CN115621568A - Electrolyte for rechargeable zinc-based battery and preparation method and application thereof - Google Patents
Electrolyte for rechargeable zinc-based battery and preparation method and application thereof Download PDFInfo
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- CN115621568A CN115621568A CN202211366993.5A CN202211366993A CN115621568A CN 115621568 A CN115621568 A CN 115621568A CN 202211366993 A CN202211366993 A CN 202211366993A CN 115621568 A CN115621568 A CN 115621568A
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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
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
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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
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides an electrolyte for a rechargeable zinc-based battery, which comprises a solvent and electrolyte salt, wherein the solvent comprises water and a nitrogen-containing polar aprotic organic solvent, the nitrogen-containing polar aprotic organic solvent is miscible with water in the presence of the electrolyte salt, the volume of the nitrogen-containing polar aprotic organic solvent is 5-100% of the total solvent volume, and the concentration of the electrolyte salt is 1-4mol/L. The electrolyte for the rechargeable zinc-based battery effectively prevents zinc ions from being subjected to water solvation coordination with low space requirement by the nitrogen-containing polar aprotic organic solvent with high coordination space requirement, and solves the problems of thermodynamic instability, dendrite, corrosion and passivation in a water-based electrolyte. The invention also provides a preparation method of the electrolyte for the rechargeable zinc-based battery and the rechargeable zinc-based battery applying the electrolyte.
Description
Technical Field
The invention relates to the technical field of electrolyte, in particular to electrolyte for a rechargeable zinc-based battery and a preparation method and application thereof.
Background
Due to high energy density and excellent cycle stability, the lithium ion battery promotes the energy storage change of portable electronic equipment, electric automobiles and energy storage power grid scale systems, occupies the leading position of a commercial electrochemical energy storage market, but the potential problems limit further development. These problems include: 1) Flammable organic electrolytes increase potential safety risks; 2) The uneven distribution of raw material areas leads to potential supply chain shortage problems; 3) High cost of raw materials. The lithium ion battery is replaced by a sodium/potassium ion battery with the same energy storage mechanism in a mode of sacrificing energy density, although the cost is reduced, the safety and environmental problems are still outstanding.
The zinc-based battery has a zinc cathode with large theoretical volume energy density (5855 mAh/cm) 3 2061mAh/cm of lithium metal cathode 3 Compared with the prior art, the battery has the characteristics of low electrochemical potential (-0.763V vs standard hydrogen electrode), abundant crustal reserves, low cost (comparing $ 3000 per ton with $ 18000 per ton of lithium metal), low toxicity, safety and the like, becomes a powerful candidate for the next-generation secondary rechargeable battery, and is particularly applied to the fields of flexibility, wearable equipment and the like.
However, in the practical application of the traditional water system zinc-based battery, a plurality of problems still exist in the zinc negative electrode, the cycle life of the battery is seriously influenced, and the commercialization popularization of the battery is hindered. First, the plating/stripping of zinc ions is dominated by liquid phase mass transfer, surface polarization and two-dimensional diffusion, resulting in surface protrusions that grow further into dendrites by the "tip effect," which pierce the separator causing short circuit failure of the cell. Secondly, zinc metal can generate hydrogen evolution reaction in an aqueous electrolyte due to thermodynamic instability of the electrolyte, so that surface corrosion and internal pressure of the battery are increased, and the service life of the battery is influenced. The hydrogen evolution reaction promotes passivation to generate an insulating layer, so that transmission of zinc ions and electrons at an interface is influenced, and the cycle performance is further deteriorated. Dendritic crystal problems, corrosion and passivation problems in the zinc-based battery are mutually influenced, so that the coulomb efficiency is low and the circulation stability is poor.
Recently, researchers have used organic solvents to reduce the content of active water in the electrolyte to solve the problem, but high content of organic electrolyte causes a sharp drop in conductivity of the electrolyte, and strong interaction of the organic solvent with zinc ions causes an increase in polarization. Therefore, comprehensively solving various problems of the zinc negative electrode has positive significance for application conversion of the water-based zinc-based battery.
Disclosure of Invention
The invention aims to provide an electrolyte for a rechargeable zinc-based battery, a nitrogen-containing polar aprotic organic solvent with high coordination space requirement effectively prevents zinc ions from being subjected to water solvation coordination with low space requirement, and solves the problems of thermodynamic instability, dendrite, corrosion and passivation in an aqueous electrolyte.
In order to solve the problems, the technical scheme of the invention is as follows:
an electrolyte for a rechargeable zinc-based cell, comprising a solvent and an electrolyte salt, the solvent comprising water and a nitrogen-containing polar aprotic organic solvent, the nitrogen-containing polar aprotic organic solvent being miscible with water in the presence of the electrolyte salt, and the volume of the nitrogen-containing polar aprotic organic solvent being 5-100% of the total solvent volume, the electrolyte salt concentration being 1-4mol/L.
Specifically, the volume of the nitrogen-containing polar aprotic organic solvent can be 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or 100% of the total solvent volume, or other values within this range; the electrolyte salt concentration may be 1mol/L, 2mol/L, 3mol/L, or 4mol/L, or may be other values within this range.
Further, the nitrogen-containing polar aprotic organic solvent is one or two of hexamethylphosphoric triamide (HMPA) and N, N-Dimethylpropyleneurea (DMPU); n, N-Dimethylpropyleneurea (DMPU) is preferred.
Preferably, the volume of the nitrogen-containing polar aprotic organic solvent is 20-80% of the total solvent volume; more preferably, the volume of the nitrogen-containing polar aprotic organic solvent is 80% of the total solvent volume.
Further, the electrolyte salt is one or more of zinc perchlorate, zinc trifluoromethanesulfonate and zinc chloride; preferably, the electrolyte salt is zinc perchlorate.
Preferably, the electrolyte salt concentration is 2-4mol/L; more preferably, the electrolyte salt is zinc perchlorate and the concentration thereof is 2mol/L.
The present invention also provides a method for preparing an electrolyte for a rechargeable zinc-based battery, comprising the steps of:
mixing a nitrogen-containing polar aprotic organic solvent and water in proportion to prepare a mixed solvent;
adding electrolyte salt into the mixed solvent, and uniformly stirring at 20-80 ℃ to prepare the electrolyte for the rechargeable zinc-based battery.
Specifically, the heating temperature may be 20 ℃,30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃ or 80 ℃, or may be other temperature values within this range. Preferably, the heating temperature is 20-50 ℃; more preferably, the heating temperature is 30 ℃.
The invention also provides a rechargeable zinc-based battery, which comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte.
Wherein the positive electrode comprises at least one of vanadium-based compound and manganese-based compound, and the vanadium-based compound is selected from V 2 O 5 、NH 4 V 4 O 10 At least one of manganese-based compounds being MnO 2 . The preparation method of the anode comprises the following steps: and uniformly mixing the positive active material, the conductive carbon and the PVDF according to a mass ratio of 7.
The diaphragm is one of a glass fiber film, polyethylene non-woven fabric or microporous filter paper.
The negative electrode is made of metal zinc foil or irregular zinc powder. If the negative electrode is made of metal zinc foil, the preparation process comprises the following steps: the thickness of the zinc foil is 10-200 μm, and the metal zinc foil is cut into a specific size to be used as a negative plate; if the negative electrode is made of irregular zinc powder, the preparation method comprises the following steps: uniformly mixing irregular zinc powder, conductive carbon and PVDF according to a mass ratio of 8.
Compared with the prior art, the electrolyte for the rechargeable zinc-based battery, and the preparation method and the application thereof have the advantages that:
1. the electrolyte for the rechargeable zinc-based battery provided by the invention takes water and a nitrogen-containing polar aprotic organic solvent as solvents and takes zinc salt as electrolyte salt to form a novel electrolyte system under the combined action of the zinc salt, the water and the nitrogen-containing polar aprotic organic solvent. The nitrogen-containing polar aprotic organic solvent in the system has high molecule coordination requirement, effectively prevents the water solvation coordination of zinc ions and space requirement, effectively inhibits the corrosion and hydrogen evolution reaction caused by thermodynamic instability of the rechargeable zinc-based battery, regulates ion flux, and reduces desolvation energy barrier to realize uniform zinc deposition and high coulombic efficiency.
2. The electrolyte for the rechargeable zinc-based battery provided by the invention has good compatibility with a rechargeable zinc battery system assembled by common vanadium-based and manganese-based anode materials and zinc cathodes, can effectively inhibit the side reaction of the zinc cathode, guides the uniform deposition of zinc, obviously prolongs the cycle life of the battery, has low battery cost, meets the requirement of large-scale energy storage, and has good application prospect.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic view of an electrolyte prepared in example 1 of the present invention;
FIG. 2 is a graph showing conductivity measurements of electrolytes prepared in example 1 of the present invention;
FIG. 3 is a graph showing the cycling stability of the electrolyte prepared in example 1 of the present invention applied to a Zn/Zn symmetrical battery;
FIG. 4 is a graph showing the cycle stability of the electrolyte prepared in example 1 of the present invention applied to a Zn/Cu asymmetric battery;
FIG. 5 shows the application of the electrolyte prepared in example 1 of the present invention to Zn/NH 4 V 4 O 10 A charge-discharge curve chart of the battery;
FIG. 6 is the bookApplication of electrolyte prepared in embodiment 1 of the invention to Zn/NH 4 V 4 O 10 Cycle stability test pattern of the battery.
Detailed Description
The following description of the present invention is provided to enable those skilled in the art to better understand the technical solutions in the embodiments of the present invention and to make the above objects, features and advantages of the present invention more comprehensible.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual values, and between the individual values may be combined with each other to yield one or more new ranges of values, which ranges of values should be considered as specifically disclosed herein.
In the following examples, a rechargeable zinc-based battery includes a positive electrode, a negative electrode, a separator, and the electrolyte prepared in each example. Wherein NH is used 4 V 4 O 10 As the positive electrode, a metal zinc plate (100 μm) was used as the negative electrode, and a glass fiber film was used as the separator.
NH 4 V 4 O 10 The preparation method of the anode comprises the following steps: 1.170g of NH 4 VO 3 The powder was placed in 35mL deionized water, heated to a pale yellow solution and 1.891g of H was added 2 C 2 O 4 ·2H 2 And O, continuously stirring until the mixture is completely dissolved. Placing the uniformly mixed solution in a 50mL reaction kettle for reaction for 48 hours at 140 ℃, washing the reaction product by using deionized water and alcohol in a suction filtration mode after the reaction, and placing the reaction product in a vacuum oven for drying for 12 hours at 80 ℃ to obtain NH 4 V 4 O 10 And (3) powder. Reacting NH 4 V 4 O 10 And uniformly mixing the positive active material, the conductive carbon and the PVDF according to a mass ratio of 7.
Assembling the battery: according to the positive electrode shell, NH 4 V 4 O 10 The 2025 type button cell is assembled by sequentially assembling a positive plate, a diaphragm, electrolyte, a zinc plate negative electrode, a gasket, an elastic sheet and a negative electrode shell.
The electrolyte for rechargeable zinc-based batteries provided by the present invention is illustrated in detail by the following specific examples.
Example 1
Mixing 1mL of deionized water and 4mL of DMPU solvent, adding 3.7238g of zinc perchlorate into the mixed solution, heating and stirring at 30 ℃ to completely dissolve the zinc salt, and completely mixing the two solvents to obtain 2mol/L of zinc perchlorate-80% 2 O electrolyte, as shown in FIG. 1.
And (3) conductivity test: 2mol/L Zinc perchlorate-80% DMPU-20% prepared in this example was tested by the AC impedance method 2 The conductivity of the O electrolyte, the experimental data were recorded in a CHI660E electrochemical workstation, as shown in figure 2. As a result, the electrolyte prepared in this example had a conductivity of 18.43mS/cm.
Using a CT2001A type blue battery test system at 1mA/cm 2 Current density of 1mAh/cm 2 The results of the cycle stability test are shown in fig. 3, and the Zn/Zn symmetric battery can stably cycle for 400 hours or more using the electrolyte prepared in this example.
At 1mA/cm 2 Current density of 1mAh/cm 2 The capacity of the zinc/copper asymmetric battery and the cutoff voltage of 0.5V, and the coulombic efficiency test result is shown in fig. 4, the metal zinc cathode can stably circulate in the electrolyte prepared in the embodiment, and the coulombic efficiency is close to 100%, so that the electrolyte prepared in the embodiment inhibits side reaction and ensures the dendrite-free deposition of zinc ions.
For NH in a voltage range of 0.4-1.4V and a current density of 0.5A/g 4 V 4 O 10 the/Zn full battery is subjected to a cyclic charge-discharge test, the charge-discharge curve is shown in figure 5, and the average discharge voltage is 0.7V; the cycle performance is shown in figure 6, under the low current density of 0.5A/g, 97 percent can still be kept after 95 cycles of cycle, which shows that the dissolution of the anode material is effectively inhibited, and shows thatGood cycle stability.
Example 2
Mixing 2.4mL of deionized water and 0.6mL of DMPU solvent, adding 2.2343g of zinc perchlorate into the mixed solution, heating and stirring at 30 ℃ to completely dissolve the zinc salt, and completely mixing the two solvents to obtain 2mol/L of zinc perchlorate-20% DMPU-80 2 And O electrolyte.
The electrolyte prepared in this example was used for conductivity and electrochemical performance tests. The test result shows that: the conductivity of the electrolyte is 60.87mS/cm and is 1mA/cm 2 Current density of 1mAh/cm 2 The Zn/Zn symmetrical battery is charged and discharged circularly under the capacity condition of (2), and the Zn/Zn symmetrical battery can stably circulate for more than 300 hours. At 1mA/cm 2 Current density of 1mAh/cm 2 The capacity of the battery is equal to that of the battery, the Zn/Cu asymmetric battery is charged and discharged circularly under the condition of 0.5V of cut-off voltage, and the average coulomb efficiency is close to 97 percent after 100 circles of circulation.
Example 3
Mixing 1.2mL deionized water and 1.8mL DMPU solvent, adding 2.2343g zinc perchlorate into the mixed solution, heating and stirring at 30 ℃ to completely dissolve the zinc salt, and mixing the two solvents to obtain 2mol/L zinc perchlorate-40% DMPU-60% 2 And O electrolyte.
The electrolyte prepared in this example was used for conductivity and electrochemical performance tests. The test result shows that: the electrolyte has a conductivity of 50.41mS/cm at 1mA/cm 2 Current density of 1mAh/cm 2 The Zn/Zn symmetrical battery is charged and discharged circularly under the capacity condition of (1), and the Zn/Zn symmetrical battery can stably circulate for more than 234 hours. At 1mA/cm 2 Current density of 1mAh/cm 2 The capacity of the battery is equal to that of the battery, the Zn/Cu asymmetric battery is charged and discharged circularly under the condition of cut-off voltage of 0.5V, and the average coulomb efficiency is close to 98 percent after 100 cycles of circulation.
Example 4
Mixing 1.8mL of deionized water and 1.2mL of DMPU solvent, adding 2.2343g of zinc perchlorate into the mixed solution, heating and stirring at 30 ℃ to completely dissolve the zinc salt, and completely mixing the two solvents to obtain 2mol/L of zinc perchlorate-60% of DMPU-40% 2 And O electrolyte.
The electrolyte prepared in this example was used for conductivity and electrochemical performance tests. The test result shows that: the conductivity of the electrolyte is 22.21mS/cm 2 At 1mA/cm 2 Current density of 1mAh/cm 2 The Zn/Zn symmetrical battery is charged and discharged circularly under the capacity condition of (2), and the Zn/Zn symmetrical battery can be stably circulated for more than 300 hours. At 1mA/cm 2 Current density of 1mAh/cm 2 The capacity of the battery is equal to that of the Zn/Cu battery, the Zn/Cu asymmetric battery is subjected to cyclic charge and discharge under the condition of 0.5V cut-off voltage, and the average coulomb efficiency of 100 cycles of the cycle is close to 99%.
Example 5
Adding 2.2343g of zinc perchlorate into 3mL of DMPU solvent, mixing, heating at 30 ℃ and stirring to completely dissolve the zinc salt, to obtain 2mol/L of zinc perchlorate-100% DMPU-0% 2 And O electrolyte.
The electrolyte prepared in this example was used for conductivity and electrochemical performance tests. The test result shows that: the electrolyte has a conductivity of 3.8mS/cm at 1mA/cm 2 Current density of 1mAh/cm 2 The Zn/Zn symmetrical battery is charged and discharged circularly under the capacity condition of (2), and the Zn/Zn symmetrical battery can stably circulate for more than 200 hours. At 1mA/cm 2 Current density of 1mAh/cm 2 The capacity of the battery is equal to that of the Zn/Cu battery, the Zn/Cu asymmetric battery is subjected to cyclic charge and discharge under the condition of 0.5V cut-off voltage, and the average coulomb efficiency of 100 cycles of the cycle is close to 96%.
Compared with the prior art, the electrolyte for the rechargeable zinc-based battery, and the preparation method and the application thereof have the advantages that:
1. the electrolyte for the rechargeable zinc-based battery provided by the invention takes water and a nitrogen-containing polar aprotic organic solvent as solvents and takes zinc salt as electrolyte salt to form a novel electrolyte system under the combined action of the zinc salt, the water and the nitrogen-containing polar aprotic organic solvent. The nitrogen-containing polar aprotic organic solvent in the system has high coordination requirement, effectively prevents the water solvation coordination of zinc ions and space with low requirement, effectively inhibits the corrosion and hydrogen evolution reaction caused by thermodynamic instability of the rechargeable zinc-based battery, regulates ion flux, and reduces desolvation energy barrier to realize uniform zinc deposition and high coulombic efficiency.
2. The electrolyte for the rechargeable zinc-based battery provided by the invention has good compatibility with a rechargeable zinc battery system assembled by common vanadium-based and manganese-based anode materials and zinc cathodes, can effectively inhibit the side reaction of the zinc cathode, guides the uniform deposition of zinc, obviously prolongs the cycle life of the battery, has low battery cost, meets the requirement of large-scale energy storage, and has good application prospect.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. Various changes, modifications, substitutions and alterations to these embodiments will occur to those skilled in the art without departing from the spirit and scope of the present invention.
Claims (10)
1. An electrolyte for a rechargeable zinc-based cell, comprising a solvent and an electrolyte salt, characterized in that the solvent comprises water and a nitrogen-containing polar aprotic organic solvent, which is miscible with water in the presence of the electrolyte salt, and the volume of the nitrogen-containing polar aprotic organic solvent is 5-100% of the total solvent volume, and the electrolyte salt concentration is 1-4mol/L.
2. The electrolyte for a rechargeable zinc-based cell according to claim 1, wherein the nitrogen-containing polar aprotic organic solvent is one or both of hexamethylphosphoric triamide and N, N-dimethylpropyleneurea.
3. The electrolyte for a rechargeable zinc-based cell according to claim 1, characterized in that the volume of the nitrogen-containing polar aprotic organic solvent is 20-80% of the total solvent volume.
4. The electrolyte for a rechargeable zinc-based cell according to claim 3, characterized in that the volume of the nitrogen-containing polar aprotic organic solvent is 80% of the total solvent volume.
5. The electrolyte for a rechargeable zinc-based battery according to claim 1, wherein the electrolyte salt is one or more of zinc perchlorate, zinc trifluoromethanesulfonate, and zinc chloride.
6. The electrolyte for a rechargeable zinc-based battery according to claim 1 or 5, characterized in that the electrolyte salt concentration is 2-4mol/L.
7. The electrolyte for a rechargeable zinc-based battery according to claim 6, characterized in that the electrolyte salt is zinc perchlorate with a concentration of 2mol/L.
8. A method of preparing the electrolyte for a rechargeable zinc-based battery according to any one of claims 1 to 7, comprising the steps of:
mixing a nitrogen-containing polar aprotic organic solvent and water in proportion to prepare a mixed solvent;
adding electrolyte salt into the mixed solvent, and uniformly stirring at 20-80 ℃ to prepare the electrolyte for the rechargeable zinc-based battery.
9. A rechargeable zinc-based battery comprising a positive electrode, a negative electrode, a separator, and the electrolyte of any one of claims 1-7.
10. The rechargeable zinc-based cell of claim 9, wherein the positive electrode comprises at least one of a vanadium-based compound selected from the group consisting of V, a manganese-based compound 2 O 5 、NH 4 V 4 O 10 At least one of manganese-based compound is MnO 2 。
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| CN102124594A (en) * | 2008-07-14 | 2011-07-13 | 永备电池有限公司 | All-temperature LiFeS2 battery with ether and low concentration LiI electrolyte |
| KR20120048038A (en) * | 2001-07-27 | 2012-05-14 | 에이일이삼 시스템즈 인코포레이티드 | Battery structures, self-organizing structures and related methods |
| CN114976295A (en) * | 2022-06-08 | 2022-08-30 | 迈奇化学股份有限公司 | Aqueous zinc ion battery electrolyte and preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120048038A (en) * | 2001-07-27 | 2012-05-14 | 에이일이삼 시스템즈 인코포레이티드 | Battery structures, self-organizing structures and related methods |
| CN102124594A (en) * | 2008-07-14 | 2011-07-13 | 永备电池有限公司 | All-temperature LiFeS2 battery with ether and low concentration LiI electrolyte |
| CN114976295A (en) * | 2022-06-08 | 2022-08-30 | 迈奇化学股份有限公司 | Aqueous zinc ion battery electrolyte and preparation method and application thereof |
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