CN115911421A - SFM-based electrode material of hydrogen energy fuel cell and preparation method thereof - Google Patents
SFM-based electrode material of hydrogen energy fuel cell and preparation method thereof Download PDFInfo
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention discloses an electrode material of an SFM-based hydrogen energy fuel cell, wherein the chemical formula of the electrolyte material is Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6‑δ . The invention also discloses a preparation method of the electrode material of the SFM-based hydrogen energy fuel cell. The invention adopts Ti element to react with Sr 2 Fe 1.5 Mo 0.5 O 6‑δ Mo element at the B position of the material is doped and substituted, and the obtained electrode material of the SFM-based hydrogen energy fuel cell has high conductivity at medium temperature, and is a good medium-temperature SOFCs electrode material.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to an SFM-based hydrogen energy fuel cell electrode material and a preparation method thereof.
Background
As a new green energy technology developed in recent years, a Solid Oxide Fuel Cell (SOFC) is used as a third-generation product of fuel cell development, and has the advantages of excellent corrosion resistance, higher energy replacement efficiency, environmental protection, high density, strong adaptability, long service life of the cell and the like, and the advantages undoubtedly arouse the attention of a great number of researchers and countries related to the aspect. From the current form, the SOFC is widely used in various fields such as power generation, thermoelectric recycling, traffic, space navigation and other fields, and is known as a green energy source in the 21 st century by people. Conventional SOFCs are usually operated at high temperature, however, too high operating temperature causes a series of complicated problems, such as sintering of electrodes, interfacial diffusion of electrode materials and electrolyte, etc., which undoubtedly greatly increase the difficulty of commercialization of SOFCs. In recent years, the focus of SOFC technology development has focused primarily on improving electrochemical performance and improving operating temperatures.
SFM is an electrode material widely studied and searched by people, and as a perovskite-type electrode, SFM shows very excellent electrical properties due to the Fe element and the Mo element, but the preparation conditions are severe, and a pure-phase material can be synthesized only in a reducing atmosphere, so Chen et al research a chemical formula of Sr 2 Fe 1.5 Mo 0.5 O 6-δ The electrode material of (1). The ratio of Fe/Mo element in SFM causes electron deletion and oxygen hole generation, so that the material shows good electron transport capability and high catalytic activity under both oxidizing condition and reducing condition. On the basis, an SFM-based hydrogen energy fuel cell electrode material with better electrochemical performance is yet to be developed, and the application of the electrode material in the field of fuel cells is further promoted.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of an electrode material of an SFM-based hydrogen energy fuel cell.
The invention provides an SFM-based electrode material for a hydrogen energy fuel cell, which has a chemical formula of Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ 。
In the formula, delta is the metering number of Sr, fe, mo and Ti elements, and the specific numerical value can be calculated according to the charge balance.
The preparation method of the electrode material of the SFM-based hydrogen energy fuel cell comprises the following steps:
s1, sr according to the stoichiometric ratio 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ Weighing Sr salt, fe salt, mo salt and TiO 2 Adding into water, stirring, adding complexing agent, heating, stirring, reacting, oven drying the obtained gel, grinding, calcining at high temperature, and cooling to obtain Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ Powder;
s2, adding the Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ And mixing the powder with a binder, uniformly grinding, and then performing compression molding and high-temperature sintering to obtain the powder.
Preferably, the Sr salt is Sr (NO) 3 ) 2 The Fe salt is Fe (NO) 3 ) 3 ·9H 2 O, mo salt is (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O。
Preferably, the complexing agent is citric acid, and the dosage of the complexing agent is 1.5 times of the sum of the mole numbers of Sr ions, fe ions, mo ions and Ti ions.
Preferably, in S1, the temperature for heating and stirring reaction is 60-90 ℃ and the time is 7-8h.
Preferably, in S1, the high-temperature calcination is carried out at 850-1050 ℃ for 4-5h.
Preferably, in S2, the pressure for compression molding is 8-15MPa.
Preferably, in S2, the temperature for high-temperature sintering is 1100-1350 ℃ and the time is 2-6h.
Preferably, in S2, the binder is a PVA solution with the mass fraction of 5-20%.
Preferably, in S2, the mass of the binder is equivalent to Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ 5-25% of the mass of the powder.
An SFM-based electrode material of a hydrogen energy fuel cell, which is prepared by the preparation method.
The invention has the following beneficial effects:
the invention adopts Ti element to add Sr at proper proportion 2 Fe 1.5 Mo 0.5 O 6-δ The B-site Mo element of the material is doped and substituted, and the obtained SFM-based hydrogen energy fuel cell electrode material has high conductivity at the intermediate temperature, and is a good intermediate-temperature SOFCs electrode material.
Drawings
Fig. 1 is an XRD spectrum of the SFM-based hydrogen fuel cell electrode material prepared in example 1.
Fig. 2 is an SEM image of the SFM-based hydrogen fuel cell electrode material prepared in example 1.
Fig. 3 is a graph of the electrical conductivity of the SFM-based hydrogen fuel cell electrode material prepared in example 1 at 400-800 c in an air atmosphere.
Fig. 4 is an Arrhenius curve of the SFM-based hydrogen energy fuel cell electrode material prepared in example 1 as a function of temperature.
Fig. 5 is an electrochemical impedance spectrum of the SFM-based hydrogen fuel cell electrode material prepared in example 1 at 800 ℃.
FIG. 6 shows the chemical formula Sr obtained in example 1 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ Thermogravimetric analysis of the electrode material of the SFM-based hydrogen energy fuel cell at 50-600 ℃.
FIG. 7 is a graph of the conductivity of SFCuM prepared in comparative example 1 at 400-800 deg.C in an air atmosphere.
Fig. 8 is a graph of the conductivity of SFSnM prepared in comparative example 2 at 400-800 c under an air atmosphere.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
Preparing an electrode material (SFMTi) of the SFM-based hydrogen energy fuel cell:
s1, sr in stoichiometric ratio 2 Fe 1.5 Mo 0.5-x Ti x O 6-δ Weighing Sr (NO) 3 ) 2 、Fe(NO 3 ) 3 ·9H 2 O、 (NH 4 ) 6 Mo 7 O 24 ·4H 2 O and TiO 2 Adding 100mL of water, stirring uniformly, adding citric acid 1.5 times of the sum of the molar numbers of Sr ions, fe ions, mo ions and Ti ions, heating and stirring at 80 ℃ for reaction for 8h, drying the obtained gel after the reaction is finished, grinding uniformly, calcining at 1000 ℃ for 5h, and cooling to obtain Sr 2 Fe 1.5 Mo 0.5-x Ti x O 6-δ Powder;
wherein, sr (NO) 3 ) 2 Ratio to water 4.236g:200mL;
s2, adding Sr 2 Fe 1.5 Mo 0.5-x Ti x O 6-δ Mixing the powder with 5% PVA solution, grinding, and pressing under 12MPa to obtain the final product with a diameter of
Sintering the biscuit piece at the high temperature of 1200 ℃ for 3h to obtain the chemical formula Sr 2 Fe 1.5 Mo 0.5-x Ti x O 6-δ The SFM-based hydrogen energy fuel cell electrode material (SFMTi) of (1), wherein the mass of the PVA solution is equivalent to Sr 2 Fe 1.5 Mo 0.5-x Ti x O 6-δ 25% of the mass of the powder. />
In S1, x =0.05, 0.1, 0.15, 0.2, respectively, was taken to give Sr of the formula 2 Fe 1.5 Mo 0.45 Ti 0.05 O 6-δ 、Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ 、Sr 2 Fe 1.5 Mo 0.35 Ti 0.15 O 6-δ 、 Sr 2 Fe 1.5 Mo 0.3 Ti 0.2 O 6-δ The SFM-based hydrogen energy fuel cell electrode material of (1).
FIG. 1 is an XRD spectrum of the electrode material of the SFM-based hydrogen energy fuel cell prepared as described above. As can be seen from fig. 1, the Ti-doped material has no hetero-peak and has the same crystal phase structure as the SFM material, which indicates that the Ti doping does not affect the self-phase structure of the SFM material.
Fig. 2 is an SEM image of the SFM-based hydrogen fuel cell electrode material prepared as described above. Wherein, fig. 2 (a) represents the SFM-based hydrogen energy fuel cell electrode material of x =0.05, fig. 2 (b) represents the SFM-based hydrogen energy fuel cell electrode material of x =0.1, fig. 2 (c) represents the SFM-based hydrogen energy fuel cell electrode material of x =0.15, and fig. 2 (d) represents the SFM-based hydrogen energy fuel cell electrode material of x = 0.2. As can be seen from fig. 2, the material is polygonal, irregularly shaped, plate-like, with particle sizes of hundreds of nanometers to microns. The particle shapes of the electrode materials of the four-component SFM-based hydrogen energy fuel cells are approximately the same, and the grain boundaries are obvious. When the Ti content is 0.05 and 0.1, the surface of the material is slightly convex, and when the Ti content is 0.15 and 0.2, the surface is smooth, the combination among particles is very tight, and the compactness of the material can be seen.
FIG. 3 is a graph of the conductivity of the electrode material of the SFM-based hydrogen energy fuel cell prepared as described above at 400-800 ℃ in an air atmosphere. It can be seen from the figure that the conductivity of the electrode ceramic sheet increases with increasing temperature, but wherein the conductivity does not change significantly with temperature when Ti =0.05, the change in temperature does not significantly affect the change in conductivity.
Table 1 shows the electrical conductivity of the SFM-based hydrogen fuel cell electrode material prepared as described above at 800 ℃ in an air atmosphere.
TABLE 1
| Sr 2 Fe 1.5 Mo 0.5-x Ti x O 6-δ | x＝o.o5 | x＝0.1 | x＝0.15 | x＝0.2 |
| Conductivity (Scm) -1 ) | 0.134 | 0.223 | 0.132 | 0.157 |
As can be seen from the results of the experiments in conjunction with FIG. 3 and Table 1, sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ The highest conductivity of the electrode material in the air atmosphere reaches 0.223S cm -1 . However, as the Ti content continues to increase, the conductivity decreases, from which Ti can be learned +4 The doping amount directly affects the contents of Mo ions and Fe ions at the B site in SFMTi. The presence of Fe in the SFM material 3+ +Mo 5+ →Fe 2+ +Mo 6+ Such an equilibrium reaction, ti 4+ Directly influence Fe 2+ 、Fe 3+ 、Mo 6+ And Mo 5+ The content of these ions allows the reaction to reach a new equilibrium, which in turn directly determines whether the electronic conductivity of the material is increasing or decreasing. It can be seen that when x =0.1, sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ The material with the highest conductivity far exceeds the other three components, and through analysis, sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ The higher conductivity relative to other materials may be due to the fact that when Ti takes 0.1, fe is made 2+ /Fe 3+ Ratio of (A) to Mo 6+ /Mo 5+ Is more favorable for
The dynamic balance of the reaction is more favorable for proceeding the balance, thereby improving the electronic conductivity.
Fig. 4 is an Arrhenius curve of the SFM-based hydrogen energy fuel cell electrode material prepared as described above as a function of temperature. As can be seen from fig. 4, the four curves are approximated to a straight line with a negative slope, and it can be seen from equation 4.1 that the change of the activation energy is only related to the temperature, and the change of the activation energy is large with the temperature.
According to the formula:
LnT/R＝LnA-E/KT
wherein R-polarization resistance; a-denotes a pre-factor; e-reaction activation energy (eV); K-Boltzmann constant, 1.38X 10-23J K -1 ；
Calculated to obtain the chemical formula of Sr 2 Fe 1.5 Mo 0.45 Ti 0.05 O 6-δ 、Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ 、 Sr 2 Fe 1.5 Mo 0.35 Ti 0.15 O 6-δ 、Sr 2 Fe 1.5 Mo 0.3 Ti 0.2 O 6-δ The activation energies of the SFM-based hydrogen fuel cell electrode materials of (a) are 1.174, 1.155, 1.170 and 1.171eV, respectively.
FIG. 5 is an electrochemical impedance spectrum of the electrode material of the SFM-based hydrogen fuel cell prepared as described above at 800 ℃, using R (QR) H )(QR L ) Is an equivalent circuit. R represents the resistance caused by the electrolyte, the electrode and the lead, and is ohmic resistance; r is H I.e. the difference between the intercepts of the high frequency arc on the real axis, corresponding to the charge transfer resistance, R, of the cathode/electrolyte interface L I.e. the intercept difference of the low-frequency arc on the real axis, representing the diffusion of the gas in the cathode and the resistance of adsorption, the polarization resistance R of the cathode material is equal to the electrode surface diffusion resistance (R) H ) And a charge transfer resistance (R) L ) Sum, i.e. R = R H +R L 。
Table 2 shows the parameters of the SFM-based hydrogen fuel cell electrode material prepared as described above, which was fitted by an electrochemical impedance meter at 800 ℃.
TABLE 2
As can be seen from FIG. 5 and Table 2, the SFMTi electrode material has a low frequency region impedance R at both low and high temperatures L Predominating, and high frequency region R H Occupies a small part, indicates O 2- The cathode diffusion and dissociation processes are controlled by the cathode ORR reaction, which is typically associated with a three-phase interface (TPB) at high frequencies in an electrochemical process. R of SFMTi when Ti =0.1 H ＝0.556Ωcm 2 R lower than other contents of SFMTi H Values indicating that the content of Ti =0.1 in the material significantly improves charge transfer kinetics.
FIG. 6 shows that Sr is a chemical formula obtained as described above 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ Thermogravimetric analysis of the electrode material of the SFM-based hydrogen energy fuel cell at 50-600 ℃. As can be seen from the figure, the TG curve is kept stable with the continuous change of the temperature, which shows that the sample has no loss of quality in the temperature rising process, so that the thermal stability of the sample can be estimated to be better. DTA is a stable substance (reference) that does not undergo any chemical reaction or physical change at a given experimental temperature, as compared to an equivalent amount of an unknown at constant temperature in the same environment, and any physical or chemical change in the unknown is temporarily increased or decreased as compared to the temperature of a standard in the same environment. It can be seen from the figure that below 400 ℃ the curve decreases, showing an endothermic reaction, and after 400 ℃ the curve increases, showing an exothermic reaction. The chemical heating effect of the sample was generally seen to be good.
Comparative example 1
Preparing an electrode material (SFCuM) of the SFM-based hydrogen energy fuel cell:
s1, sr in stoichiometric ratio 2 Fe 1.4 Cu 0.1 Mo 0.5 O 6-δ Weighing Sr (NO) 3 ) 2 、Fe(NO 3 ) 3 ·9H 2 O、 (NH 4 ) 6 Mo 7 O 24 ·4H 2 O and Cu (NO) 3 ) 2 · 3 H 2 Adding O into 200mL of water, fully and uniformly stirring, then adding ammonia water to adjust the pH value to 6-7, then adding citric acid which is 1.5 times of the sum of the mole numbers of Sr ions, fe ions, mo ions and Cu ions, heating and stirring at 80 ℃ to react for 8h, drying and uniformly grinding the obtained gel after the reaction is finished, calcining at 1000 ℃ for 5h, and cooling to obtain Sr 2 Fe 1.4 Cu 0.1 Mo 0.5 O 6-δ Powder;
wherein, sr (NO) 3 ) 2 Ratio to water 4.236g:200mL;
s2, adding Sr 2 Fe 1.4 Cu 0.1 Mo 0.5 O 6-δ Mixing the powder with 5% PVA solution, grinding, and pressing under 12MPa to obtain the final product with diameter of
Sintering the biscuit piece at the high temperature of 1200 ℃ for 3 hours to obtain the chemical formula Sr 2 Fe 1.4 Cu 0.1 Mo 0.5 O 6-δ The SFM-based electrode material (SFCuM) for hydrogen fuel cells, wherein the mass of the PVA solution is equivalent to Sr 2 Fe 1.4 Cu 0.1 Mo 0.5 O 6-δ 25% of the mass of the powder.
Comparative example 2
Preparing an electrode material (SFSnM) of an SFM-based hydrogen energy fuel cell:
s1, sr in stoichiometric ratio 2 Fe 1.4 Sn 0.1 Mo 0.5 O 6-δ Weighing Sr (NO) 3 ) 2 、Fe(NO 3 ) 3 ·9H 2 O、 (NH 4 ) 6 Mo 7 O 24 ·4H 2 O and Sn (NO) 3 ) 4 Adding 200mL of water, fully and uniformly stirring, then adding ammonia water to adjust the pH value to 6-7, then adding citric acid which is 1.5 times of the sum of the mole numbers of Sr ions, fe ions, mo ions and Sn ions, heating and stirring at 80 ℃ to react for 8h, drying and uniformly grinding the obtained gel after the reaction is finished, calcining at 1000 ℃ for 5h, and cooling to obtain Sr 2 Fe 1.4 Sn 0.1 Mo 0.5 O 6-δ A powder;
wherein, sr (NO) 3 ) 2 Ratio to water 4.236g:200mL;
s2, adding Sr 2 Fe 1.4 Sn 0.1 Mo 0.5 O 6-δ Mixing the powder with 5% PVA solution, grinding, and pressing under 12MPa to obtain the final product with diameter of
Sintering the biscuit piece at the high temperature of 1200 ℃ for 3h to obtain the chemical formula Sr 2 Fe 1.4 Sn 0.1 Mo 0.5 O 6-δ The SFM-based hydrogen energy fuel cell electrode material (SFSnM) of (1), wherein the mass of the PVA solution is equivalent to Sr 2 Fe 1.4 Sn 0.1 Mo 0.5 O 6-δ 25% of the mass of the powder.
The conductivity tests were performed on the sfcums and the sfsnms prepared in comparative example 1 and comparative example 2, respectively, and the test results are shown in fig. 7 to 8. Wherein fig. 7 is a conductivity test result of SFCuM, and fig. 8 is a conductivity test result of SFSnM. The test result shows that the conductivity of the SFSnM is highest at 800 ℃ and is 0.187Scm -1 (ii) a The conductivity of SFCuM increases with temperature, and at 400 ℃ the conductivity is 0.129S cm -1 And an electrical conductivity of 0.157S cm at 800 deg.C -1 . Whereas the conductivity of the undoped SFM material at 800 ℃ is only 0.092Scm -1 。
Therefore, compared with the electrode material doped with Sn and Cu elements and undoped SFM, the conductivity of the electrode material is obviously improved, and the electrode material is an intermediate-temperature SOFCs electrode material with excellent performance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. An electrode material of an SFM-based hydrogen energy fuel cell, which is characterized in that the chemical formula of the electrode material is Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ 。
2. A method of making the SFM-based hydrogen fuel cell electrode material of claim 1, comprising the steps of:
s1, sr in stoichiometric ratio 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ Weighing Sr salt, fe salt, mo salt and TiO 2 Adding into water, stirring, adding complexing agent, heating, stirring, reacting, oven drying the obtained gel, grinding, calcining at high temperature, and cooling to obtain Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ Powder;
s2, adding Sr 2 Fe 1.5 Mo 0.4 Ti 0.1 O 6-δ And mixing the powder with a binder, uniformly grinding, and then performing compression molding and high-temperature sintering to obtain the powder.
3. The method for preparing an SFM-based hydrogen energy fuel cell electrode material as defined in claim 2, wherein the Sr salt is Sr (NO) 3 ) 2 The Fe salt is Fe (NO) 3 ) 3 ·9H 2 O, mo salt is (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O。
4. The preparation method of the SFM-based hydrogen energy fuel cell electrode material as claimed in claim 2, wherein the complexing agent is citric acid, and the dosage of the complexing agent is 1.5 times of the sum of moles of Sr ions, fe ions, mo ions and Ti ions.
5. The preparation method of the SFM-based hydrogen energy fuel cell electrode material as claimed in claim 2, wherein the temperature of the heating stirring reaction in S1 is 60-90 ℃ and the time is 7-8h.
6. The preparation method of the SFM-based hydrogen energy fuel cell electrode material as claimed in claim 2, wherein the high-temperature calcination in S1 is carried out at 850-1050 ℃ for 4-5h.
7. The method for preparing an SFM-based hydrogen fuel cell electrode material according to claim 2, wherein in S2, the pressure for press forming is 8 to 15MPa.
8. The method for preparing the electrode material of the SFM-based hydrogen energy fuel cell as claimed in claim 2, wherein the temperature of the high-temperature sintering in S2 is 1100-1350 ℃ and the time is 2-6h.
9. An electrode material for an SFM-based hydrogen fuel cell, characterized by being produced by the production method according to any one of claims 2 to 8.
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| CN113299934A (en) * | 2021-05-13 | 2021-08-24 | 中国科学技术大学 | Anti-carbon deposition and carbon dioxide resistant fuel electrode material, preparation method thereof and solid oxide cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113299934A (en) * | 2021-05-13 | 2021-08-24 | 中国科学技术大学 | Anti-carbon deposition and carbon dioxide resistant fuel electrode material, preparation method thereof and solid oxide cell |
Non-Patent Citations (1)
| Title |
|---|
| CHUNMING XU ET AL.: "Co-improving the electrocatalytic performance and H2S tolerance of a Sr2Fe1.5Mo0.4O6-δ based anode for solid oxide fuel cells", 《J. MATER. CHEM. A》, 21 July 2022 (2022-07-21), pages 1 - 2 * |
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