CN114759274A - Preparation method of hydrogel electrolyte with high adhesion - Google Patents
Preparation method of hydrogel electrolyte with high adhesion Download PDFInfo
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- CN114759274A CN114759274A CN202210279360.4A CN202210279360A CN114759274A CN 114759274 A CN114759274 A CN 114759274A CN 202210279360 A CN202210279360 A CN 202210279360A CN 114759274 A CN114759274 A CN 114759274A
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 72
- 239000003792 electrolyte Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000011701 zinc Substances 0.000 claims abstract description 25
- 229910000071 diazene Inorganic materials 0.000 claims abstract description 7
- ZMLPZCGHASSGEA-UHFFFAOYSA-M zinc trifluoromethanesulfonate Chemical compound [Zn+2].[O-]S(=O)(=O)C(F)(F)F ZMLPZCGHASSGEA-UHFFFAOYSA-M 0.000 claims abstract description 7
- CITILBVTAYEWKR-UHFFFAOYSA-L zinc trifluoromethanesulfonate Substances [Zn+2].[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F CITILBVTAYEWKR-UHFFFAOYSA-L 0.000 claims abstract description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 8
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 8
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- RAABOESOVLLHRU-UHFFFAOYSA-N diazene Chemical compound N=N RAABOESOVLLHRU-UHFFFAOYSA-N 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052725 zinc Inorganic materials 0.000 abstract description 15
- 230000014759 maintenance of location Effects 0.000 abstract description 5
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- -1 diimine lithium salt Chemical class 0.000 abstract 1
- 229910003002 lithium salt Inorganic materials 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000002985 plastic film Substances 0.000 description 3
- 229920006255 plastic film Polymers 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XQVWYOYUZDUNRW-UHFFFAOYSA-N N-Phenyl-1-naphthylamine Chemical compound C=1C=CC2=CC=CC=C2C=1NC1=CC=CC=C1 XQVWYOYUZDUNRW-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 2
- 229960003351 prussian blue Drugs 0.000 description 2
- 239000013225 prussian blue Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910003266 NiCo Inorganic materials 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/52—Amides or imides
- C08F20/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F20/56—Acrylamide; Methacrylamide
-
- 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
- H01M2300/0085—Immobilising or gelification of electrolyte
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A preparation method of a hydrogel electrolyte with high adhesiveness belongs to the field of hydrogel electrolytes, and the preparation method of the hydrogel electrolyte with high adhesiveness adopts high-concentration zinc trifluoromethanesulfonate and diimine lithium salt solution. The adhesive force of the high-adhesion hydrogel electrolyte disclosed by the invention can reach 0.4kPa when the high-adhesion hydrogel electrolyte is peeled from an electrode, and the capacity retention rate of a flexible zinc battery prepared by using the hydrogel electrolyte is 90% after the flexible zinc battery is bent for 100 times and is subjected to 1500 charge-discharge cycles.
Description
Technical Field
The invention belongs to the field of hydrogel electrolytes, and particularly relates to a preparation method of a high-adhesion hydrogel electrolyte.
Background
Hydrogels are generally composed of elastically crosslinked hydrated polymer chains and are formed byThe interstitial spaces absorb large amounts of water, and thus the hydrogels generally exhibit a wet, soft morphology with relatively high flexibility. By virtue of the above characteristics, the hydrogel electrolyte has a considerable application prospect in flexible batteries, and hydrogel electrolytes of various characteristics have been successively reported in recent years. Polyvinyl alcohol (PVA) has been widely used as a polymer material in flexible energy storage electronic devices, and Wang et al (Journal of Materials Chemistry A,2017,5(25):12969-12976) prepared a hydrogel electrolyte having high ionic conductivity by mixing an electrolytic salt with a polyvinyl alcohol (PVA) hydrogel. Li et al (Energy Environ Sci,2018,11:941- -2S/cm). Huang et al (Advanced Energy Materials,2018,8(31):1802288) reported a molecular structure consisting of 0.2M Zn (CH3COO)2The hydrogel (PANA) composed of 6M KOH and sodium polyacrylate can maintain good stability and excellent mechanical property in a strong alkaline corrosive medium, and Zn// NiCo batteries and zinc-air batteries adopting the PANA hydrogel electrolyte have longer cycle life and higher capacity. Tang et al (Applied Catalysis B: Environmental,2020,260:118209) reported a polyacrylamide-co-acrylic acid (PAM-co-PAA) hydrogel electrolyte that, due to its rich amido/carboxyl groups, PAM-co-PAA hydrogel has excellent moisture retention upon repeated stretching and retains more than half of the water after being left in the air for 10 days.
In addition to the above-mentioned studies on the ionic conductivity, moisture retention, and other properties of the hydrogel electrolyte, the adhesion of the hydrogel electrolyte should be more remarkable. General hydrogel electrolytes (such as PAM) have poor adhesion, and when they are directly used in flexible batteries, the hydrogel electrolyte may fall off from the electrode interface when the batteries are subjected to various mechanical deformations such as bending, twisting, and stretching, thereby causing the failure of the batteries. In conclusion, the preparation of the hydrogel electrolyte with high adhesiveness has important significance for the application of the hydrogel electrolyte in the field of flexible batteries.
Disclosure of Invention
Aiming at the problem of low adhesion of the traditional hydrogel electrolyte, the invention provides a preparation method of a hydrogel electrolyte with high adhesion.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the invention provides a preparation method of a hydrogel electrolyte with high adhesiveness, which comprises the following steps:
step 1, using deionized water as a solvent, and preparing a solution containing 20-22M zinc trifluoromethanesulfonate (Zn (OTf)2) And 1-2M lithium diimine (LiTFSI).
Step 2, taking 4-5 mL of the solution prepared in the step 1, and then respectively adding 0.5-1.5 g of acrylamide (C) into the solution3H5NO), 0.2-0.5 mg of a crosslinking agent (C)7H10N2O2) And 10-14 mg ammonium persulfate ((NH)4)2S2O8) And stirring for 1-3 h at 25 ℃ until the added reagent is completely dissolved.
And 3, taking 5-10 ml of the solution prepared in the step 2, injecting the solution into a mold, and then putting the mold into a 60-80 ℃ oven for 2-3 hours.
The hydrogel electrolyte with high adhesiveness prepared by the invention can be used for flexible batteries, and the high adhesiveness of the prepared hydrogel electrolyte can ensure that the flexible batteries can still keep good contact with electrodes when deformed, thereby improving the working stability of the flexible batteries.
The principle of the invention is as follows:
the preparation of the highly adhesive hydrogel is carried out by adding Zn (OTf) in high concentration2And LiTFSI, so that free water in the hydrogel is reduced, bound water is increased, high molecular functional groups of salt substances in the hydrogel can be in more sufficient contact with the surface of the electrode and are bonded, and more hydrogen bonds are introduced at the interface of the hydrogel and the electrode. When the hydrogel is subjected to mechanical deformation such as stretching, bending and twisting, stress is generated at the interface of the hydrogel and the electrode, and the hydrogen bond can dissipate the stress, so that the hydrogel and the electrode interface can be kept in tight connection, namely, the hydrogel and the electrode interface are enhancedAdhesion between the hydrogel electrolyte and the electrodes is improved.
Compared with the prior art, the invention has the beneficial effects that:
comprising a high concentration of Zn (OTf)2And the hydrogel prepared by LiTFSI has less internal free water and more bound water, can be more fully contacted and bonded with the surface of an electrode, introduces a large number of hydrogen bonds at the interface contacted with a material, greatly enhances the adhesive force between the hydrogel and the material, and can effectively avoid the performance reduction of the battery caused by the peeling of hydrogel electrolyte from the electrode when the battery is deformed.
Drawings
The invention and the advantages thereof are further explained in detail with reference to the drawings and the detailed description.
FIG. 1 is SEM topography of hydrogels prepared by example 1 and comparative example;
FIG. 2 is a graph showing the adhesion curves of the hydrogels prepared in example 1 and comparative example;
fig. 3 shows the cycle performance of the flexible zinc cell prepared in example 2 and the comparative example.
Detailed Description
Example 1
A hydrogel electrolyte with high adhesiveness is prepared by the following steps:
step 1, preparing zinc trifluoromethanesulfonate (Zn (OTf)) containing 21M by taking deionized water as a solvent2) And 1M lithium diimine (LiTFSI).
Step 2, taking 4mL of the solution prepared in the step 1, and then respectively adding 1g of acrylamide (C) to the solution3H5NO), 0.4mg of crosslinking agent (C)7H10N2O2) And 12mg of ammonium persulfate ((NH)4)2S2O8) The mixture was stirred at 25 ℃ for 1h until the added reagents were completely dissolved.
And 3, taking 6ml of the solution prepared in the step 2, injecting the solution into a mold, and then putting the mold into a 60 ℃ oven for 3 hours.
The hydrogel electrolyte obtained by the preparation is the hydrogel electrolyte with high adhesiveness.
Example 2
A hydrogel electrolyte with high adhesiveness is prepared by the following steps:
step 1, preparing 22M zinc trifluoromethanesulfonate (Zn (OTf)) by using deionized water as a solvent2) And 1.5M lithium diimine (LiTFSI).
Step 2, 5mL of the solution prepared in step 1 is taken, and then 1.2g of acrylamide (C) is added to the solution respectively 3H5NO), 0.5mg of crosslinking agent (C)7H10N2O2) And 13mg ammonium persulfate ((NH)4)2S2O8) Stirring was carried out at 25 ℃ for 3h until the added reagents were completely dissolved.
And 3, taking 7ml of the solution prepared in the step 2, injecting the solution into a mold, and then putting the mold into a 70 ℃ oven for 3 hours.
And 3, taking the high-adhesiveness hydrogel electrolyte prepared in the step 3 as an electrolyte of the flexible zinc battery.
Preparing a flexible zinc battery: and 3, adopting a zinc foil as a flexible negative electrode, adopting carbon cloth coated with Prussian blue as a flexible positive electrode, clamping the high-adhesiveness hydrogel electrolyte prepared in the step 3 between the positive electrode and the negative electrode according to a sandwich structure, coating the high-adhesiveness hydrogel electrolyte with a plastic film, and sealing the coated high-adhesiveness hydrogel electrolyte to prepare the flexible zinc battery.
Comparative example
This comparative example prepared a hydrogel using a low concentration of salt and assembled a flexible zinc cell.
Step 1, preparing zinc trifluoromethanesulfonate (Zn (OTf)) containing 1M by taking deionized water as a solvent2) And 0.5M lithium diimine (LiTFSI).
Step 2, taking 4mL of the solution prepared in the step 1, and then respectively adding 1g of acrylamide (C) to the solution3H5NO), 0.4mg of crosslinking agent (C)7H10N2O2) And 12mg of ammonium persulfate ((NH)4)2S2O8) Stirring for 1h at normal temperature until the added reagent is completely dissolved.
And 3, taking 6ml of the solution prepared in the step 2, injecting the solution into a mold, and then putting the mold into a 60 ℃ oven for 3 hours.
And (4) taking the hydrogel electrolyte prepared in the step (3) as an electrolyte of a flexible zinc battery.
Preparing a flexible zinc battery: and (3) adopting a zinc foil as a flexible negative electrode, adopting carbon cloth coated with Prussian blue as a flexible positive electrode, clamping the hydrogel electrolyte prepared in the step (3) between the positive electrode and the negative electrode according to a sandwich structure, coating the hydrogel electrolyte with a plastic film, and sealing the plastic film to prepare the flexible zinc battery.
FIG. 1 is an SEM image of hydrogels prepared according to example 1 and a comparative example, wherein the hydrogel in example 1 has a porous network structure with higher density than the comparative example, and the diameters and the pore sizes of meshes are uniform, so that the structure can show more excellent mechanical properties; FIG. 2 is a graph showing the adhesion curves when the hydrogels prepared in example 1 and the comparative examples were peeled off from the zinc foil by force, and the adhesion of the hydrogel prepared in example 1 was as high as 0.4kPa, whereas the adhesion of the comparative example was only as high as 0.1kPa, demonstrating that the hydrogel electrolyte prepared by using the high concentrated salt according to the present invention has high adhesion. Fig. 3 is a cycle performance diagram of the flexible zinc battery prepared in example 2 and the flexible zinc battery prepared in the comparative example after being bent for 100 times, the specific capacity of the flexible zinc battery prepared in the comparative example is greatly reduced to 35mAh/g after being cycled for 1500 times, and the capacity retention rate is only 49%; the specific capacity of the flexible zinc battery prepared in the embodiment 2 is still 65mAh/g after 1500 times of charge-discharge cycles, and the capacity retention rate is 90%, which proves that the high-adhesion hydrogel electrolyte can still be in close contact with an electrode interface after being stressed, and the capacity of the flexible zinc battery is stabilized.
Claims (10)
1. A method for preparing a hydrogel electrolyte having high adhesiveness, comprising the steps of:
step 1, preparing zinc trifluoromethanesulfonate (Zn (OTf) with a certain concentration by using deionized water as a solvent2) And lithium diimine (LiTFSI).
Step 2, taking a plurality of milliliters of the solution prepared in the step 1, and then respectively adding a proper amount of acrylamide (C) into the solution3H5NO), a proper amount of a crosslinking agent (C)7H10N2O2) And ammonium persulfate ((NH)4)2S2O8) Stirring at normal temperature for several hours until the added reagent is completely dissolved.
And 3, taking a plurality of milliliters of the solution prepared in the step 2, injecting the solution into a mold, and then putting the mold into an oven at a certain temperature for several hours.
2. The method for preparing a hydrogel electrolyte having high adhesiveness as claimed in claim 1, wherein zinc trifluoromethanesulfonate (Zn (OTf))2) The concentration is 20-22M.
3. The method for preparing a hydrogel electrolyte having high adhesiveness as claimed in claim 1, wherein the concentration of lithium diimine (LiTFSI) in step 1 is 1-2M.
4. The method for preparing a hydrogel electrolyte having high adhesiveness as claimed in claim 1, wherein in step 2, 5 to 10ml of the solution prepared in step 1 is taken.
5. The method for preparing a hydrogel electrolyte having high adhesiveness as defined in claim 1, wherein in step 2, acrylamide (C) is added3H5NO) of 0.5 to 1.5 g.
6. The method for preparing a hydrogel electrolyte having high adhesiveness as claimed in claim 1, wherein the crosslinking agent (C) is added in step 27H10N2O2) 0.2-0.5 mg.
7. The method for preparing a hydrogel electrolyte having high adhesiveness according to claim 1, wherein ammonium persulfate ((NH) is added in step 24)2S2O8) 10-14 mg.
8. The method for preparing a hydrogel electrolyte with high adhesiveness as defined in claim 1, wherein in step 2, the temperature is 25 ℃ and the stirring time is 1-3 hours.
9. The method according to claim 1, wherein the amount of the solution prepared in step 2 in step 3 is 5-10 ml.
10. The method for preparing a hydrogel electrolyte with high adhesiveness according to claim 1, wherein in step 3, the oven temperature is 60 ℃ to 80 ℃ for 2 to 3 hours.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111740172A (en) * | 2020-07-03 | 2020-10-02 | 南京林业大学 | Gel electrolyte for zinc ion battery and preparation method thereof |
| US20200343586A1 (en) * | 2019-04-29 | 2020-10-29 | The Johns Hopkins University | Deep Eutectic Solvent-Based Gel Polymer Electrolytes |
| US20210066755A1 (en) * | 2017-03-10 | 2021-03-04 | University Of Maryland, College Park | Aqueous hydrogel electrolyte systems with wide electrochemical stability window |
| CN113851739A (en) * | 2021-10-25 | 2021-12-28 | 长春工业大学 | Preparation and application of gel electrolyte for anti-freezing zinc-based battery |
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2022
- 2022-03-21 CN CN202210279360.4A patent/CN114759274A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210066755A1 (en) * | 2017-03-10 | 2021-03-04 | University Of Maryland, College Park | Aqueous hydrogel electrolyte systems with wide electrochemical stability window |
| US20200343586A1 (en) * | 2019-04-29 | 2020-10-29 | The Johns Hopkins University | Deep Eutectic Solvent-Based Gel Polymer Electrolytes |
| CN111740172A (en) * | 2020-07-03 | 2020-10-02 | 南京林业大学 | Gel electrolyte for zinc ion battery and preparation method thereof |
| CN113851739A (en) * | 2021-10-25 | 2021-12-28 | 长春工业大学 | Preparation and application of gel electrolyte for anti-freezing zinc-based battery |
Non-Patent Citations (1)
| Title |
|---|
| JIAN ZHANG等: "Amide-based molten electrolyte with hybrid active ions for rechargeable Zn batteries" * |
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