CN116315158A - Application of carboxylic ester compound as aqueous electrolyte additive, electrolyte containing aqueous electrolyte additive and zinc ion battery - Google Patents
Application of carboxylic ester compound as aqueous electrolyte additive, electrolyte containing aqueous electrolyte additive and zinc ion battery Download PDFInfo
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- CN116315158A CN116315158A CN202310197678.2A CN202310197678A CN116315158A CN 116315158 A CN116315158 A CN 116315158A CN 202310197678 A CN202310197678 A CN 202310197678A CN 116315158 A CN116315158 A CN 116315158A
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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
- H01M10/36—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
- H01M2300/00—Electrolytes
- H01M2300/0002—Aqueous electrolytes
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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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention belongs to the field of batteries, and relates to application of a carboxylate compound as an additive of an aqueous electrolyte, an electrolyte containing the additive and a zinc ion battery. The carboxylic ester compound has a structure shown in formula I, wherein R 1 、R 2 Identical or different, each independently selected from C 1 ‑C 6 An alkyl group. The additive structure of the invention contains polar group ester group, in electrolyte containing the additive, the additive can enter a solvation structure of zinc ions and form hydrogen bonds with water, so as to change the hydrogen bond network of the water, further inhibit hydrogen evolution and oxygen evolution reaction of the electrolyte in a battery and slow down corrosion of a zinc cathode. In addition, the additive can be preferentially adsorbed on the surface of the zinc negative electrode, so that the wettability of the electrolyte to the zinc negative electrode is improved, the uniform deposition of zinc is promoted, and the growth of dendrite-free crystals is realized. Thus, using the present inventionThe zinc ion battery of the electrolyte has long cycle life and high coulombic efficiency.
Description
Technical Field
The invention belongs to the field of batteries, and particularly relates to application of a carboxylate compound as an additive of an aqueous electrolyte, an aqueous electrolyte containing the additive, and an aqueous zinc ion battery containing the electrolyte.
Background
Since fossil fuels bring about various environmental problems (e.g., greenhouse effect) during use, clean energy sources such as solar energy, wind energy, and tidal energy have been widely studied. However, these clean energy sources have problems of discontinuity and fluctuation, and to solve these problems, the development of large-scale energy storage systems has become more and more important and urgent. Currently, lithium ion batteries have been widely used in portable digital devices, electric vehicles, and energy storage devices. However, its safety and resource starvation problems have hindered its further development. The water-based zinc ion battery is regarded as a powerful substitute for the lithium ion battery in the energy storage field due to the advantages of high safety, low cost, high volume energy density, environmental friendliness and the like.
However, zinc metal anodes are susceptible to corrosion passivation in aqueous electrolytes; during charge and discharge, zinc uneven electro-dissolution and dendrite growth caused by electro-deposition tend to puncture the separator, resulting in a short circuit of the battery. These problems with zinc metal anodes result in lower coulombic efficiency and poorer cycling stability.
Electrolyte modification is a simple and effective method to solve the above-mentioned problems. On the one hand, the electrolyte additive can change the solvation structure of the electrolyte, reduce the quantity of coordinated water and active water, and further inhibit a series of side reactions caused by water decomposition reaction. On the other hand, the electrolyte additive can also obviously improve the electrode interface property, such as improving the electrolyte wettability, forming a solid electrolyte interface film in situ, further uniformly distributing charges, promoting the uniform deposition of zinc and inhibiting the formation of zinc dendrites. And finally, the improvement of coulomb efficiency and cycle stability of the water system zinc ion battery is realized.
Disclosure of Invention
The invention aims to solve the technical problems, and provides a novel aqueous zinc ion battery electrolyte additive carboxylate, an electrolyte containing the additive and an aqueous zinc ion battery, wherein the aqueous zinc ion battery using the additive has excellent electrochemical performance.
In order to achieve the above object, the present invention provides an application of a carboxylate compound as an additive for aqueous electrolyte, the carboxylate compound having a structure represented by formula I,
wherein R is 1 、R 2 Identical or different, each independently selected from C 1 -C 6 Alkyl, preferably C 1 -C 4 An alkyl group.
In the invention, C 1 -C 6 Alkyl groups include, but are not limited to, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, n-pentyl, isopentyl, n-hexyl.
According to a preferred embodiment of the present invention, the carboxylic acid ester compound is at least one of methyl acetate, ethyl propionate, propyl propionate and methyl butyrate.
The second aspect of the present invention provides an aqueous electrolyte containing the above carboxylic acid ester compound as an electrolyte additive.
Specifically, the electrolyte comprises a solute and a solvent, wherein the solute is zinc salt, and the solvent comprises water and a mixed solution of carboxylate compounds, namely deionized water and an additive.
According to a preferred embodiment of the present invention, the carboxylate compound accounts for 0.01 to 90wt.% of the total mass of the electrolyte solvent; preferably 5-50 wt.%, e.g., 10wt.%, 15wt.%, 20wt.%, 25wt.%, 30wt.%, 35wt.%, 40wt.%, 45wt.%, 46wt.%, 47wt.%, 48wt.%, 49wt.%; more preferably 35 to 45wt.%.
According to the present invention, preferably, the zinc salt in the electrolyte is selected from at least one of zinc trifluoromethane sulfonate, zinc bis (trifluoromethyl) sulfonyl imide, zinc bis fluoro sulfonyl imide, zinc tetrafluoroborate, zinc perchlorate, zinc nitrate, zinc chloride, zinc acetate and zinc sulfate.
According to a preferred embodiment of the invention, the concentration of zinc salt in the electrolyte is between 0.1 and 7mol/kg, preferably between 0.5 and 4mol/kg.
A third aspect of the present invention provides an aqueous zinc-ion battery containing the aqueous electrolyte described above.
According to the invention, the water-based zinc ion battery further comprises a positive plate containing a positive electrode active material, a zinc metal negative plate or a zinc metal modified metal negative plate, and a diaphragm arranged between the positive plate and the negative plate.
According to the present invention, the positive electrode active material in the positive electrode sheet may be selected from at least one of a vanadium-based material, a manganese-based oxide, a prussian blue derivative, a polyanion compound, and an organic positive electrode material.
According to a preferred embodiment of the invention, the vanadium-based material is selected from the group consisting of NaV 3 O 8 ·1.5H 2 O、V 2 O 5 、VO 2 And VS (VS) 2 At least one of them.
According to a preferred embodiment of the invention, the manganese-based oxide is selected from MnO 2 、Mn 2 O 3 、Mn 3 O 4 And at least one of MnO.
According to a preferred embodiment of the invention, the Prussian blue derivative is selected from KCu [ Fe (CN) 6 ]At least one of CuHCF and ZnHCF.
According to a preferred embodiment of the invention, the polyanionic compound is selected from the group consisting of NaV 2 (PO 4 ) 3 、VOPO 4 ·xH 2 O and Li 3 V 2 (PO 4 ) 3 At least one of them.
According to a preferred embodiment of the present invention, the organic positive electrode material is selected from at least one of P-chloro-anil and Calix-quinone.
The beneficial effects of the invention are as follows:
the additive structure of the invention contains polar group ester group, in electrolyte containing the additive, the additive can enter a solvation structure of zinc ions and form hydrogen bonds with water, thereby changing a hydrogen bond network of water, reducing the content of coordinated water and free water, further inhibiting hydrogen evolution and oxygen evolution reactions of the electrolyte in a battery, and slowing down corrosion of a zinc cathode. In addition, the additive can be preferentially adsorbed on the surface of the zinc negative electrode, so that the wettability of the electrolyte to the zinc negative electrode is improved, the uniform deposition of zinc is promoted, and the growth of dendrite-free crystals is realized. Therefore, the cycle service life and the coulombic efficiency of the zinc ion battery using the electrolyte provided by the invention are obviously improved.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings.
FIG. 1 is an LSV plot of the electrolyte of comparative example 1 and the electrolyte of example 1 of the present invention.
Fig. 2 is a graph comparing contact angles of the inventive comparative example 1 electrolyte and the example 1 electrolyte on commercial zinc foil.
Fig. 3 is a graph showing comparison of coulombic efficiencies of Zn Ti asymmetric cells of comparative example 1 and example 1 of the present invention.
Fig. 4 is a graph comparing the cycle stability of Zn Cu asymmetric cells of comparative example 1 and examples 1-2 of the present invention.
Fig. 5 is a graph comparing the cycle stability of Zn symmetric batteries of comparative example 1 and example 1 of the present invention.
Fig. 6 is an SEM comparison of the surface of the zinc anode after 50 cycles of Zn symmetric battery of comparative example 1 and example 1.
Fig. 7 is a graph comparing the Zn NVO full cell cycle stability of comparative example 1 of the present invention with that of example 1.
Detailed Description
The invention is further described below with reference to examples. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
Comparative example 1
10g of deionized water was taken, 7.27g of zinc trifluoromethane sulfonate was added, and after 10 minutes of ultrasonic treatment, filtration was carried out to obtain 2mol/kg of zinc trifluoromethane sulfonate as the electrolyte of comparative example 1.
Example 1
Based on comparative example 1, 40wt.% of deionized water was replaced with methyl acetate, and the other preparation methods were exactly the same as comparative example 1, to obtain an electrolyte of example 1.
Example 2
Based on comparative example 1, 20wt.% of deionized water was replaced with methyl acetate, and the other preparation methods were exactly the same as comparative example 1, to obtain an electrolyte of example 2.
Example 3
Based on comparative example 1, 60wt.% of deionized water was replaced with methyl acetate, and the other preparation methods were exactly the same as comparative example 1, to obtain an electrolyte of example 3.
Example 4
Based on comparative example 1, 40wt.% of deionized water was replaced with ethyl acetate, and the other preparation methods were exactly the same as comparative example 1, to obtain an electrolyte of example 4.
Example 5
Based on comparative example 1, 40wt.% of deionized water was replaced with ethyl propionate, and the other preparation methods were exactly the same as comparative example 1, to obtain an electrolyte of example 5.
Example 6
Based on comparative example 1, 40wt.% of deionized water was replaced with methyl butyrate, and the other preparation methods were exactly the same as comparative example 1, to obtain an electrolyte of example 6.
Test example 1
A linear sweep voltammetry test was performed with a commercial zinc foil in the electrolyte of comparative example 1 and the electrolyte of example 1, using a three electrode system with a platinum electrode as the working electrode, a commercial zinc foil as the counter electrode, and an Ag/AgCl electrode as the reference electrode. The test voltage interval was 2 to-1.5V and the scan speed was 0.5mV/s. The LSV curve shown in FIG. 1 is obtained, and it can be seen that the electrolyte of example 1 significantly reduces the hydrogen evolution and oxygen evolution currents and reduces the side reactions of the aqueous electrolyte on the zinc anode.
Test example 2
The contact angles of the electrolyte of comparative example 1 and the electrolyte of example 1 on the surface of commercial zinc foil are tested, and the comparison result is shown in fig. 2, so that the electrolyte of example 1 has stronger wettability, the contact of a solid-liquid interface is enhanced, and the uniform deposition of zinc can be promoted.
Test example 3
The electrolytes obtained in comparative example 1 and examples 1 to 6 were respectively injected into batteries using Ti foil as a positive electrode, commercial zinc foil as a negative electrode, and glass fiber as a separator, to obtain Zn Ti asymmetric batteries of the corresponding comparative example and example. The Zn Ti asymmetric battery coulombic efficiency of each example and comparative example 1 was tested by: charge for 10h, then discharge to 0.5V, recharge for 10h, record charge capacity Q r Then, 9 discharge and charge cycles are carried out, the discharge and charge time is 1h respectively, and each discharge capacity is recorded as Q c Finally, discharging to 0.5V, recording discharge capacity as Q s The charge-discharge current density in the test process is 1mA/cm -2 . The coulombic efficiency calculation formula is: ce= (9Q) c +Q s )/(9Q c +Q r )。
Fig. 3 is a graph comparing coulombic efficiencies of the Zn Ti asymmetric battery of comparative example 1 and example 1, and it can be seen that: the Zn Ti asymmetric battery of example 1 has high coulombic efficiency.
Table 1 is a record of the coulombic efficiency of the Zn Ti asymmetric battery of comparative example 1 and examples 1 to 6, and it can be seen that the addition of different carboxylic acid esters to the electrolyte can improve the coulombic efficiency of the Zn Ti asymmetric battery, but the methyl acetate effect is optimal, and the coulombic efficiency can be further improved by controlling the addition amount of the carboxylic acid ester to the preferred range.
TABLE 1
| Coulombic efficiency (%) | |
| Comparative example 1 | 68.8 |
| Example 1 | 98.7 |
| Example 2 | 98.5 |
| Example 3 | 98.4 |
| Example 4 | 97.4 |
| Example 5 | 96.8 |
| Example 6 | 96.2 |
Test example 4
The electrolytes obtained in comparative example 1 and examples 1 to 2 were respectively injected into a battery having a Cu foil as a positive electrode, a commercial zinc foil as a negative electrode, and a glass fiber as a separator, to obtain Zn Cu asymmetric batteries of the corresponding comparative example and example. Test Zn Cu asymmetric battery circulation stabilityThe charge-discharge current density was measured to be 0.5mA/cm -2 The discharge cutoff voltage was 0.5V.
Fig. 4 is a graph comparing the cycle stability of the Zn Cu asymmetric battery of comparative example 1 and examples 1-2, it can be seen that: when the amount of methyl acetate added is increased, the cycle stability of the battery is improved. However, the carboxylic esters are inflammable organic compounds, and the addition of too much may decrease the safety of the battery and increase the polarization of the battery, and the carboxylic esters should preferably be added in an amount of less than 50wt.%, particularly preferably controlled to 35 to 45wt.%.
Test example 5
The electrolytes obtained in comparative example 1 and example 1 were respectively injected into batteries using commercial zinc foil as positive and negative electrodes and glass fiber as separator, to obtain Zn symmetric batteries of the corresponding comparative example and example. Test example Zn is symmetric battery cycle stability, and the test charge-discharge current density is 1mA/cm -2 The method comprises the steps of carrying out a first treatment on the surface of the The charge and discharge time was 1h, respectively.
Fig. 5 is a graph comparing the cycle stability of the Zn symmetric battery of comparative example 1 with that of example 1, it can be seen that: the electrolyte of the embodiment 1 can obviously improve the cycle stability of Zn symmetric batteries. Fig. 6 is an SEM comparison of the zinc anode surface after 50 cycles of Zn symmetric battery cycles for comparative example 1 and example 1, as can be seen: zinc dendrites on the surface of the Zn symmetric battery pole piece of comparative example 1 grow in disorder, and zinc on the surface of the Zn symmetric battery pole piece of example 1 grows in a plane, which indicates that the introduction of methyl acetate can inhibit side reactions on the surface of a zinc negative electrode and promote uniform deposition of zinc.
Test example 6
The electrolytes obtained in comparative example 1 and example 1 were respectively injected with NaV as a positive electrode active material 3 O 8 ·1.5H 2 O (NVO): binder polyvinylidene fluoride (PVDF): the conductive agent acetylene black comprises the following components in percentage by mass: 1:2, a commercial zinc foil is used as a cathode, and glass fiber is used as a diaphragm, so as to obtain the Zn NVO full battery of the corresponding comparative example and embodiment. The Zn NVO full battery cycle stability is tested, the charge and discharge current density is 0.2A in 3-cycle before testing, and the 3 rd cycle is cycledThe current density of charge and discharge is 1A, and the voltage interval of charge and discharge is 0.3-1.4V.
Fig. 7 is a graph comparing the zn||nvo full cell cycle stability of comparative example 1 with that of example 1, it can be seen that: the electrolyte of the embodiment 1 can obviously improve the cycle stability of the Zn NVO full cell.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
Claims (10)
1. The application of the carboxylate compound as the additive of the water-based electrolyte is characterized in that the carboxylate compound has a structure shown in a formula I,
wherein R is 1 、R 2 Identical or different, each independently selected from C 1 -C 6 Alkyl, preferably C 1 -C 4 An alkyl group.
2. The use according to claim 1, wherein the carboxylic acid ester compound is at least one of methyl acetate, ethyl propionate, propyl propionate and methyl butyrate.
3. An aqueous electrolyte comprising the carboxylic acid ester compound according to claim 1 or 2 as an electrolyte additive.
4. The aqueous electrolyte according to claim 3, wherein the electrolyte comprises a solute and a solvent, the solute being a zinc salt, the solvent comprising water and the carboxylate compound.
5. The aqueous electrolyte according to claim 4, wherein the carboxylate compound accounts for 0.01 to 90wt.% of the total mass of the electrolyte solvent; preferably 5 to 50wt.%; more preferably 35 to 45wt.%.
6. The aqueous electrolyte according to claim 4, wherein the zinc salt in the electrolyte is at least one selected from zinc trifluoromethane sulfonate, zinc bis (trifluoromethyl) sulfonyl imide, zinc bis (fluoro) sulfonyl imide, zinc tetrafluoroborate, zinc perchlorate, zinc nitrate, zinc chloride, zinc acetate and zinc sulfate.
7. The aqueous electrolyte according to claim 4, wherein the concentration of zinc salt in the electrolyte is 0.1-7 mol/kg, preferably 0.5-4 mol/kg.
8. An aqueous zinc-ion battery comprising the aqueous electrolyte according to any one of claims 3 to 7.
9. The aqueous zinc-ion battery of claim 8, wherein the aqueous zinc-ion battery further comprises a positive electrode sheet containing a positive electrode active material, a zinc metal negative electrode sheet, or a zinc metal modified metal negative electrode sheet, and a separator disposed between the positive electrode sheet and the negative electrode sheet.
10. The aqueous zinc-ion battery according to claim 9, wherein the positive electrode active material in the positive electrode sheet is selected from at least one of a vanadium-based material, a manganese-based oxide, a prussian blue derivative, a polyanion compound, and an organic positive electrode material;
the vanadium-based material is preferably selected from NaV 3 O 8 ·1.5H 2 O、V 2 O 5 、VO 2 And VS (VS) 2 At least one of (a) and (b); the manganese-based oxide is preferably selected from MnO 2 、Mn 2 O 3 、Mn 3 O 4 And MnO; the Prussian blue derivative is preferably selected from KCu [ Fe (CN) 6 ]、CuHAt least one of CF and ZnHCF; the polyanionic compound is preferably selected from NaV 2 (PO 4 ) 3 、VOPO 4 ·xH 2 O and Li 3 V 2 (PO 4 ) 3 At least one of (a) and (b); the organic positive electrode material is preferably at least one selected from the group consisting of P-chloranil and Calix quinone.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117613432A (en) * | 2024-01-24 | 2024-02-27 | 中南大学 | Containing acyl esters C having both keto and ester groups 5~8 Aqueous zinc ion battery composite electrolyte of alkane chain-like organic additive, and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117613432A (en) * | 2024-01-24 | 2024-02-27 | 中南大学 | Containing acyl esters C having both keto and ester groups 5~8 Aqueous zinc ion battery composite electrolyte of alkane chain-like organic additive, and preparation method and application thereof |
| CN117613432B (en) * | 2024-01-24 | 2024-04-09 | 中南大学 | Aqueous zinc ion battery composite electrolyte and preparation method and application thereof |
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