CN115483387B - Positive electrode active material and preparation method thereof, composite positive electrode and aqueous zinc ion battery - Google Patents
Positive electrode active material and preparation method thereof, composite positive electrode and aqueous zinc ion battery Download PDFInfo
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
- H01M10/38—Construction or 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
- H01M4/02—Electrodes composed of, or comprising, active material
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
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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
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Abstract
本发明属于锌离子电池技术领域，具体涉及一种正极活性材料及其制备方法、复合正极和水系锌离子电池。本发明提供了一种正极活性材料的制备方法，包括以下步骤：将第一有机化合物和第二有机化合物混合，经脱水缩合反应，得到所述正极活性材料；所述第一有机化合物包括氨基醌类化合物；所述第二有机化合物的官能团包括羰基。由本发明提供的正极活性材料制备得到的水系锌离子电池具有较高的比容量。
The present invention belongs to the technical field of zinc ion batteries, and specifically relates to a positive electrode active material and a preparation method thereof, a composite positive electrode and an aqueous zinc ion battery. The present invention provides a preparation method of a positive electrode active material, comprising the following steps: mixing a first organic compound and a second organic compound, and subjecting the mixture to a dehydration condensation reaction to obtain the positive electrode active material; the first organic compound comprises an aminoquinone compound; and the functional group of the second organic compound comprises a carbonyl group. The aqueous zinc ion battery prepared from the positive electrode active material provided by the present invention has a high specific capacity.
Description
Technical Field
The invention belongs to the technical field of zinc ion batteries, and particularly relates to an anode active material, a preparation method thereof, a composite anode and a water-based zinc ion battery.
Background
Due to the use of traditional fossil fuels, environmental pollution is increasingly serious, and the demand of clean energy is increasingly urgent, and electric energy storage is a mature method for storing clean energy. Currently, lithium ion batteries are widely used in portable electronic products, biomedical devices, and new generation electric vehicles. However, due to the safety, high cost, limited lithium resources, etc. of lithium ion batteries, there is an urgent need to develop new energy storage devices to replace lithium ion batteries.
The water-based zinc ion battery uses zinc metal rich in resources on earth as a negative electrode, and adopts water-based electrolyte with high ion conductivity, so that the water-based zinc ion battery has the advantages of high safety, environmental friendliness, high energy density and high coulomb efficiency, and becomes a hot spot for energy research. The selection of the anode material plays a vital role in realizing high specific capacity and long cycle life of the water-based zinc ion battery.
The conventional cathode material is mainly an inorganic electrode material including manganese-based oxide, vanadium-based derivative or Prussian blue analog. The inorganic electrode material has the advantages of high capacity, high energy density, high power density and the like, but the further improvement of the battery performance is limited due to the problems of resource shortage, environmental pollution, complex synthesis process, high energy consumption and the like. In addition, during charge and discharge cycles, the continuous intercalation/deintercalation of hydrated Zn 2+ and H + tends to cause collapse of the structure of the inorganic material, reducing the cycling stability of the battery.
In recent years, some organic compounds having redox activity, such as small molecule quinone-based compounds containing conjugated carbonyl groups, can effectively buffer volume changes caused by intercalation/deintercalation of hydrated Zn 2+ and H + and exhibit good cycle stability due to having a flexible skeleton. However, the zinc ion battery prepared from the small molecular quinone-based compound still has the defect of low specific capacity.
Disclosure of Invention
The invention aims to provide a positive electrode active material, a preparation method thereof, a composite positive electrode and a water-based zinc ion battery.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a preparation method of an anode active material, which comprises the following steps:
Mixing a first organic compound and a second organic compound, and obtaining the positive electrode active material through dehydration condensation reaction;
The first organic compound comprises an amino quinone compound;
the functional group of the second organic compound includes a carbonyl group.
Preferably, the amino quinone compound comprises one or more of 1, 2-diaminoanthraquinone, 1, 2-diaminonaphthoquinone, 2-amino-1, 4-naphthoquinone, 2,3,5, 6-tetra (amino) p-benzoquinone, 2-aminoanthraquinone, 2, 6-diaminoanthraquinone, 1-aminoanthraquinone-2-carboxylic acid, 1-hydroxy-4-aminoanthraquinone and 1, 5-dihydroxy-4, 8-diaminoanthraquinone.
Preferably, the second organic compound comprises a quinone compound and/or a ketone compound.
Preferably, the quinone compound comprises one or more of 2, 5-dihydroxyl-1, 4-benzoquinone, tetrahydroxy-1, 4-benzoquinone, 2, 5-dihydroxyl-3, 6-dichlorobenzoquinone, anthraquinone and phenanthrenequinone;
the ketone compound comprises one or more of cyclohexanones, cyclopentanones, 3, 4-dihydroxyl-3-cyclobutene-1, 2-diketones and 4, 5-dihydroxyl-4-cyclopentene-1, 2, 3-triones.
Preferably, the molar ratio of the first organic compound to the second organic compound is 1-6:1-4.
Preferably, the temperature of the dehydration condensation reaction is 100-200 ℃, the temperature rising rate from the temperature of the dehydration condensation reaction to the temperature of the dehydration condensation reaction is 1-5 ℃ per minute, and the time is 2-8 hours.
The invention also provides the positive electrode active material prepared by the preparation method.
The invention also provides a composite positive electrode, which comprises a current collector and a positive electrode material loaded on the current collector, wherein the positive electrode material comprises a positive electrode active material, a conductive agent and a binder, and the positive electrode active material is prepared by the positive electrode active material according to the technical scheme or the preparation method according to the technical scheme.
Preferably, the mass ratio of the positive electrode active material to the conductive agent to the binder is (3-9): 0.5-6): 0.5-1.
The invention also provides a water-based zinc ion battery, which comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, wherein the positive electrode is the composite positive electrode according to the technical scheme.
The invention provides a preparation method of a positive electrode active material, which comprises the following steps of mixing a first organic compound and a second organic compound, and obtaining the positive electrode active material through dehydration condensation reaction, wherein the first organic compound comprises an amino quinone compound, and the functional group of the second organic compound comprises a carbonyl group. According to the invention, the positive electrode active material obtained by the method contains two active sites of C=O and C=N by utilizing dehydration condensation of-NH 2 in the amino quinone compound and carbonyl in the second compound, so that the zinc storage site density of the positive electrode active material is improved, and the specific capacity of the water-based zinc ion battery is further improved.
Drawings
Fig. 1 is an infrared spectrum of the positive electrode active material obtained in example 1;
FIG. 2 is a charge-discharge curve of the aqueous zinc ion battery obtained in example 1 in a voltage range of 0.2 to 1.7V and a current density of 50 mA/g;
FIG. 3 is a charge-discharge curve of the aqueous zinc ion battery obtained in example 1 under a voltage range of 0.2 to 1.5V and a current density of 50 mA/g;
FIG. 4 is a cycle curve of the aqueous zinc ion battery obtained in example 2 under a voltage range of 0.2 to 1.5V and a current density of 50 mA/g;
FIG. 5 is a cycle curve of the aqueous zinc ion battery obtained in example 3 at a voltage ranging from 0.2 to 1.5V and a current density of 50 mA/g.
Detailed Description
The invention provides a preparation method of an anode active material, which comprises the following steps:
Mixing a first organic compound and a second organic compound, and obtaining the positive electrode active material through dehydration condensation reaction;
The first organic compound comprises an amino quinone compound;
the functional group of the second organic compound includes a carbonyl group.
In the present invention, all raw materials are commercially available products well known to those skilled in the art unless specified otherwise.
In the present invention, the amino quinone compound preferably includes one or more of 1, 2-diaminoanthraquinone, 1, 2-diaminonaphthoquinone, 2-amino-1, 4-naphthoquinone, 2,3,5, 6-tetra (amino) p-benzoquinone, 2-aminoanthraquinone, 2, 6-diaminoanthraquinone, 1-aminoanthraquinone-2-carboxylic acid, 1-hydroxy-4-aminoanthraquinone and 1, 5-dihydroxy-4, 8-diaminoanthraquinone, and when the amino quinone compound is two or more of the above-mentioned choices, the ratio of specific substances is not particularly limited, and the specific substances may be mixed in any ratio.
In the present invention, the second organic compound preferably includes a quinone compound and/or a ketone compound. In the present invention, the quinone compound preferably includes one or more of 2, 5-dihydroxy-1, 4-benzoquinone, tetrahydroxy-1, 4-benzoquinone, 2, 5-dihydroxy-3, 6-dichlorobenzoquinone, anthraquinone and phenanthrenequinone, the ketone compound preferably includes one or more of cyclohexanecarbon, cyclopentanone, 3, 4-dihydroxy-3-cyclobutene-1, 2-dione, 4, 5-dihydroxy-4-cyclopentene-1, 2, 3-trione, and when the second organic compound is two or more of the above-mentioned choices, the ratio of specific substances is not particularly limited, and the second organic compound may be mixed in any ratio.
In the invention, the molar ratio of the first organic compound to the second organic compound is preferably 1-6:1-4, and more preferably 2-5:2-3.
In the present invention, the mixing means is preferably grinding. The grinding process is not particularly limited, and may be performed by a process well known to those skilled in the art. In the present invention, the grinding is preferably performed in a mortar.
In the present invention, the temperature of the dehydration condensation reaction is preferably 100 to 200 ℃, more preferably 120 to 180 ℃, still more preferably 150 to 160 ℃, the temperature rising rate from the temperature of the dehydration condensation reaction to the temperature of the dehydration condensation reaction is preferably 1 to 5 ℃ per minute, more preferably 2 to 4 ℃ per minute, and the time is preferably 2 to 8 hours, more preferably 3 to 7 hours, more preferably 4 to 6 hours.
In the present invention, the dehydration condensation reaction is preferably performed under a nitrogen atmosphere.
In the present invention, the dehydration condensation reaction is preferably carried out in a tube furnace.
After the dehydration condensation reaction is completed, the invention also preferably comprises post-treatment of the obtained product, wherein the post-treatment preferably comprises ethanol washing and drying. The process of washing and drying the ethanol is not particularly limited, and may be performed by a process well known to those skilled in the art.
The invention also provides the positive electrode active material prepared by the preparation method. In the present invention, the positive electrode active material includes two active sites of c=o and c=n.
The invention also provides a composite positive electrode, which comprises a current collector and a positive electrode material loaded on the current collector, wherein the positive electrode material comprises a positive electrode active material, a conductive agent and a binder, and the positive electrode active material is prepared by the positive electrode active material according to the technical scheme or the preparation method according to the technical scheme.
In the present invention, the current collector preferably includes a stainless steel mesh, a stainless steel foil, a titanium mesh, a titanium foil, a porous stainless steel belt, a carbon cloth, a carbon mesh, or a carbon felt.
In the present invention, the positive electrode material includes a positive electrode active material, a conductive agent, and a binder. In the invention, the conductive agent preferably comprises a first conductive agent and/or a second conductive agent, the first conductive agent preferably comprises ketjen black and/or acetylene black, and the second conductive agent preferably comprises one or more of carbon nanotubes, graphene, mxene two-dimensional materials and carbon fibers. In the present invention, when the conductive agent preferably includes a first conductive agent and a second conductive agent, the mass percentage of the first conductive agent is preferably 5 to 95%.
In the invention, the mass ratio of the positive electrode active material to the conductive agent to the binder is preferably (3-9): 0.5-6): 0.5-1, more preferably (4-8): 1.0-5.0): 0.6-0.9, and even more preferably (5-7): 2.0-4.0): 0.7-0.8. In the invention, the loading amount of the positive electrode material on the current collector is preferably 1.5-2.0 mg/cm 2.
In the present invention, the preparation method of the composite positive electrode preferably includes the steps of:
mixing an anode active material, a conductive agent, a binder and a polar solvent to obtain slurry;
and coating the slurry on the surface of the current collector, and drying to obtain the composite anode.
In the present invention, the polar solvent preferably includes one or more of N-methylpyrrolidone, water and ethanol. The amount of the polar solvent to be added in the present invention is not particularly limited, and may be any one known to those skilled in the art.
In the present invention, the mixing process is preferably:
primary mixing an anode active material and a conductive agent to obtain a primary mixture;
Secondary mixing the binder and the polar solvent to obtain a secondary mixture;
the primary mixture and the secondary mixture are tertiary mixed.
In the present invention, the primary mixing means is preferably grinding. The grinding process is not particularly limited, and may be performed by a process well known to those skilled in the art. In the present invention, the grinding is preferably performed in a mortar.
The process of the secondary mixing is not particularly limited, and may be employed as is well known to those skilled in the art.
In the present invention, the three-stage mixing is preferably performed by grinding. The grinding process is not particularly limited, and may be performed by a process well known to those skilled in the art. In the present invention, the grinding is preferably performed in a mortar.
The process of the coating is not particularly limited, and may be performed by a process well known to those skilled in the art.
In the invention, the drying temperature is preferably 60-120 ℃, more preferably 70-110 ℃, still more preferably 80-100 ℃, and the drying time is preferably 8-12 h, still more preferably 9-10 h.
In the present invention, the diameter of the composite positive electrode is preferably 10mm. In a specific embodiment of the present invention, it is preferable that the composite positive electrode having a diameter of 10mm is obtained by cutting after the drying.
The invention also provides a water-based zinc ion battery, which comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, wherein the positive electrode is the composite positive electrode according to the technical scheme.
In the present invention, the negative preferably includes a metallic zinc foil or zinc alloy. In the present invention, the membrane preferably comprises a water-based filter paper, a proton exchange membrane or a glass fiber filter paper.
In the present invention, the electrolyte is preferably an aqueous solution containing a zinc salt or a polyvinyl alcohol hydrogel containing a zinc salt. In the present invention, the zinc salt preferably includes Zn (one or more of CF 3SO3)2、ZnSO4、Zn(NO3)2、ZnCl2 and Zn (CH 3COO)2), and in the present invention, the molar concentration of the zinc salt in the electrolyte is preferably 1 to 3mol/L.
The method for assembling the battery is not particularly limited, and the battery may be assembled by sequentially assembling the positive electrode shell, the positive electrode, the electrolyte, the separator, the negative electrode, the gasket, the elastic sheet and the negative electrode shell. The types of the positive electrode case, the gasket, the elastic sheet and the negative electrode case are not particularly limited, and those skilled in the art can be adopted. In the present invention, the assembly is preferably performed in an air atmosphere.
In order to further illustrate the present invention, the following describes in detail a positive electrode active material and its preparation method, a composite positive electrode and an aqueous zinc ion battery provided by the present invention with reference to the accompanying drawings and examples, but they should not be construed as limiting the scope of the present invention.
Example 1
2Mmol of 1, 2-diaminoanthraquinone and 0.5mmol of 2, 5-dihydroxy-1, 4-benzoquinone were weighed, put into a mortar and ground and mixed. Putting the obtained mixture into a tube furnace, introducing nitrogen, heating to 180 ℃ at a heating rate of 2 ℃ per min for dehydration condensation reaction for 5 hours, washing the obtained product with ethanol after the reaction is completed, and then performing vacuum drying to obtain the anode active material;
grinding and mixing 60mg of positive electrode active material, 20mg of ketjen black and 10mg of carbon nano tube in a mortar to obtain a first-stage mixture, mixing 10mg of polyvinylidene fluoride and 0.5mL of N-methyl pyrrolidone to obtain a second-stage mixture, mixing the first-stage mixture and the second-stage mixture, grinding to obtain slurry, coating the obtained slurry on a stainless steel mesh by using a glass rod, then placing the stainless steel mesh in a vacuum drying oven, drying at 80 ℃ for 12 hours, and cutting to obtain a composite positive electrode with the diameter of 10mm (the loading amount of the positive electrode material on the composite positive electrode is 1.6mg/cm 2);
The positive electrode shell, the composite positive electrode and 1mol/L Zn (CF 3SO3)2 aqueous electrolyte, glass fiber diaphragm, zinc foil, gasket, elastic sheet and negative electrode shell) are assembled in the air in sequence to obtain the aqueous zinc ion battery.
Example 2
2Mmol of 1, 2-diaminoanthraquinone and 0.5mmol of 2, 5-dihydroxy-1, 4-benzoquinone were weighed, put into a mortar and ground and mixed. Putting the obtained mixture into a tube furnace, introducing nitrogen, heating to 180 ℃ at a heating rate of 2 ℃ per min for dehydration condensation reaction for 5 hours, washing the obtained product with ethanol after the reaction is completed, and then performing vacuum drying to obtain the anode active material;
Grinding and mixing 60mg of positive electrode active material and 30mg of ketjen black in a mortar to obtain a first-stage mixture, mixing 10mg of polyvinylidene fluoride and 1.5mL of N-methyl pyrrolidone to obtain a second-stage mixture, mixing the first-stage mixture and the second-stage mixture and grinding to obtain slurry, coating the obtained slurry on a stainless steel net by using a glass rod, then placing the stainless steel net in a vacuum drying oven, drying at 80 ℃ for 12 hours, and cutting to obtain a composite positive electrode with the diameter of 10mm (the loading amount of the positive electrode material on the composite positive electrode is 1.6mg/cm 2);
The water-based zinc ion battery is obtained by assembling a positive electrode shell, a composite positive electrode, 1mol/L Zn (CF 3SO3)2 aqueous solution, a glass fiber diaphragm, zinc foil, a gasket, an elastic sheet and a negative electrode shell in the air in sequence.
Example 3
2Mmol of 1, 2-diaminoanthraquinone and 0.5mmol of 2, 5-dihydroxy-1, 4-benzoquinone were weighed, put into a mortar and ground and mixed. Putting the obtained mixture into a tube furnace, introducing nitrogen, heating to 180 ℃ at a heating rate of 2 ℃ per min for dehydration condensation reaction for 5 hours, washing the obtained product with ethanol after the reaction is completed, and then performing vacuum drying to obtain the anode active material;
Grinding and mixing 60mg of positive electrode active material, 20mg of ketjen black and 10mg of carbon nano tube in a mortar to obtain a first-stage mixture, mixing 10mg of polyvinylidene fluoride and 0.5mL of N-methyl pyrrolidone to obtain a second-stage mixture, mixing the first-stage mixture and the second-stage mixture and grinding to obtain slurry, coating the obtained slurry on a stainless steel mesh by using a glass rod, then placing the stainless steel mesh in a vacuum drying oven, drying at 80 ℃ for 12 hours, and cutting to obtain a composite positive electrode with the diameter of 10mm (the loading amount of the positive electrode material on the composite positive electrode is 1.6mg/cm 2);
the water-based zinc ion battery is obtained by assembling a positive electrode shell, a composite positive electrode, 1mol/L Zn (CF 3SO3)2 polyvinyl alcohol hydrogel electrolyte, a glass fiber diaphragm, zinc foil, a gasket, an elastic sheet and a negative electrode shell in the air in sequence.
Performance testing
Test example 1
The positive electrode active material obtained in example 1 was subjected to infrared spectrogram test, and the obtained test curve is shown in fig. 1, and it can be seen from fig. 1 that the positive electrode active material obtained in this example contains characteristic peaks of c=o and c=n bonds.
Test example 2
The aqueous zinc ion battery obtained in example 1 was subjected to charge-discharge cycle and CV test in a new Wei battery test system and an electrochemical workstation, the voltage test range was 0.2 to 1.7V, the current density was 50mA.g -1, the charge-discharge curve was as shown in FIG. 2, and it can be seen from FIG. 2 that the initial charge specific capacity was 191 mAh.g -1, and the charge specific capacity of the battery after 5 cycles was 185 mAh.g -1.
Test example 3
The aqueous zinc ion battery obtained in example 1 was subjected to charge-discharge cycle and CV test in a new Wei battery test system and an electrochemical workstation, the voltage test range was 0.2 to 1.5V, the current density was 50mA.g -1, the charge-discharge curve was as shown in FIG. 3, it can be seen from FIG. 3 that the initial charge specific capacity was 59 mAh.g -1, the charge specific capacity of the battery after 25 cycles was 158 mAh.g -1, and the charge specific capacity of the battery after 100 cycles was 131 mAh.g -1, showing good cycle stability.
Test example 4
The aqueous zinc ion battery obtained in example 2 was subjected to charge-discharge cycle and CV test in a new wei battery test system and an electrochemical workstation, the voltage test range was 0.2 to 1.5v, the current density was 50ma·g -1, the cycle curve obtained was as shown in fig. 4, and as seen from fig. 4, the specific charge capacity of the battery was 117mah·g -1 when the battery was cycled to 100 cycles.
Test example 5
The aqueous zinc ion battery obtained in example 3 was subjected to charge-discharge cycle and CV test in a new Wei battery test system and an electrochemical workstation, the voltage test range was 0.2 to 1.5V, the current density was 50 mA.g -1, the cycle curve obtained was as shown in FIG. 5, and as can be seen from FIG. 5, the specific charge capacity of the battery at 100 cycles was 128 mAh.g -1, and excellent electrochemical performance was exhibited.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
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| CN114883559A (en) * | 2022-04-29 | 2022-08-09 | 安徽大学 | Naphthoquinone-quinoxaline organic electrode material and application thereof in aqueous zinc ion battery |
| CN115232308A (en) * | 2022-08-10 | 2022-10-25 | 燕山大学 | Quinone polymer positive electrode material and preparation method and application thereof |
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| US12148915B2 (en) * | 2018-11-02 | 2024-11-19 | Nissan Chemical Corporation | Composition for forming an active material composite, an active material composite, and a method for producing an active material composite |
| CN112961163B (en) * | 2021-01-29 | 2022-07-05 | 华中科技大学 | High-capacity metal ion battery organic electrode material and preparation method and application thereof |
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