CN111725003A - Cubic iron-based oxyhydroxide/graphene composite material for supercapacitor and preparation method thereof - Google Patents
Cubic iron-based oxyhydroxide/graphene composite material for supercapacitor and preparation method thereof Download PDFInfo
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- CN111725003A CN111725003A CN202010661039.3A CN202010661039A CN111725003A CN 111725003 A CN111725003 A CN 111725003A CN 202010661039 A CN202010661039 A CN 202010661039A CN 111725003 A CN111725003 A CN 111725003A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 74
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 41
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000007832 Na2SO4 Substances 0.000 claims abstract description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 9
- 238000000967 suction filtration Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 16
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 abstract description 11
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 abstract description 11
- 239000007772 electrode material Substances 0.000 abstract description 6
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 239000003990 capacitor Substances 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 238000006479 redox reaction Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000001351 cycling effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000013329 compounding Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- 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
- Y02E60/13—Energy storage using capacitors
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Abstract
A cubic iron-based oxyhydroxide/graphene composite material for a supercapacitor and a preparation method thereof belong to the technical field of electrode materials. The cubic iron-based oxyhydroxide/graphene composite material has the size of 360-540 nm, and the electrochemical specific capacity of 596-688F/g. The preparation method comprises the following steps: firstly, weighing a certain amount of metallic iron source and Na2SO4Adding GO into a 100mL beaker, adding a certain amount of deionized water, magnetically stirring, placing into an oven for reaction at a certain temperature for a period of time, cooling to room temperature, and then performing suction filtration and washing with deionized waterWashing to neutrality, and freeze drying to obtain the product. The cubic iron-based oxyhydroxide/graphene composite material has the characteristics of simple preparation method and low cost, the graphene induces the formation of uniform cubic iron oxyhydroxide, realizes the synergistic effect of the cubic iron oxyhydroxide and the graphene, and combines the advantages of high specific capacity and good conductivity of the cubic iron oxyhydroxide and the graphene.
Description
Technical Field
The invention relates to a cubic iron-based oxyhydroxide/graphene composite material for a supercapacitor and a preparation method thereof, belonging to the technical field of electrode materials.
Background
Along with the rapid development of the current high-energy-consumption industry, the traditional battery can not meet the requirements of people, and the super capacitor is a novel energy storage device between the traditional capacitor and a rechargeable battery, has excellent electrochemical performance and cycling stability, and is divided into a double electric layer capacitor and a pseudo capacitor. Among them, the pseudocapacitance capacitor can generate oxidation-reduction reaction, so that it has higher specific capacity and energy density. The performance of supercapacitors is closely related to the structure and chemical composition of the electrode material. The transition metal oxyhydroxide can rapidly carry out redox reaction due to the multi-valence state and the unique crystal structure of metal ions, and has good electrochemical performance. Among them, iron has various valence states, can undergo rich redox reactions, and has attracted extensive attention due to its advantages of high theoretical specific capacity, abundant resources, low price, environmental friendliness, etc. In 2008, gold et al was first in Li2SO4In the solution, iron oxyhydroxide was used as a negative electrode material, and the capacitance characteristics thereof were investigated. However, iron oxyhydroxide as an electrode material has problems of poor conductivity and electrochemical instability, which seriously hinders its application in supercapacitors.
In order to solve the problems, the hydroxyl iron oxide and the graphene are combined, the introduction of the graphene can induce the formation and the uniform dispersion of the hydroxyl iron oxide, and a good synergistic effect can be formed between the hydroxyl iron oxide and the graphene, so that the problem of low specific capacity of the graphene is solved, and the conductivity of the hydroxyl iron oxide can be further improved. The prepared material can exert the advantages of the two materials in a centralized manner and simultaneously make up the respective defects, so that the synergistic effect is perfectly exerted, and the electrochemical performance is improved. At present, most of the iron oxyhydroxide/graphene composite materials prepared by the method are sheet-shaped structures, for example, Yue et al synthesize sheet-shaped FeOOH/EAGFs composite materials by an electrodeposition method, and have good electrochemical performance and cycling stability (J.colloid Interf.Sci.2020,560, 237-246). The cubic structure has a regular shape and smaller particle size, can provide more active sites, performs redox reaction, and has great advantages in energy storage application. However, the method for preparing the three-dimensional cubic iron oxyhydroxide/graphene composite material under the mild condition is less, the simple one-step hydrothermal synthesis strategy is adopted, the uniformly dispersed cubic iron-based oxyhydroxide/graphene composite material is very important, and the cubic iron oxyhydroxide and graphene have good synergistic effect, so that the cubic iron oxyhydroxide/graphene composite material has wide application prospect as the electrode material of the supercapacitor.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a cubic iron-based oxyhydroxide/graphene composite material capable of being used as a supercapacitor electrode material and a preparation method thereof. The material has good electrochemical performance and cycling stability, and the preparation method is simple and controllable, and has wide application prospect.
In order to achieve the technical purpose, the invention adopts the technical scheme that:
a preparation method of a cubic iron-based oxyhydroxide/graphene composite material for a supercapacitor comprises the step of adding a certain amount of metallic iron source and Na2SO4And GO is dissolved in a certain amount of deionized water, the reaction is carried out for a period of time at a certain temperature, and the cubic iron-based oxyhydroxide/graphene composite material is obtained after washing to be neutral and drying. The method comprises the following specific steps:
at room temperature, adding metallic iron source and Na2SO4And GO is placed in a beaker, and then deionized water is added, wherein 120-720 mg of Na is correspondingly added into every 20-40 mL of deionized water2SO4(ii) a And (2) magnetically stirring for 10 minutes, transferring the mixture into 50mL of polytetrafluoroethylene, putting the polytetrafluoroethylene into an oven, reacting for 4-12 hours at the temperature of 100-160 ℃, cooling to room temperature, performing suction filtration and washing by using deionized water until the mixture is neutral, and performing freeze drying to obtain the cubic iron-based oxyhydroxide/graphene composite material with the size of 360-540 nm.
The metallic iron source is ferric chloride, ferric nitrate and ferric sulfate. Said Na2SO4The mass ratio of the metal iron source to the metal iron source is 1: 3-8: 5; said Na2SO4The mass ratio of the carbon to GO is 3.2: 1-16: 1. The freeze drying time is 10-15 h.
The cubic iron-based oxyhydroxide/graphene composite material for the supercapacitor prepared by the method has the specific capacitance of 596-688F/g and the rate capability of 63-72.2%.
The invention has the beneficial effects that: 1) the preparation method is simple and low in cost; 2) the introduction of the graphene can induce the formation and uniform dispersion of cubic iron oxyhydroxide; 3) the cubic iron oxyhydroxide and the graphene have a good synergistic effect, and high specific capacity and good conductivity are realized.
Drawings
Fig. 1 is an SEM image of a cubic iron-based oxyhydroxide/graphene composite material in example 3.
Fig. 2 is an SEM image of a cubic iron-based oxyhydroxide/graphene composite material in example 4.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
Example 1
Weighing 360mg of ferric sulfate and 120mg of Na2SO4And 30mg of GO in a 100mL beaker, then adding 30mL of deionized water, magnetically stirring for 10 minutes, transferring the mixture into 50mL of polytetrafluoroethylene, putting the polytetrafluoroethylene into an oven for reaction at 100 ℃ for 10 hours, cooling to room temperature, and then performing suction filtration and washing by using deionized water until the temperature is reduced to room temperatureAnd (4) neutralizing, and treating for 12h by using a freeze dryer to obtain the cubic iron-based oxyhydroxide/graphene composite material. The electrochemical specific capacity of the material is tested in a three-electrode system with 6M KOH as electrolyte, and finally under the constant current condition of 0.5A/g, the specific capacitance is 643F/g, 418F/g can be achieved at 10A/g, and the multiplying power is kept at 65%.
Example 2
540mg of ferric nitrate and 720mg of Na were weighed2SO4And 90mg of GO is placed in a 100mL beaker, then 40mL of deionized water is added, magnetic stirring is carried out for 10 minutes, the mixture is transferred into 50mL of polytetrafluoroethylene, the polytetrafluoroethylene is placed in an oven for reaction at 140 ℃ for 4 hours, the deionized water is used for suction filtration and washing to be neutral after the mixture is cooled to room temperature, and a freeze dryer is used for processing for 15 hours to obtain the cubic iron-based oxyhydroxide/graphene composite material with the size of 450 nm. The electrochemical specific capacity of the material is tested in a three-electrode system with 6M KOH as electrolyte, and finally under the constant current condition of 0.5A/g, the specific capacitance is 614F/g, the specific capacitance can reach 409F/g at 10A/g, and the multiplying power is kept at 66.6%.
Example 3
473mg of ferric chloride and 240mg of Na are weighed2SO4And 15mg of GO is placed in a 100mL beaker, 35mL of deionized water is added, magnetic stirring is carried out for 10 minutes, the mixture is transferred into 50mL of polytetrafluoroethylene, the polytetrafluoroethylene is placed in an oven to react for 6 hours at 120 ℃, the deionized water is used for suction filtration and washing to be neutral after the mixture is cooled to room temperature, and a freeze dryer is used for processing for 12 hours to obtain the cubic iron-based oxyhydroxide/graphene composite material with the size of 360 nm. The electrochemical specific capacity of the material is tested in a three-electrode system with 6M KOH as electrolyte, and finally, under the constant current condition of 0.5A/g, the specific capacitance is 632F/g, the specific capacitance can reach 445F/g at 10A/g, and the multiplying power is kept at 70.4%. Fig. 1 is an SEM image of a cubic iron-based oxyhydroxide/graphene composite material in example 3, from which it can be seen that: the average particle size of the material is 360nm, a regular cubic structure is presented, and the uniform compounding with graphene is realized.
Example 4
473mg of ferric chloride and 240mg of Na are weighed2SO4And 75mg GO in a 100mL beaker, followed by 35mL deionized water, magnetic stirring for 10 minutes, and then transferred to 50mL of polytetrafluoroethylene is put into an oven to react for 6h at 120 ℃, deionized water is used for suction filtration and washing to be neutral after the polytetrafluoroethylene is cooled to room temperature, and a freeze dryer is used for processing for 10h to obtain the cubic iron-based oxyhydroxide/graphene composite material with the size of 540 nm. The electrochemical specific capacity of the material is tested in a three-electrode system with 6M KOH as electrolyte, and finally under the constant current condition of 0.5A/g, the specific capacitance is 688F/g, the specific capacitance can reach 497F/g at 10A/g, and the multiplying power is kept at 72.2%. Fig. 2 is an SEM image of the cubic iron-based oxyhydroxide/graphene composite material of example 4, from which it can be seen that: the average particle size of the material is 540nm, a regular cubic structure is presented, and the uniform compounding with graphene is realized.
Example 5
600mg of ferric nitrate and 480mg of Na are weighed2SO4And adding 45mg of GO into a 100mL beaker, then adding 20mL of deionized water, magnetically stirring for 10 minutes, transferring the mixture into 50mL of polytetrafluoroethylene, putting the polytetrafluoroethylene into an oven to react for 12 hours at 100 ℃, performing suction filtration and washing to neutrality by using the deionized water after cooling to room temperature, and treating the mixture by using a freeze dryer for 12 hours to obtain the cubic iron-based oxyhydroxide/graphene composite material. The electrochemical specific capacity of the electrochemical capacitor is tested in a three-electrode system with 6M KOH as electrolyte, and finally under the condition of constant current of 0.5A/g, the specific capacitance is 596F/g, and can reach 417F/g at 10A/g, and the multiplying power is kept at 69.9%.
Example 6
300mg of ferric chloride and 480mg of Na are weighed2SO4And 75mg of GO is placed in a 100mL beaker, then 30mL of deionized water is added, magnetic stirring is carried out for 10 minutes, the mixture is transferred into 50mL of polytetrafluoroethylene, the polytetrafluoroethylene is placed in an oven to react for 8 hours at 160 ℃, the deionized water is used for suction filtration and washing to be neutral after the mixture is cooled to room temperature, and a freeze dryer is used for processing for 12 hours, so that the cubic iron-based oxyhydroxide/graphene composite material is obtained. The electrochemical specific capacity of the material is tested in a three-electrode system with 6M KOH as electrolyte, and finally under the condition of constant current of 0.5A/g, the specific capacitance is 603F/g, the specific capacitance can reach 380F/g at 10A/g, and the multiplying power is kept at 63%.
The above-mentioned embodiments only express the embodiments of the present invention, but not should be understood as the limitation of the scope of the invention patent, it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the concept of the present invention, and these all fall into the protection scope of the present invention.
Claims (3)
1. A preparation method of a cubic iron-based oxyhydroxide/graphene composite material for a supercapacitor is characterized by comprising the following steps:
at room temperature, adding metallic iron source and Na2SO4Adding GO into deionized water, wherein 120-720 mg of Na is correspondingly added into every 20-40 mL of deionized water2SO4(ii) a Stirring for 10 minutes by magnetic force, transferring the mixture into polytetrafluoroethylene, putting the polytetrafluoroethylene into an oven, reacting for 4-12 hours at the temperature of 100-160 ℃, cooling to room temperature, performing suction filtration and washing by deionized water until the mixture is neutral, and performing freeze drying to obtain a cubic iron-based oxyhydroxide/graphene composite material with the size of 360-540 nm; said Na2SO4The mass ratio of the metal iron source to the metal iron source is 1: 3-8: 5; said Na2SO4The mass ratio of the carbon to GO is 3.2: 1-16: 1.
2. The method for preparing a cubic iron-based oxyhydroxide/graphene composite material for a supercapacitor according to claim 1, wherein the metallic iron source is ferric chloride, ferric nitrate and ferric sulfate.
3. The cubic iron-based oxyhydroxide/graphene composite material for the supercapacitor obtained by the method of claim 1 or 2, wherein the specific capacitance of the composite material is 596-688F/g, and the rate capability is 63-72.2%.
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| CN113077993A (en) * | 2021-04-12 | 2021-07-06 | 中南大学 | FeOOH/GO composite electrode material and preparation method and application thereof |
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