CN111697243A - Nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell and preparation method thereof - Google Patents
Nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a perovskite type intermediate temperature solid oxide fuel cell nanofiber cathode material and a preparation method thereof, wherein the B site of the perovskite type intermediate temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the chemical formula of the perovskite type intermediate temperature solid oxide fuel cell nanofiber cathode material is YCoxFe1‑xO3Wherein x is more than 0 and less than 1, the surface of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is smooth, the diameter is 300-400nm, the specific surface area of the cathode material is high, the contact area of the cathode material to gas is large, and the pairing can be efficiently finishedThe oxygen molecule reaction is convenient for the transmission of oxygen ions and electrons, and the preparation method is simpler.
Description
Technical Field
The invention belongs to the technical field of solid oxide fuel cells, and relates to a perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material and a preparation method thereof.
Background
A Solid Oxide Fuel Cell (SOFC) is an all-solid-component energy conversion device that directly converts chemical energy of fuel gas (hydrogen, methane, etc.) into electrical energy, has outstanding advantages of high energy conversion efficiency, environmental friendliness, no pollution, etc., and has become a new energy technology that draws attention. The traditional SOFC generally works at high temperature (above 1000 ℃), but the application of the cell material is limited by the high temperature, the cell material is expensive and easy to age after long-term operation, so that the cell material faces a lot of difficulties in application, and the exploration and application (550-700 ℃) of the medium-temperature fuel cell are a hotspot and development direction of current research.
The total loss of the solid oxide fuel cell at the intermediate temperature is mainly caused by the polarization of the cathode. As the operating temperature decreases, the oxygen ion and electron transfer rates of the electrode, particularly the cathode, decrease, and the oxygen reduction capability becomes weaker, so that the electrode polarization increases. Compared with the oxidation reaction of fuel gas such as anode hydrogen, the reduction reaction of oxygen at the cathode has higher reaction activation energy and lower chemical reaction rate, and the diffusion adsorption and dissociation of oxygen molecules are more complicated and difficult compared with the hydrogen molecules at the anode, so the key of the intermediate-temperature solid oxide fuel cell lies in the selection and structural improvement of cathode materials.
In the study of intermediate temperature solid oxide fuel cells, YCoxFe1-xO3(YCF, wherein x is more than or equal to 0 and less than or equal to 1) is a cathode material with industrial prospect. The YCF material is in YFeO3And YCoO3On the basis, the B-site element has higher mixed conductance of ions and electrons and excellent oxygen catalytic activity by doping. In addition, the middle-temperature SOFC test cell mostly uses a gadolinium oxide doped cerium oxide (GDC) electrolyte, the GDC electrolyte has high oxygen ion conduction activity at the middle temperature, and the GDC electrolyte and a YCF material have good thermal matching property and chemical stability at the middle temperature.
The cathode performance of the solid oxide fuel cell is not only reflected in the process of adsorption, dissociation and reduction of oxygen molecules after contacting with oxygen, but also reflected in the rapid transmission of oxygen ions and electrons. Besides the performance of the cathode is related to the properties of the cathode material, the microstructure of the cathode is also a key factor influencing the performance of the cathode. The traditional electrode material mainly uses a micron particle stacking structure, the specific surface area is low, the contact area to gas is small, the reaction to oxygen molecules cannot be efficiently completed, and contact resistance exists between micron particles and particles, so that the transmission of oxygen ions and electrons is not facilitated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material and a preparation method thereof.
In order to achieve the purpose, the B site of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the chemical formula of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is YCoxFe1-xO3Wherein x is more than 0 and less than 1, the surface of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is smooth, and the diameter is 300-400 nm.
The preparation method of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material comprises the following steps:
according to the stoichiometric ratio of nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell, adding Y (NO)3)3·6H2O、Co(NO3)2·6H2O and Fe (NO)3)3·9H2Mixing O, adding dimethylformamide and polyvinylpyrrolidone, mixing and magnetically stirring to form uniform and stable dark red sol, putting the sol into an electrostatic spinning device through an injector for electrostatic spinning to obtain an electrostatic spun fiber sample, calcining the electrostatic spun fiber sample, and naturally stirringAnd cooling to room temperature to obtain the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell.
In the electrostatic spinning treatment process, the distance between a needle head in an injector and a collector in an electrostatic spinning device is 15cm, the electrostatic spinning voltage is 18kV, the temperature is 20 ℃, and the relative humidity is 35%.
The inside diameter of the needle in the syringe was 0.6 mm.
The temperature in the calcination process is 950 ℃, and the calcination time is 3 h.
The invention has the following beneficial effects:
when the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material and the preparation method thereof are operated specifically, the B site of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is doped with one or two of Co element and Fe element, namely YFeO3In addition, when the invention is prepared, the temperature solid oxide fuel cell nanofiber prepared by combining the electrostatic spinning technology and the sol-gel method forms a net structure at the cathode, compared with the traditional electrode structure, the specific surface area and the adsorption capacity with oxygen are greatly improved, the three-phase interface (TPB) of the cathode reaction is increased, the transmission of oxygen ions and electrons is facilitated, the polarization resistance of the cathode is reduced, and the invention has good application prospect. Tests prove that the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material has good catalytic activity for oxygen reduction reaction and excellent electrochemical performance at the intermediate temperature of 550-750 ℃, can simultaneously meet the performance requirement of an intermediate-temperature SOFC cathode, and can be used as an intermediate-temperature SOFC cathode material.
Drawings
FIG. 1 is an XRD pattern of YCF nanofibers, GDC electrolyte powder and YCF-GDC mixed powder obtained after air atmosphere treatment for 3h at 950 ℃;
FIG. 2a is a scanning electron microscope image of a sample of YCF nanofibers after treatment in air atmosphere at 950 ℃ for 3h at low resolution;
FIG. 2b is a high resolution scanning electron microscope image of a sample of YCF nanofibers after treatment in air atmosphere at 950 ℃ for 3 h;
FIG. 3a is a graph of the energy dispersive X-ray spectroscopy of Y after YCF nanofibers were treated at 950 ℃ for 3h in air;
FIG. 3b is the energy dispersive X-ray spectrum of Co after YCF nanofibers are treated for 3h at 950 ℃ in air atmosphere;
FIG. 3c is a graph of energy dispersive X-ray spectroscopy of Fe after YCF nanofibers are treated for 3h at 950 ℃ in air atmosphere;
FIG. 3d is an energy dispersive X-ray spectroscopy plot of O after YCF nanofibers were treated at 950 ℃ for 3h in air;
YCo in FIG. 4axFe1-xO3The polarization impedance spectrogram of the corresponding nanofiber at 550 ℃ and 600 ℃ in the air atmosphere;
YCo in FIG. 4bxFe1-xO3A polarization impedance spectrogram of the nano fiber corresponding to 550 ℃ and 700 ℃ in air atmosphere;
FIG. 4c is a graph of power density at 550 ℃ for a NiO-GDC YCF full cell.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
example one
The B site of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the chemical formula of the material is YCoxFe1-xO3(YCF), wherein x is 0.5, the surface of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell is smooth.
The preparation method of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material comprises the following steps:
according to YCoxFe1-xO3Is stoichiometric ratio of Y (NO)3)3·6H2O、Co(NO3)2·6H2O and Fe (NO)3)3·9H2Mixing O, mixing with dimethylformamide (DMF for short, AR analytically pure) and polyvinylpyrrolidone (PVP for short, molecular weight is approximately equal to 130000, purity is 99.99%), magnetically stirring for 24h to form uniform and stable dark red sol, sucking the sol through an injector, putting the sol into an electrostatic spinning device, keeping the inner diameter of a needle of the injector at 0.6mm, keeping the distance between the needle and a collector at 15cm, carrying out the electrostatic spinning process under the environment of 18kV, 20 ℃ room temperature and 35% relative humidity, putting a fiber sample after electrostatic spinning in an oven, keeping the temperature for 1h at 80 ℃, then putting in a high-temperature furnace, calcining for 3h at 950 ℃, and finally naturally cooling to room temperature to obtain the perovskite type moderate-temperature solid oxide fuel cell nanofiber cathode material.
Grinding and mixing the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material and GDC powder according to the mass ratio of 5:5, and calcining the mixture for 3 hours at 950 ℃ to obtain YCF-GDC mixed powder, wherein the YCF-GDC mixed powder is used for testing the chemical stability of the YCF nanofiber and the GDC electrolyte at high temperature.
YCo will be mixedxFe1-xO3Mixing fiber cathode material powder with an organic solvent obtained by mixing 5% terpineol and 95% turpentine to obtain electrode slurry, symmetrically coating the electrode slurry on the central positions of two sides of a GDC (gadolinium oxide doped cerium oxide) electrolyte sheet by adopting a screen printing method, calcining for 3 hours at the air atmosphere of 950 ℃, then coating silver paste on the electrode attachment positions of the two sides of the electrolyte sheet, leading out by using silver wires, and calcining for 1 hour at the air atmosphere of 600 ℃ to obtain the YCF | GDC | YCF symmetrical half cell for testing the electrochemical impedance spectroscopy.
Adding NiO (nickel oxide with the particle size of 30nm and the purity of 99.99 percent), GDC electrolyte (with the particle size of 2 mu m and the purity of 99.9 percent) powder and graphite powder (with the particle size of 4000 meshes and the purity of 99.99 percent) into a ball mill, then ball-milling for 24 hours, drying in an oven at 70 ℃ to obtain anode powder, tabletting the anode powder under the pressure of 90MPa of a tabletting machine and calcining for 3 hours at 1100 ℃ to obtain a NiO-GDC anode porous supporting substrate, mixing the GDC electrolyte powder, terpineol and ethyl cellulose, ball-milling for 24 hours to obtain GDC electrolyte spin-coating slurry, uniformly dripping the GDC electrolyte spin-coating slurry on the NiO-GDC anode substrate, and spin-coating the GDC electrolyte spin-coating slurry on the NiO-GDC anode substrateSpin-coating at 3000 r/min for 30s to obtain GDC electrolyte film, repeating the spin-coating steps for three times, air-drying the electrolyte film at room temperature, calcining at 1500 deg.C for 3h to obtain compact GDC electrolyte layer, and mixing YCoxFe1-xO3Mixing fiber cathode material powder with an organic solvent obtained by mixing 5% terpineol and 95% turpentine to obtain electrode slurry, coating the electrode slurry on the central position of the upper layer of a GDC (gadolinium oxide doped cerium oxide) electrolyte sheet by adopting a screen printing method, calcining for 3 hours at the air atmosphere of 950 ℃, then coating electrode attachment positions on two sides of the electrolyte sheet and leading out silver paste by silver wires, and calcining for 1 hour at the air atmosphere of 600 ℃ to obtain the NiO-GDC | GDC | YCF full cell for testing, wherein the NiO-GDC | GDC | YCF full cell is used for testing the electrochemical power density.
Fig. 1 is an XRD chart of the YCF nanofibers, GDC electrolyte powder and YCF-GDC mixed powder obtained after air atmosphere treatment at 950 ℃ for 3 hours, and the results show that the YCF cathode fibers obtained in this example have a single perovskite structure, no impurity phase is generated at 950 ℃, and the XRD patterns of the YCF and GDC substances show that the YCF and GDC powders have good chemical stability at 950 ℃ and below.
Fig. 2a and 2b are respectively a low-resolution scanning electron microscope image and a high-resolution scanning electron microscope image of a YCF nanofiber sample treated in air atmosphere at 950 ℃ for 3 hours, and the results show that the diameter of the YCF nanofiber is 300-400nm, the fiber surface is smooth, and the whole fiber has a net structure, which is beneficial to gas adsorption and ion electron transmission.
FIGS. 3a to 3d are the energy dispersive X-ray spectroscopy (EDS-mapping) graphs of YCF nanofibers treated for 3 hours in air atmosphere at 950 ℃, and the results show that the diameter of the YCF nanofibers is 400nm at 300 ℃ and the elements of Y, Co, Fe and O are uniformly distributed in the YCF fibers.
YCo in FIG. 4a, FIG. 4b and FIG. 4cxFe1-xO3(where x ═ 0.5) polarization impedance spectra corresponding to different test temperatures of nanofibers in air atmosphere (550 ℃ with 600 ℃ (a), 650 ℃ with 700 ℃ (b)) were plotted against power density at 550 ℃ for NiO-GDC | YCF full cell. The result shows that the YCF nano-fiber has excellent electrochemical performance under the air atmosphere conditionThe YCF nano-fiber can be used as a cathode material with excellent performance.
Example two
The B site of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the chemical formula of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is YCoxFe1-xO3Wherein x is 0.01, and the surface of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell is smooth.
The preparation method of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material comprises the following steps:
according to the stoichiometric ratio of nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell, adding Y (NO)3)3·6H2O、Co(NO3)2·6H2O and Fe (NO)3)3·9H2And O, mixing, adding dimethylformamide and polyvinylpyrrolidone, mixing, magnetically stirring uniformly to form uniform and stable dark red sol, putting the sol into an electrostatic spinning device through an injector for electrostatic spinning to obtain an electrostatic spun fiber sample, calcining the electrostatic spun fiber sample, and naturally cooling to room temperature to obtain the perovskite type moderate-temperature solid oxide fuel cell nanofiber cathode material.
In the electrostatic spinning treatment process, the distance between a needle head in an injector and a collector in an electrostatic spinning device is 15cm, the electrostatic spinning voltage is 18kV, the temperature is 20 ℃, and the relative humidity is 35%.
The inside diameter of the needle in the syringe was 0.6 mm.
The temperature in the calcination process is 950 ℃, and the calcination time is 3 h.
EXAMPLE III
The B site of the perovskite type intermediate temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the material is characterized in thatHas a chemical formula of YCoxFe1-xO3Wherein x is 0.99, the surface of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell is smooth, and the diameter is 300-400 nm.
The preparation method of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material comprises the following steps:
according to the stoichiometric ratio of nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell, adding Y (NO)3)3·6H2O、Co(NO3)2·6H2O and Fe (NO)3)3·9H2And O, mixing, adding dimethylformamide and polyvinylpyrrolidone, mixing, magnetically stirring uniformly to form uniform and stable dark red sol, putting the sol into an electrostatic spinning device through an injector for electrostatic spinning to obtain an electrostatic spun fiber sample, calcining the electrostatic spun fiber sample, and naturally cooling to room temperature to obtain the perovskite type moderate-temperature solid oxide fuel cell nanofiber cathode material.
In the electrostatic spinning treatment process, the distance between a needle head in an injector and a collector in an electrostatic spinning device is 15cm, the electrostatic spinning voltage is 18kV, the temperature is 20 ℃, and the relative humidity is 35%.
The inside diameter of the needle in the syringe was 0.6 mm.
The temperature in the calcination process is 950 ℃, and the calcination time is 3 h.
Example four
The B site of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the chemical formula of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is YCoxFe1-xO3Wherein x is 0.3, the surface of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell is smooth, and the diameter is 300-400 nm.
The preparation method of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material comprises the following steps:
according to the stoichiometric ratio of nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell, adding Y (NO)3)3·6H2O、Co(NO3)2·6H2O and Fe (NO)3)3·9H2And O, mixing, adding dimethylformamide and polyvinylpyrrolidone, mixing, magnetically stirring uniformly to form uniform and stable dark red sol, putting the sol into an electrostatic spinning device through an injector for electrostatic spinning to obtain an electrostatic spun fiber sample, calcining the electrostatic spun fiber sample, and naturally cooling to room temperature to obtain the perovskite type moderate-temperature solid oxide fuel cell nanofiber cathode material.
In the electrostatic spinning treatment process, the distance between a needle head in an injector and a collector in an electrostatic spinning device is 15cm, the electrostatic spinning voltage is 18kV, the temperature is 20 ℃, and the relative humidity is 35%.
The inside diameter of the needle in the syringe was 0.6 mm.
The temperature in the calcination process is 950 ℃, and the calcination time is 3 h.
EXAMPLE five
The B site of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the chemical formula of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is YCoxFe1-xO3Wherein x is 0.6, the surface of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell is smooth, and the diameter is 300-400 nm.
The preparation method of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material comprises the following steps:
according to the stoichiometric ratio of nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell, adding Y (NO)3)3·6H2O、Co(NO3)2·6H2O and Fe (NO)3)3·9H2Mixing with dimethyl formamide and polyvinylpyrrolidone, and mixingAnd combining the mixed solution, magnetically stirring the mixed solution uniformly to form uniform and stable dark red sol, putting the sol into an electrostatic spinning device through an injector for electrostatic spinning treatment to obtain an electrostatic spun fiber sample, calcining the electrostatic spun fiber sample, and naturally cooling the fiber sample to room temperature to obtain the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material.
In the electrostatic spinning treatment process, the distance between a needle head in an injector and a collector in an electrostatic spinning device is 15cm, the electrostatic spinning voltage is 18kV, the temperature is 20 ℃, and the relative humidity is 35%.
The inside diameter of the needle in the syringe was 0.6 mm.
The temperature in the calcination process is 950 ℃, and the calcination time is 3 h.
EXAMPLE six
The B site of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the chemical formula of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is YCoxFe1-xO3Wherein x is 0.8, the surface of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell is smooth, and the diameter is 300-400 nm.
The preparation method of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material comprises the following steps:
according to the stoichiometric ratio of nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell, adding Y (NO)3)3·6H2O、Co(NO3)2·6H2O and Fe (NO)3)3·9H2And O, mixing, adding dimethylformamide and polyvinylpyrrolidone, mixing, magnetically stirring uniformly to form uniform and stable dark red sol, putting the sol into an electrostatic spinning device through an injector for electrostatic spinning to obtain an electrostatic spun fiber sample, calcining the electrostatic spun fiber sample, and naturally cooling to room temperature to obtain the perovskite type moderate-temperature solid oxide fuel cell nanofiber cathode material.
In the electrostatic spinning treatment process, the distance between a needle head in an injector and a collector in an electrostatic spinning device is 15cm, the electrostatic spinning voltage is 18kV, the temperature is 20 ℃, and the relative humidity is 35%.
The inside diameter of the needle in the syringe was 0.6 mm.
The temperature in the calcination process is 950 ℃, and the calcination time is 3 h.
Claims (5)
1. The perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is characterized in that the B site of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is doped with Co element and Fe element, and the chemical formula of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is YCoxFe1-xO3Wherein x is more than 0 and less than 1, the surface of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material is smooth, and the diameter is 300-400 nm.
2. A preparation method of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell of claim 1 is characterized by comprising the following steps:
according to the stoichiometric ratio of nano-fiber cathode material of perovskite type intermediate-temperature solid oxide fuel cell, adding Y (NO)3)3·6H2O、Co(NO3)2·6H2O and Fe (NO)3)3·9H2And O, mixing, adding dimethylformamide and polyvinylpyrrolidone, mixing, magnetically stirring uniformly to form uniform and stable dark red sol, putting the sol into an electrostatic spinning device through an injector for electrostatic spinning to obtain an electrostatic spun fiber sample, calcining the electrostatic spun fiber sample, and naturally cooling to room temperature to obtain the perovskite type moderate-temperature solid oxide fuel cell nanofiber cathode material.
3. The preparation method of the perovskite type intermediate-temperature solid oxide fuel cell nanofiber cathode material as claimed in claim 2, wherein in the electrostatic spinning process, the distance between a needle in an injector and a collector in an electrostatic spinning device is 15cm, the electrostatic spinning voltage is 18kV, the temperature is 20 ℃, and the relative humidity is 35%.
4. The preparation method of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell according to claim 2, wherein the inner diameter of a needle in a syringe is 0.6 mm.
5. The preparation method of the nano-fiber cathode material of the perovskite type intermediate-temperature solid oxide fuel cell according to claim 2, wherein the temperature in the calcination process is 950 ℃, and the calcination time is 3 h.
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