemical reaction. The energy-saving type energy-saving power supply has the remarkable advantages of high energy conversion efficiency, fuel flexibility, low pollutant emission and the like, is suitable for small fixed power supplies of distributed power stations and families, and is known as a novel green energy source in 21 century. The basic structure of the solid oxide fuel cell system mainly comprises three parts, namely a cathode, an anode and an electrolyte. The cathode is mainly used as an oxidation electrode to perform oxygen reduction reaction, and the electrocatalytic performance of the cathode directly influences the long-term stability and the output efficiency of a fuel cell system. Sr of Ruddlesden-Popper (Ludwiston-Borol) structure3Fe2O7-δThe oxide has two SrFeO3A perovskite layer with a SrO rock salt layer sandwiched in between. Compared with the traditional perovskite structure cathode material, the material has excellent high-temperature chemical stability and thermal stability, and the material has good oxygen ion conductivity, which means Sr3Fe2O7-δThe material is a promising cathode catalyst for solid oxide fuel cells.
With the development of high-performance fuel cells, the oxygen reduction activity of the cathode catalyst of the cell has been gaining attention. The traditional cobalt-based cathode material has the defects of high price, high thermal expansion coefficient, poor chemical compatibility, low electrocatalytic performance and the like, so that the application range of the traditional cobalt-based cathode material is limited. The iron-based cathode catalyst has the advantages of high-temperature chemical stability, good thermal matching property, high oxygen reduction activity and the like, and has good research and application in the fields of oxygen permeable membranes and ion-electron mixed conductors.
Disclosure of Invention
The invention aims to solve the problems that the ion-electron mixed conductivity and the oxygen reduction activity of the iron-based cathode catalyst of the existing solid oxide fuel cell are low, and the contact resistance of the cathode catalyst and the interface of a solid electrolyte is large, and provides a preparation method of the iron-based cathode catalyst with the Ruddlesden-Popper layered structure.
A preparation method of an iron-based cathode catalyst with Ruddlesden-Popper layered structure is realized by the following steps:
one, according to the chemical formula Sr3-xLnxFe2O7-δWeighing strontium nitrate, rare earth nitrate and ferric nitrate according to a stoichiometric ratio, dissolving the strontium nitrate, the rare earth nitrate and the ferric nitrate in deionized water to obtain a mixed solution, adding glycine, uniformly mixing, heating and concentrating at 150-300 ℃ until a combustion reaction occurs, and finally obtaining black powder;
secondly, performing steel die pressing on the black powder under the pressure of 100-250 MPa to obtain a wafer-shaped catalyst precursor, then sintering at 800-1000 ℃ for 8-12 h, taking out and grinding to obtain cathode catalyst powder;
thirdly, solid electrolyte Ce0.9Gd0.1O1.95Performing steel die pressing on the (CGO) powder under the pressure of 180-250 MPa to obtain an electrolyte substrate precursor, and then sintering at 1200-1400 ℃ for 12-20 h to obtain a solid CGO electrolyte substrate;
fourthly, mixing terpineol and ethyl cellulose according to a mass ratio of (2-5) to 1 to obtain an electrode adhesive, adding the cathode catalyst powder obtained in the second step into the electrode adhesive, uniformly mixing, and symmetrically coating the cathode catalyst powder on the solid CGO electrolyte substrate obtained in the third step by using a hairbrush to form a symmetrical electrode;
fifthly, sintering the symmetrical electrode for 2-8 hours at 900-1100 ℃ to obtain Sr3-xLnxFe2O7-δCathode, namely, the preparation of the Ruddlesden-Popper layered structure iron-based cathode catalyst is completed;
wherein step one has the chemical formula Sr3-xLnxFe2O7-δWherein Ln is La, Sm, Pr, Nd or Eu, and x is 0.1, 0.2, 0.3, 0.4 or 0.5;
in the first step, the total mole number of the metal ions Sr, Ln and Fe and the mole number of the glycine are 1: 2.
The invention has the advantages that:
the invention adopts a glycine-nitrate method to prepare the solid oxide fuel cell Sr with high ion-electron mixed conductivity and thermochemical stability3-xLnxFe2O7-δA nano cathode catalyst. Thereby increasing the electrocatalytic activity of the cathode material and improving the output performance of the fuel cell.
The nano cathode catalyst prepared by the invention has high ion-electron mixed conductivity and high oxygen ion transmission speed in the temperature range of 500-700 ℃, and has lower interfacial polarization resistance compared with the traditional powder cathode material, thereby obtaining the general iron-based Sr of the solid oxide fuel cell with high catalytic activity3-xLnxFe2O7-δAn electrode catalyst.
The preparation method has the advantages of easily available raw materials, good thermal matching with the solid electrolyte, and high durability and high-temperature chemical stability.
The method is suitable for preparing the cathode catalyst of the solid oxide fuel cell.
Drawings
FIG. 1 is Sr prepared in the example2.8La0.2Fe2O7-δAn X-ray diffraction spectrum of the cathode;
FIG. 2 shows Sr prepared in the example2.8La0.2Fe2O7-δA surface topography map of the cathode;
FIG. 3 is Sr prepared in the example2.8La0.2Fe2O7-δCathode and Sr3Fe2O7-δThe alternating current impedance spectrum of the cathode tested in 700 ℃ air, wherein Sr represents Sr2.8La0.2Fe2O7-δAC impedance spectrum of cathode, ○ represents Sr3Fe2O7-δThe AC impedance spectrum of the cathode.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the embodiment of the invention relates to a preparation method of an iron-based cathode catalyst with Ruddlesden-Popper layered structure, which is realized by the following steps:
one, according to the chemical formula Sr3-xLnxFe2O7-δWeighing strontium nitrate, rare earth nitrate and ferric nitrate according to a stoichiometric ratio, dissolving the strontium nitrate, the rare earth nitrate and the ferric nitrate in deionized water to obtain a mixed solution, adding glycine, uniformly mixing, heating and concentrating at 150-300 ℃ until a combustion reaction occurs, and finally obtaining black powder;
secondly, performing steel die pressing on the black powder under the pressure of 100-250 MPa to obtain a wafer-shaped catalyst precursor, then sintering at 800-1000 ℃ for 8-12 h, taking out and grinding to obtain cathode catalyst powder;
thirdly, solid electrolyte Ce0.9Gd0.1O1.95Performing steel die pressing on the (CGO) powder under the pressure of 180-250 MPa to obtain an electrolyte substrate precursor, and then sintering at 1200-1400 ℃ for 12-20 h to obtain a solid CGO electrolyte substrate;
fourthly, mixing terpineol and ethyl cellulose according to a mass ratio of (2-5) to 1 to obtain an electrode adhesive, adding the cathode catalyst powder obtained in the second step into the electrode adhesive, uniformly mixing, and symmetrically coating the cathode catalyst powder on the solid CGO electrolyte substrate obtained in the third step by using a hairbrush to form a symmetrical electrode;
fifthly, sintering the symmetrical electrode for 2-8 hours at 900-1100 ℃ to obtain Sr3-xLnxFe2O7-δCathode, namely, the preparation of the Ruddlesden-Popper layered structure iron-based cathode catalyst is completed;
wherein step one has the chemical formula Sr3-xLnxFe2O7-δWherein Ln is La, Sm, Pr, Nd or Eu, and x is 0.1, 0.2, 0.3, 0.4 or 0.5;
in the first step, the total mole number of the metal ions Sr, Ln and Fe and the mole number of the glycine are 1: 2.
The raw materials used in the present embodiment are all commercially available analytical pure raw materials.
The second embodiment is as follows: the difference between the present embodiment and the first embodiment is that the molar ratio of the metal ions Sr, Ln and Fe in the mixed solution in the first step is 2.8 (0.1, 0.2, 0.3, 0.4 or 0.5): 2. Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: the difference between the first and second embodiments is that the rare earth nitrate in the first step is lanthanum nitrate, samarium nitrate, praseodymium nitrate, neodymium nitrate or europium nitrate. Other steps and parameters are the same as those in the first or second embodiment.
The fourth concrete implementation mode: this embodiment differs from one of the first to third embodiments in that step one is concentrated by heating at 250 ℃. Other steps and parameters are the same as those in one of the first to third embodiments.
The fifth concrete implementation mode: this embodiment is different from one of the first to fourth embodiments in that the black powder is steel die-pressed under a pressure of 200MPa in the second step. Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is that the diameter of the wafer-shaped catalyst precursor in the second step is 100mm, and the thickness thereof is 50 mm. Other steps and parameters are the same as those in one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is that in the second step, the sintering is performed at 900 ℃ for 10 hours. Other steps and parameters are the same as those in one of the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and the first to seventh embodiments is that the particle size of the cathode catalyst powder ground in the second step is 3 μm. Other steps and parameters are the same as those in one of the first to seventh embodiments.
The specific implementation method nine: this embodiment is different from the first to eighth embodiments in that the solid electrolyte Ce in the third step0.9Gd0.1O1.95Performing steel die pressing on the (CGO) powder under the pressure of 2000MPa to obtain an electrolyte substrate precursor, and then placing at 1300 DEG CAnd sintering for 16 h. Other steps and parameters are the same as those in one to eight of the embodiments.
The detailed implementation mode is ten: this embodiment is different from one of the first to ninth embodiments in that the electrolyte base precursor in the third step has a diameter of 15mm and a thickness of 1 mm. Other steps and parameters are the same as those in one of the first to ninth embodiments.
The concrete implementation mode eleven: this embodiment differs from the first to tenth embodiments in that terpineol and ethyl cellulose are mixed in a mass ratio of 4:1 in step four. Other steps and parameters are the same as in one of the first to tenth embodiments.
The specific implementation mode twelve: the difference between the present embodiment and one of the first to eleventh embodiments is that the mass volume ratio of the cathode catalyst powder to the electrode binder in the fourth step is (1-4): 3. Other steps and parameters are the same as those in one of the first to eleventh embodiments.
The specific implementation mode is thirteen: the difference between this embodiment and the first to twelfth embodiments is that in the fifth step, the symmetrical electrodes are sintered for 5 hours at 1000 ℃. Other steps and parameters are the same as those in one to twelve embodiments.
The beneficial effects of the present invention are demonstrated by the following examples:
example (b):
a preparation method of an iron-based cathode catalyst with Ruddlesden-Popper layered structure is realized by the following steps:
one, according to the chemical formula Sr3-xLnxFe2O7-δWeighing strontium nitrate, lanthanum nitrate and ferric nitrate according to a stoichiometric ratio, dissolving the strontium nitrate, the lanthanum nitrate and the ferric nitrate in deionized water to obtain a mixed solution, adding glycine, uniformly mixing, heating and concentrating at 150 ℃ until a combustion reaction occurs, and finally obtaining black powder;
secondly, performing steel die pressing on the black powder under the pressure of 200MPa to obtain a wafer-shaped catalyst precursor, then sintering the wafer-shaped catalyst precursor at 900 ℃ for 10 hours, taking out the wafer-shaped catalyst precursor and grinding the wafer-shaped catalyst precursor to obtain cathode catalyst powder;
thirdly, mixing the solid electrolyteCe0.9Gd0.1O1.95Performing steel die pressing on the (CGO) powder under the pressure of 200MPa to obtain an electrolyte substrate precursor, and then sintering at 1400 ℃ for 12 hours to obtain a solid CGO electrolyte substrate;
fourthly, mixing terpineol and ethyl cellulose according to a mass ratio of 4:1 to obtain an electrode adhesive, then adding 0.1g of the cathode catalyst powder obtained in the second step into 0.3ml of the electrode adhesive, uniformly mixing, and symmetrically coating the mixture on the solid CGO electrolyte substrate obtained in the third step by using a brush to form a symmetrical electrode;
fifthly, the symmetrical electrode is sintered for 4 hours at 1000 ℃ to obtain Sr3-xLnxFe2O7-δCathode, namely, the preparation of the Ruddlesden-Popper layered structure iron-based cathode catalyst is completed;
wherein step one has the chemical formula Sr3-xLnxFe2O7-δWherein Ln is La, x is 0.2;
in the first step, the total mole number of metal ions Sr, La and Fe and the mole number of glycine are 1: 2.
Sr prepared in this example2.8La0.2Fe2O7-δThe cathode material is a typical Ruddlesden-Popper layered oxide, and the phase test of the cathode catalyst is performed by using an X-ray diffractometer, and the result is shown in figure 1.
Observation of Sr with a scanning Electron microscope SEM2.8La0.2Fe2O7-δThe result of the micro-morphology of the cathode is shown in fig. 2, the obtained cathode catalyst is nano-scale and has a certain porous structure, and certain sintering connection exists among electrode particles, and the micro-morphology is favorable for the diffusion and transportation of oxygen ions on the electrode.
The polarization resistance of the cathode of the material is tested by using a symmetrical electrode system under the air of 700 ℃ through an alternating-current impedance spectrum testing technology: the test result shows that Sr2.8La0.2Fe2O7-δThe cathode had a polarization resistance of 0.1ohm2The result is Sr3Fe2O7-δOne third of the powder cathode material (also tested)At a temperature of 0.3ohm2) (see FIG. 3). This indicates the use of rare earth element for Sr3Fe2O7-δThe electro-catalytic activity of the cathode catalyst can be improved by doping modification, the ion-electron mixed conductivity is increased, and the electrochemical performance of the cathode material is improved.
Claims (10)
1. A preparation method of an iron-based cathode catalyst with Ruddlesden-Popper layered structure is characterized by comprising the following steps:
one, according to the chemical formula Sr3-xLnxFe2O7-δWeighing strontium nitrate, rare earth nitrate and ferric nitrate according to a stoichiometric ratio, dissolving the strontium nitrate, the rare earth nitrate and the ferric nitrate in deionized water to obtain a mixed solution, adding glycine, uniformly mixing, heating and concentrating at 150-300 ℃ until a combustion reaction occurs, and finally obtaining black powder;
secondly, performing steel die pressing on the black powder under the pressure of 100-250 MPa to obtain a wafer-shaped catalyst precursor, then sintering at 800-1000 ℃ for 8-12 h, taking out and grinding to obtain cathode catalyst powder;
thirdly, solid electrolyte Ce0.9Gd0.1O1.95Performing steel die pressing on the powder under the pressure of 180-250 MPa to obtain an electrolyte substrate precursor, and then sintering at 1200-1400 ℃ for 12-20 h to obtain a solid CGO electrolyte substrate;
fourthly, mixing terpineol and ethyl cellulose according to a mass ratio of (2-5) to 1 to obtain an electrode adhesive, adding the cathode catalyst powder obtained in the second step into the electrode adhesive, uniformly mixing, and symmetrically coating the cathode catalyst powder on the solid CGO electrolyte substrate obtained in the third step by using a hairbrush to form a symmetrical electrode;
fifthly, sintering the symmetrical electrode for 2-8 hours at 900-1100 ℃ to obtain Sr3-xLnxFe2O7-δCathode, namely, the preparation of the Ruddlesden-Popper layered structure iron-based cathode catalyst is completed;
wherein step one has the chemical formula Sr3-xLnxFe2O7-δIn the formula Ln ═ La, Sm and PrNd or Eu, x ═ 0.1, 0.2, 0.3, 0.4, or 0.5;
in the first step, the total mole number of the metal ions Sr, Ln and Fe and the mole number of the glycine are 1: 2.
2. The method as claimed in claim 1, wherein the molar ratio of Sr, Ln and Fe in the mixed solution in the first step is 2.8 (0.1, 0.2, 0.3, 0.4 or 0.5): 2.
3. The method of claim 1, wherein the step one is concentrated by heating at 250 ℃.
4. The method of claim 1, wherein the black powder is steel-die pressed under a pressure of 200MPa in the second step.
5. The method as claimed in claim 1, wherein the diameter of the disk-shaped catalyst precursor in the second step is 100mm, and the thickness thereof is 50 mm.
6. The method for preparing an iron-based cathode catalyst with Ruddlesden-Popper layered structure as claimed in claim 1, wherein the sintering is performed at 900 ℃ for 10h in the second step.
7. The method of claim 1, wherein the electrolyte substrate precursor has a diameter of 15mm and a thickness of 1mm in the third step.
8. The method for preparing an iron-based cathode catalyst with Ruddlesden-Popper layered structure as claimed in claim 1, wherein terpineol and ethyl cellulose are mixed in a mass ratio of 4:1 in the step four.
9. The preparation method of the Ruddlesden-Popper layered structure iron-based cathode catalyst as claimed in claim 1, wherein the mass volume ratio of the cathode catalyst powder to the electrode binder in the fourth step is (1-4): 3.
10. The method as claimed in claim 1, wherein the symmetric electrode is sintered at 1000 ℃ for 5h in step five.
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Inventor after: Li Qiang Inventor after: Ma Tiezhu Inventor after: Zou Jinlong Inventor after: Huo Lihua Inventor after: Zhao Hui Inventor before: Li Qiang Inventor before: Zou Jinlong Inventor before: Ma Tiezhu Inventor before: Huo Lihua Inventor before: Zhao Hui |
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Application publication date: 20200508 |