CN112133962A - Preparation method of bis (trifluoromethyl) sulfimide lithium-glucose carbon quantum dot solid electrolyte - Google Patents
Preparation method of bis (trifluoromethyl) sulfimide lithium-glucose carbon quantum dot solid electrolyte Download PDFInfo
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- CN112133962A CN112133962A CN202011024512.3A CN202011024512A CN112133962A CN 112133962 A CN112133962 A CN 112133962A CN 202011024512 A CN202011024512 A CN 202011024512A CN 112133962 A CN112133962 A CN 112133962A
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- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- -1 bis (trifluoromethyl) sulfimide lithium-glucose carbon Chemical compound 0.000 title claims abstract description 9
- 239000002096 quantum dot Substances 0.000 title description 4
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 49
- 239000008103 glucose Substances 0.000 claims abstract description 42
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 42
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 5
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 229920003196 poly(1,3-dioxolane) Polymers 0.000 abstract description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 6
- 238000000227 grinding Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 125000001889 triflyl group Chemical group FC(F)(F)S(*)(=O)=O 0.000 description 3
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 150000003949 imides Chemical class 0.000 description 2
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical group [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 230000005476 size effect Effects 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M2300/0085—Immobilising or gelification of electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention relates to a preparation method of a lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot solid electrolyte, which comprises a high molecular polymer and lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dots, wherein the high molecular polymer is selected from polyoxyethylene or one of poly (1, 3-dioxolane), and the preparation method of the lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dots comprises the following steps: dissolving 5-10 parts of lithium bis (trifluoromethyl) sulfonyl imide and 10 parts of glucose in water, and adding the mixed solution into a hydrothermal reaction kettle; placing the hydrothermal reaction kettle in a muffle furnace, heating for 6-24 hours at 200-400 ℃, and naturally cooling to obtain a lithium bis (trifluoromethyl) sulfonimide-glucose carbon quantum dot aqueous solution; and (3) carrying out freeze drying treatment on the lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot aqueous solution to obtain the dried lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot.
Description
Technical Field
The invention relates to a polymer electrolyte and a preparation method thereof, in particular to a preparation method of a bis (trifluoromethyl) sulfimide lithium-glucose carbon quantum dot solid electrolyte.
Background
Solid electrolytes have received much attention because of their high safety. However, the ion conductivity is too low due to the difficulty in ion conduction of the conventional solid electrolyte, and the lithium ion transport number is too low due to polarization in electrochemical reaction, which limits the application of the solid electrolyte in batteries.
In order to improve the ion conductivity and the lithium ion transfer number of the solid electrolyte, the invention provides the preparation of the lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot solid electrolyte, and the purpose of preparing the solid electrolyte with high lithium ion transfer number and ion conductivity is achieved.
Disclosure of Invention
The invention aims to provide a preparation method of a bis (trifluoromethyl) sulfimide lithium-glucose carbon quantum dot solid electrolyte, which can effectively improve the ion conductivity and the lithium ion mobility of the solid electrolyte. The invention is realized by the following scheme:
a preparation method of a lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot solid electrolyte comprises a high molecular polymer and a lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot, wherein the high molecular polymer is selected from one of polyoxyethylene or poly 1, 3-dioxolane, and the preparation method of the lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot comprises the following steps:
1) dissolving 5-10 parts of lithium bis (trifluoromethyl) sulfonyl imide and 10 parts of glucose (by weight) in water, and adding the mixed solution into a hydrothermal reaction kettle;
2) placing the hydrothermal reaction kettle in a muffle furnace, heating for 6-24 hours at 200-400 ℃, and naturally cooling to obtain a lithium bis (trifluoromethyl) sulfonimide-glucose carbon quantum dot aqueous solution;
3) and (3) carrying out freeze drying treatment on the lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot aqueous solution to obtain the dried lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot.
Preferably, the mass ratio of the lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dots to the high molecular polymer is (3-6): 10.
Dissolving the prepared carbon quantum dot powder (3-6 parts) and high molecular polymer powder (10 parts) in an organic solution, heating and stirring for at least 12 hours, pouring into a mold, and performing vacuum drying (at the temperature of 30-100 ℃) to obtain the lithium bis (trifluoromethyl sulfonyl imide) -glucose carbon quantum dot solid electrolyte.
The method is convenient and easy to implement, the lithium bis (trifluoromethyl sulfonyl) imide-glucose carbon quantum dot solid electrolyte is prepared by the method, the prepared carbon quantum dot effectively reserves the lithium bis (trifluoromethyl sulfonyl) imide structure, and the carbon quantum dot skeleton structure after glucose carbonization is constructed. The prepared carbon quantum dot has the characteristics of high electron delocalization of the sulfimide group and large size of the carbon quantum dot. In the electrochemical reaction process, lithium ions can be well dissociated, and meanwhile, carbon quantum dot anions are difficult to move due to the size effect. Thereby obtaining the solid electrolyte with high ionic conductivity and lithium ion transference number performance.
Drawings
Fig. 1 shows ion conductivity of lithium bis (trifluoromethylsulfonyl) imide-glucose carbon quantum dot solid electrolyte and lithium bis (trifluoromethylsulfonyl) imide solid electrolyte with temperature change.
FIG. 2 is a polarization curve of a lithium/lithium symmetric battery prepared by using a lithium bis (trifluoromethyl) sulfonimide-glucose carbon quantum dot solid electrolyte.
Fig. 3 is a polarization curve of a lithium/lithium symmetric battery prepared using a lithium bistrifluoromethylsulfonimide solid electrolyte.
Detailed Description
Preparation of lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dots
1) Adding 1g of lithium bistrifluoromethylsulfonyl imide and 1g of glucose into a beaker respectively, adding 20ml of deionized water for dissolving, and then adding the mixed solution into a hydrothermal reaction kettle;
2) and then placing the hydrothermal reaction kettle in a muffle furnace, heating for 12 hours at the temperature of 200 ℃, and naturally cooling to obtain the lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot aqueous solution.
3) And then placing the lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot aqueous solution in a freeze drying box, freezing to 60 ℃ below zero, keeping for 6 hours, then vacuumizing and keeping for 5Pa, and then closing a compressor to slowly thaw so as to sublimate water to obtain the dried lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot.
Example 1
1) Adding 20mg of prepared lithium bis (trifluoromethyl) sulfonimide-glucose carbon quantum dot powder and 80mg of polyoxyethylene into a mortar for grinding;
2) and then dissolving the ground mixed powder in 10mL of acetonitrile, stirring for 6 hours, pouring into a mold, and performing vacuum drying (at the temperature of 50 ℃) to obtain the lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot solid electrolyte film with the thickness of 60 mu m.
The ionic conductivity of the lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot solid electrolyte at 25 ℃ is tested to be 4.32 multiplied by 10-4S/cm (FIG. 1), and the lithium ion mobility is as high as 0.65 (FIG. 2).
Example 2
1) Adding 20mg of prepared lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot powder and 80mg of poly (1, 3-dioxolane) into a mortar for grinding;
2) and then dissolving the ground mixed powder in 10mL of acetonitrile, stirring for 6 hours, pouring into a mold, and performing vacuum drying (at the temperature of 50 ℃) to obtain the lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot solid electrolyte film with the thickness of 60 mu m.
The ionic conductivity of the lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot solid electrolyte at 25 ℃ is tested to be 3.29 multiplied by 10-5S/cm (FIG. 1), the lithium ion mobility is as high as 0.61.
Comparative example
1) Adding 20mg of lithium bistrifluoromethylsulfonyl imide powder and 80mg of poly (1, 3-dioxolane) into a mortar for grinding;
2) and then dissolving the ground mixed powder in 10mL of acetonitrile, stirring for 6 hours, pouring into a mold, and performing vacuum drying (at the temperature of 50 ℃) to obtain the lithium bis (trifluoromethyl) sulfonyl imide solid electrolyte film with the thickness of 60 mu m.
The ionic conductivity of the lithium bis (trifluoromethyl) sulfonyl imide solid electrolyte film is 1.56 multiplied by 10 under the temperature of 25 DEG C-5S/cm (FIG. 1), and the lithium ion mobility was 0.31 (FIG. 3).
Claims (3)
1. A preparation method of a lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot solid electrolyte comprises a high molecular polymer and a lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot, wherein the high molecular polymer is selected from one of polyoxyethylene or poly 1, 3-dioxolane, and the preparation method of the lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot comprises the following steps:
1) dissolving 5-10 parts of lithium bis (trifluoromethyl) sulfonyl imide and 10 parts of glucose (by weight) in water, and adding the mixed solution into a hydrothermal reaction kettle;
2) placing the hydrothermal reaction kettle in a muffle furnace, heating for 6-24 hours at 200-400 ℃, and naturally cooling to obtain a lithium bis (trifluoromethyl) sulfonimide-glucose carbon quantum dot aqueous solution;
3) and (3) carrying out freeze drying treatment on the lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot aqueous solution to obtain the dried lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dot.
2. The method for producing a solid electrolyte according to claim 1, wherein: the mass ratio of the lithium bistrifluoromethylsulfonyl imide-glucose carbon quantum dots to the high molecular polymer is (3-6): 10.
3. The method for producing a solid electrolyte according to claim 1, wherein: dissolving the prepared lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot powder (3-6 parts) and high polymer powder (10 parts) in an organic solution, heating and stirring for at least 12 hours, pouring into a mold, and performing vacuum drying to obtain the lithium bis (trifluoromethyl) sulfonyl imide-glucose carbon quantum dot solid electrolyte.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112909333A (en) * | 2021-01-19 | 2021-06-04 | 中北大学 | Boron-containing carbon quantum dot nano composite solid electrolyte and preparation method thereof |
| CN114430062A (en) * | 2022-01-24 | 2022-05-03 | 中南大学 | Composite electrolyte based on lithiation carbon point modification and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112909333A (en) * | 2021-01-19 | 2021-06-04 | 中北大学 | Boron-containing carbon quantum dot nano composite solid electrolyte and preparation method thereof |
| CN112909333B (en) * | 2021-01-19 | 2022-08-23 | 中北大学 | Boron-containing carbon quantum dot nano composite solid electrolyte and preparation method thereof |
| CN114430062A (en) * | 2022-01-24 | 2022-05-03 | 中南大学 | Composite electrolyte based on lithiation carbon point modification and preparation method and application thereof |
| CN114430062B (en) * | 2022-01-24 | 2023-10-10 | 中南大学 | Composite electrolyte based on lithiated carbon point modification and preparation method and application thereof |
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