CN116387533A - Method for preparing iron-chromium redox flow battery electrode material - Google Patents
Method for preparing iron-chromium redox flow battery electrode material Download PDFInfo
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- CN116387533A CN116387533A CN202211670765.7A CN202211670765A CN116387533A CN 116387533 A CN116387533 A CN 116387533A CN 202211670765 A CN202211670765 A CN 202211670765A CN 116387533 A CN116387533 A CN 116387533A
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- graphite felt
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- 238000000034 method Methods 0.000 title claims abstract description 30
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000007772 electrode material Substances 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 73
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 60
- 239000010439 graphite Substances 0.000 claims abstract description 60
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000004809 Teflon Substances 0.000 claims description 6
- 229920006362 Teflon® Polymers 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- UOFRJXGVFHUJER-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;hydrate Chemical compound [OH-].OCC[NH+](CCO)CCO UOFRJXGVFHUJER-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 102000020897 Formins Human genes 0.000 claims description 2
- 108091022623 Formins Proteins 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000006479 redox reaction Methods 0.000 abstract description 4
- 229910001430 chromium ion Inorganic materials 0.000 abstract description 3
- 239000000835 fiber Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract 1
- 238000010248 power generation Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012983 electrochemical energy storage Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 230000000051 modifying effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000013643 reference control Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007740 vapor deposition 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
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
-
- 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
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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
- H01M4/96—Carbon-based electrodes
-
- 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
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Sustainable Energy (AREA)
- Fuel Cell (AREA)
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Abstract
The invention discloses a method for preparing an electrode material of an iron-chromium redox flow battery, which relates to the technical field of batteries, and specifically relates to a method for preparing an electrode material of an iron-chromium redox flow battery by taking a graphite felt as a matrix material. The triethanolamine hydrothermal reaction can corrode the fiber bundle surface of the graphite felt, increase the specific surface area of the electrode, improve the electrochemical performance of the graphite felt, and improve the electrochemical reversibility of the graphite felt on the redox reaction of chromium ions. The preparation method of the electrode material has the advantages that: the method is convenient and quick, simple in operation, low in price, low in requirements on external environment of preparation and suitable for commercial production of the iron-chromium redox flow battery.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a method for preparing an electrode material of an iron-chromium redox flow battery.
Background
The energy is props and power for civilized development, and the development of solar energy, wind energy and other clean energy power generation is an important way for achieving the goals of carbon peak and carbon neutralization. However, since renewable energy power generation does not have a continuous and stable characteristic, large-scale new energy power generation projects are not suitable for incorporation into the power grid. Therefore, the energy storage technology becomes a key support technology for realizing the large-scale application of new energy. The electrochemical energy storage capacity is large, the response is quick, the electrochemical energy storage is not limited by geographical factors, and sustainable electric energy can be effectively integrated. In large-scale energy storage projects, the lead battery has small capacity and short cycle life, and the lithium battery is inflammable, explosive and unsafe. Therefore, in recent years, it has been proposed to solve the problem of continuous power generation of new energy by using flow batteries. The flow battery system comprises an electrochemical reactor, a liquid storage tank and an electrolyte conveying unit. The system structure separates the power unit from the energy storage unit, decouples the power design and the capacity design, can carry out flexible and large-scale module design, reduces maintenance cost and prolongs the cycle life. In a plurality of flow battery systems, the iron/chromium salt solution adopted by the iron-chromium flow battery is used as a cathode and anode electrolyte, so that the cost is low, the environment is protected, and the maximum commercial prospect is achieved.
In the prior art, graphite felt is often adopted as an electrode material of the iron-chromium redox flow battery because of good chemical stability and good resistance to Fe 2+ /Fe 3+ Has good reactivity and low cost. However, unmodified graphite felt is less hydrophilic to Cr 3+ /Cr 2+ The ions exhibit poor kinetic reversibility of the redox reaction, and oxygen-containing functional groups, such as hydroxyl groups, are typically introduced into the surface of the graphite felt electrode in order to increase its activityRadical, carboxyl, etc., but the modifying effect is general. In recent years, research shows that doping nitrogen atoms on the surface of the graphite felt can provide a pair of lone electron pairs and positively polarize carbon atoms on the fiber bundles, so that the electron absorption rate is accelerated. The existing modification methods for doping nitrogen elements comprise ammonia water treatment, electrochemical vapor deposition, nitrogen-containing particle wrapping and the like, but the methods have the disadvantages of large harm, high cost and complex preparation process, and are not suitable for large-scale commercial use.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing the iron-chromium redox flow battery electrode material, which solves the problems of large harm, high cost, complex preparation process and inapplicability to large-scale commercial use of the methods in the background art.
In order to achieve the above purpose, the invention is realized by the following technical scheme: a method of preparing an iron-chromium redox flow battery electrode material comprising the steps of:
s1, cutting graphite felt into blocks, then placing the blocks in a muffle furnace, introducing air, carrying out high-temperature oxidation treatment for 7-9 hours at 380-420 ℃, wherein the heating rate is 5 ℃ for min -1 Obtaining a graphite felt after heat treatment;
s2, placing the graphite felt after heat treatment into a Teflon liner of a hydrothermal reaction kettle, adding a prepared triethanolamine aqueous solution, completely immersing the graphite felt in the solution, sealing the reaction kettle, placing the sealed reaction kettle in an oven, setting the heating temperature to be 120-210 ℃, continuously heating for 9-11 hours, taking the reaction kettle out of the oven after the reaction is finished, cooling to room temperature, taking out a graphite felt sample, repeatedly flushing the graphite felt with deionized water for 3 times, finally placing the cleaned graphite felt in the oven, and drying for 2-3 hours at the temperature of 120 ℃.
In the invention, in the step S1, the graphite felt is a polyacrylonitrile-based graphite felt, the thickness of the graphite felt is 6mm, and the graphite felt is cut into a rectangular shape with the size of 5cm multiplied by 8 cm.
In the present invention, in S1, the heat-treated graphite felt is divided into two parts, one part is used as a reference (GF) of the graphite felt, and the other part is subjected to triethanolamine hydrothermal modification.
In the present invention, in the step S2, the aqueous solution of triethylamine alcohol is prepared by the following steps:
s21, accurately weighing 10.5g of triethanolamine liquid;
s22, adding triethanolamine liquid into 94.5g deionized water to prepare 10% triethanolamine water solution;
s23, fully stirring the mixture on a magnetic stirrer for 10-12 minutes.
In the invention, in the step S2, different heating temperatures of the oven outside the reaction kettle are set to obtain modified graphite felt samples under different hydrothermal reaction temperature conditions, wherein the set heating temperatures are 120 ℃, 150 ℃, 180 ℃ and 210 ℃.
In the present invention, the modified graphite felt sample with the heating temperature of 120 ℃ is recorded as N-GF120; the modified graphite felt sample with the heating temperature of 150 ℃ is recorded as N-GF150; the modified graphite felt sample with the heating temperature of 180 ℃ is recorded as N-GF180; the modified graphite felt sample with a heating temperature of 210 ℃ was designated as N-GF210.
The invention provides a method for preparing an iron-chromium redox flow battery electrode material, which has the following beneficial effects:
according to the method for preparing the iron-chromium redox flow battery electrode material, fiber bundles on the surface of the graphite felt are corroded through a high-temperature oxidation and low-temperature triethanolamine hydrothermal reaction method, and nitrogen-containing functional groups are doped on the surface of the graphite felt while the specific surface area of the electrode is increased. The inorganic nitrogen atoms can provide lone electron pairs, and when the chromium ion redox pair generates redox reaction on the surface of the graphite felt, the electron conduction rate can be accelerated, so that the electrochemical performance of the graphite felt is improved, and the electrochemical reversibility of the graphite felt on the redox reaction of chromium ions is improved. The preparation method is convenient and quick, simple to operate, low in cost and low in requirements on external environment of preparation, and is suitable for commercial production of the iron-chromium redox flow battery.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Referring to fig. 1, the present invention provides a technical solution: a method for preparing an electrode material of an iron-chromium redox flow battery, which comprises the following steps:
example 1:
the high-temperature graphite oxide felt is prepared by the following steps:
cutting 5 graphite felts with the thickness of 6mm into rectangular shapes with the size of 5cm multiplied by 8cm, placing the graphite felts in a muffle furnace, introducing air, carrying out high-temperature oxidation treatment for 8 hours at the temperature of 400 ℃, and obtaining the graphite felts after heat treatment at the temperature rising rate of 5 ℃/min. Of these, 1 graphite felt was used as a reference control (noted GF) and the remaining graphite felt was subjected to triethanolamine hydrothermal modification.
Example 2:
the 10% triethanolamine aqueous solution is prepared by the following steps:
10.5g of triethanolamine liquid was precisely weighed, added to 94.5g of deionized water to prepare a 10% aqueous solution of triethanolamine, and stirred well on a magnetic stirrer for 10 minutes.
Example 3:
a method of preparing an iron-chromium redox flow battery electrode material comprising the steps of:
placing a piece of graphite felt after heat treatment into a Teflon liner of a hydrothermal reaction kettle, adding the prepared 10% triethanolamine aqueous solution, completely immersing the graphite felt in the solution, and sealing the reaction kettle. And placing the sealed reaction kettle in an oven, and setting the heating temperature of the oven to 120 ℃ for heating for 10 hours. And taking the reaction kettle out of the oven after the reaction is finished, cooling to room temperature, taking out a graphite felt sample, and repeatedly flushing with deionized water for 3 times. Finally, the cleaned graphite felt was placed in an oven and dried at 120 ℃ for 2 hours, and the prepared sample was designated as N-GF120.
Example 4:
a method of preparing an iron-chromium redox flow battery electrode material comprising the steps of:
placing a piece of graphite felt after heat treatment into a Teflon liner of a hydrothermal reaction kettle, adding the prepared 10% triethanolamine aqueous solution, completely immersing the graphite felt in the solution, and sealing the reaction kettle. And placing the sealed reaction kettle in an oven, and setting the heating temperature of the oven to 150 ℃ for heating for 10 hours. And taking the reaction kettle out of the oven after the reaction is finished, cooling to room temperature, taking out a graphite felt sample, and repeatedly flushing with deionized water for 3 times. Finally, the cleaned graphite felt was placed in an oven and dried at 120 ℃ for 2 hours, and the prepared sample was designated as N-GF150.
Example 5:
a method of preparing an iron-chromium redox flow battery electrode material comprising the steps of:
placing a piece of graphite felt after heat treatment into a Teflon liner of a hydrothermal reaction kettle, adding the prepared 10% triethanolamine aqueous solution, completely immersing the graphite felt in the solution, and sealing the reaction kettle. And placing the sealed reaction kettle in an oven, and setting the heating temperature of the oven to 180 ℃ for heating for 10 hours. And taking the reaction kettle out of the oven after the reaction is finished, cooling to room temperature, taking out a graphite felt sample, and repeatedly flushing with deionized water for 3 times. Finally, the cleaned graphite felt was placed in an oven and dried at 120 ℃ for 2 hours, and the prepared sample was designated as N-GF180.
Example 6:
a method of preparing an iron-chromium redox flow battery electrode material comprising the steps of:
placing a piece of graphite felt after heat treatment into a Teflon liner of a hydrothermal reaction kettle, adding the prepared 10% triethanolamine aqueous solution, completely immersing the graphite felt in the solution, and sealing the reaction kettle. And placing the sealed reaction kettle in an oven, and setting the heating temperature of the oven to 210 ℃ for heating for 10 hours. And taking the reaction kettle out of the oven after the reaction is finished, cooling to room temperature, taking out a graphite felt sample, and repeatedly flushing with deionized water for 3 times. Finally, the cleaned graphite felt was placed in an oven and dried at 120 ℃ for 2 hours, and the prepared sample was designated as N-GF210.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. A method for preparing an electrode material of an iron-chromium redox flow battery, which is characterized by comprising the following steps: the method comprises the following steps:
s1, cutting graphite felt into blocks, then placing the blocks in a muffle furnace, introducing air, carrying out high-temperature oxidation treatment for 7-9 hours at 380-420 ℃, wherein the heating rate is 5 ℃ for min -1 Obtaining a graphite felt after heat treatment;
s2, placing the graphite felt after heat treatment into a Teflon liner of a hydrothermal reaction kettle, adding a prepared triethanolamine aqueous solution, completely immersing the graphite felt in the solution, sealing the reaction kettle, placing the sealed reaction kettle in an oven, setting the heating temperature to be 120-210 ℃, continuously heating for 9-11 hours, taking the reaction kettle out of the oven after the reaction is finished, cooling to room temperature, taking out a graphite felt sample, repeatedly flushing the graphite felt with deionized water for 3 times, finally placing the cleaned graphite felt in the oven, and drying for 2-3 hours at the temperature of 120 ℃.
2. The method for preparing the iron-chromium redox flow battery electrode material according to claim 1, wherein the method comprises the following steps: in the step S1, the graphite felt is a polyacrylonitrile-based graphite felt, the thickness of the graphite felt is 6mm, and the graphite felt is cut into rectangular shapes with the size of 5cm multiplied by 8 cm.
3. The method for preparing the iron-chromium redox flow battery electrode material according to claim 1, wherein the method comprises the following steps: in the step S1, the graphite felt after heat treatment is divided into two parts, one part is used as a reference comparison item (marked as GF) of the graphite felt, and the other part is subjected to triethanolamine hydrothermal modification.
4. The method for preparing the iron-chromium redox flow battery electrode material according to claim 1, wherein the method comprises the following steps: in the step S2, the triethylamine alcohol aqueous solution is prepared by the following steps:
s21, accurately weighing 10.5g of triethanolamine liquid;
s22, adding triethanolamine liquid into 94.5g deionized water to prepare 10% triethanolamine water solution;
s23, fully stirring the mixture on a magnetic stirrer for 10-12 minutes.
5. The method for preparing the iron-chromium redox flow battery electrode material according to claim 1, wherein the method comprises the following steps: in the step S2, different heating temperatures of the oven outside the reaction kettle are set to obtain modified graphite felt samples under different hydrothermal reaction temperature conditions, wherein the set heating temperatures are 120 ℃, 150 ℃, 180 ℃ and 210 ℃.
6. The method for preparing the iron-chromium redox flow battery electrode material according to claim 5, wherein the method comprises the following steps: the modified graphite felt sample with the heating temperature of 120 ℃ is recorded as N-GF120; the modified graphite felt sample with the heating temperature of 150 ℃ is recorded as N-GF150; the modified graphite felt sample with the heating temperature of 180 ℃ is recorded as N-GF180; the modified graphite felt sample with a heating temperature of 210 ℃ was designated as N-GF210.
7. An iron chromium redox flow battery electrode material prepared by the preparation method of any one of claims 1-6.
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