CN112117489A - Solid electrolyte membrane and preparation method and application thereof - Google Patents
Solid electrolyte membrane and preparation method and application thereof Download PDFInfo
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- 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
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- 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
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Abstract
The invention discloses a solid electrolyte membrane and a preparation method and application thereof, wherein the solid electrolyte membrane is prepared from the following components in percentage by mass: 40-69% of polyacrylonitrile, 15-30% of lithium bis (trifluoromethanesulfonyl) imide and Li1.3Al0.3Ti1.7(PO4)31 to 30 percent. The solid electrolyte film prepared by the method can obviously reduce the using amount of the conventional electrolyte, has higher ionic conductivity and electrochemical stability, and improves the cycle performance of the battery. The invention utilizes the film forming property of polymer PAN, the lithium ion conductivity of LiTFSI and the LATP as fillers to improve the electrochemical stability of a solid electrolyte membrane, thereby realizing the starting of the PAN/LiTFSI/LATP composite material membraneThe double functions of the diaphragm and the lithium ion conduction of the lithium ion battery are achieved.
Description
Technical Field
The invention belongs to the technical field of solid lithium ion batteries, and particularly relates to a solid electrolyte membrane and a preparation method and application thereof.
Background
With the increasing demand of clean energy, the lithium ion battery as an efficient energy storage device has the advantages of high output voltage, high specific capacity and the like, and is widely applied to the fields of electric automobiles, large-scale electricity storage and the like. At present, two main components of a diaphragm and electrolyte in a lithium ion battery widely applied to the market play an important role in the electrochemical performance of the battery. However, organic solvents (such as ethylene carbonate, propylene carbonate, dimethyl carbonate, etc.) used for porous polymer separators and organic electrolytes still face challenges in terms of safety performance and high voltage resistance of lithium batteries. The organic liquid electrolyte and the electrode material adopted by the lithium ion battery are easy to generate side reactions in the charging and discharging processes, so that the battery capacity is subjected to irreversible attenuation, and the organic liquid electrolyte can volatilize, dry, leak and the like in the long-term use process, so that the service life of the battery is influenced.
The electrolyte of the lithium ion battery which is commercially used at present mainly comprises liquid electrolyte and gel electrolyte. Both the electrolyte and the carbon nano-tube have higher conductivity, and can well soak electrode material particles and form an electrolyte film layer on the surface of the electrode material. However, the thermal stability of these two electrolytes is to be improved. When the internal or external temperature of the battery increases, the electrochemical reaction speed between the electrolyte and the electrode material is significantly increased, further generating a large amount of heat, eventually leading to thermal runaway. Meanwhile, the organic solvent in the electrolyte is heated to generate a large amount of gas, so that the battery sealing effect is caused, and serious consequences such as fire explosion and the like are generated after the organic solvent is contacted with the outside. In recent years, research on all solid-state lithium batteries with solid electrolyte has found that the solid electrolyte provides a feasible research path for further improving the energy density and safety of the batteries. The solid electrolyte has high ionic conductivity, low electronic conductivity, incombustibility, wide use temperature range, stability in air environment, potential use prospect in various fields such as electrochemical devices, high-energy and high-density batteries, high energy storage and conversion relations and the like, and has attracted extensive attention.
The all-solid-state electrolyte also has some problems in practical application, such as (1) the conductivity of the solid-state electrolyte at room temperature is not high, and the internal resistance of the all-solid-state lithium ion battery is high; (2) due to the inherent particle characteristics of the electrode material and the solid electrolyte, there is severe interfacial resistance between the electrolyte and the electrode material; (3) the micron-sized solid electrolyte membrane is difficult to prepare and form, so that the assembly of the all-solid-state lithium ion battery is difficult to realize, and the practical application of the solid lithium battery is severely restricted.
Disclosure of Invention
The purpose of the invention is as follows: to overcome these disadvantages of the prior art, the present invention provides a solid electrolyte membrane.
The technical problem to be solved by the invention is to provide a preparation method of the solid electrolyte membrane.
The invention finally solves the technical problem of providing the application of the solid electrolyte membrane in preparing the lithium battery.
The technical scheme is as follows: in order to solve the technical problems, the invention provides a solid electrolyte membrane which is prepared from the following components in percentage by mass: 40-69% of Polyacrylonitrile (PAN), 15-30% of lithium bis (trifluoromethane sulfonyl) imide (LiTFSI), and Li1.3Al0.3Ti1.7(PO4)3 (LATP)1～30%。
Wherein the mass average molecular weight of the polyacrylonitrile is 100000-600000.
Wherein, the Li1.3Al0.3Ti1.7(PO4)3The preparation method comprises the following steps: according to Li1.3Al0.3Ti1.7(PO4)3In a stoichiometric ratio of (A), weighing Li2CO3、TiO2、Al2O3、(NH4)2HPO4Mixing, ball milling, and reacting at high temperature and air atmosphere.
The invention also comprises a preparation method of the solid electrolyte membrane, which comprises the following steps:
1) obtaining of LATP suspension: according to Li1.3Al0.3Ti1.7(PO4)3In a stoichiometric ratio of (A), weighing Li2CO3、TiO2、Al2O3、(NH4)2HPO4Mixing, ball-milling and sieving, dispersing the sieved powder in DMF, and performing ultrasonic treatment to form a LATP suspension, which is marked as a solution A;
2) dissolving polyacrylonitrile in DMF, stirring in a dry environment to obtain a PAN/DMF solution, adding lithium bistrifluoromethanesulfonylimide into the PAN/DMF solution, and continuously stirring in the dry environment to obtain a solution B;
3) and mixing the solution A and the solution B, stirring, performing ultrasonic treatment, performing wet coating, and drying to form a film, thus obtaining the solid electrolyte flexible film.
Wherein the ball milling rotation speed in the step 1) is 300-600 rpm, and the ball milling time is 3-6 h.
Wherein, the ball milling in the step 1) is carried out, and then the reaction is carried out for 6-12 h at 850-950 ℃ in an air atmosphere.
Wherein, the step 1) is carried out by sieving with a sieve of 300-500 meshes.
Wherein the ultrasonic power in the step 1) is 800-1200W, and the ultrasonic time is 30-60 min.
Wherein the thickness of the solid electrolyte flexible film is 20-50 μm.
The invention also comprises the application of the solid electrolyte membrane in the preparation of a lithium battery, and particularly the solid electrolyte membrane is assembled into a solid lithium ion battery to test the electrochemical performance.
Has the advantages that: compared with the prior art, the invention has the following advantages: the solid electrolyte film prepared by the method can obviously reduce the using amount of the conventional electrolyte, has higher electrochemical stability and improves the cycle performance of the battery. The invention utilizes the film forming property of polymer PAN, the lithium ion conductivity of LiTFSI and the LATP as fillers to improve the electrochemical stability of the solid electrolyte film, thereby realizing the double functions of the PAN/LiTFSI/LATP composite material film of diaphragm and lithium ion conduction of the lithium ion battery.
Drawings
FIG. 1 photograph of a sample of example 1;
FIG. 2 XRD pattern of the sample of example 1;
FIG. 3 cycle performance of examples 1, 2, 3 and comparative example;
figure 4 XRD pattern of example 3 sample.
Detailed Description
The following are preferred embodiments of the present invention, which are intended to be illustrative only and not limiting, and all modifications thereto which fall within the scope of the appended claims.
PAN was purchased from Shanghai Macklin Biochemical co., ltd., cat # P823208; LiTFSI was purchased from Shanghai Aladdin Biotechnology GmbH under the designation B102576.
Commercial lithium battery diaphragm (Shenzhen, Star Source Material science and technology Co., Ltd., product No. SD 216102) and commercial electrolyte (Zhang, hong, Guotai Huarong, chemical New Material Co., Ltd., product No. NCA)&NCM 811), and a commercial high nickel ternary material LiNi0.8Co0.1Mn0.1O2(Ningbo gold and New materials Co., Ltd., Cat number NCM 811)
Example 1
Preparation of 2g of LATP, according to Li1.3Al0.3Ti1.7(PO4)3In a stoichiometric ratio of (A), weighing Li2CO3、TiO2、Al2O3、(NH4)2HPO4Mixing, ball milling at 360rpm for 4 h, and reacting at 850 deg.C under air atmosphere for 6h to obtain LATP material. Ball-milling the obtained LATP material at 500rpm for 4 h, sieving with a 400-mesh sieve, dispersing the sieved powder in 60 mL DMF, and performing ultrasonic treatment for 40 min to form LATP suspension.
5.6g of PAN (with a mass average molecular weight of 150000) is dissolved in 100mL of DMF, and stirred at 80 ℃ under a dry environment for 5 hours, 2.4g of LiTFSI is added, and stirring is continued at 80 ℃ under a dry environment for 3 hours to obtain a PAN/LiTFSI solution.
Mixing the LATP suspension with the PAN/LiTFSI solution, stirring for 1h, carrying out ultrasonic treatment for 30min, carrying out wet coating, drying at 80 ℃ for 12h, and forming a film to obtain the solid electrolyte flexible film with the thickness of 35 μm.
The photograph of the obtained solid electrolyte flexible film is shown in fig. 1, and the film has flexibility and uniform appearance. The XRD pattern of the composite membrane as shown in figure 2 shows characteristic spectrum peaks of LATP at positions of 14.6 degrees, 21.0 degrees, 24.9 degrees and the like, and a bulge peak of PAN at 17.5 degrees. Soaking the obtained solid electrolyte membrane in commercial electrolyte for 10s, taking out to be used as a diaphragm and electrolysisLiNi, a commercial high-nickel ternary material0.8Co0.1Mn0.1O2The lithium ion battery is assembled by taking the lithium ion battery as a positive electrode and taking metal lithium as a negative electrode, the electrochemical performance is tested, the cycle curve at 0.5C multiplying power is shown in figure 3, and the performance is superior to that of a comparative sample after 100 cycles.
Example 2
Preparation of 1 g of LATP, according to Li1.3Al0.3Ti1.7(PO4)3In a stoichiometric ratio of (A), weighing Li2CO3、TiO2、Al2O3、(NH4)2HPO4Mixing, ball milling at 360rpm for 4 h, and reacting at 850 deg.C under air atmosphere for 6h to obtain LATP material. Ball-milling the obtained LATP material at 500rpm for 4 h, sieving with a 400-mesh sieve, dispersing the sieved powder in 60 mL DMF, and performing ultrasonic treatment for 30min to form LATP suspension.
6.3g of PAN (with a mass average molecular weight of 150000) is dissolved in 100mL of DMF, and stirred at 80 ℃ under a dry environment for 5 hours, 2.7 g of LiTFSI is added, and stirring is continued at 80 ℃ under a dry environment for 3 hours to obtain a PAN/LiTFSI solution.
Mixing the LATP suspension with the PAN/LiTFSI solution, stirring for 1h, carrying out ultrasonic treatment for 30min, carrying out wet coating, drying at 80 ℃ for 12h, and forming a film to obtain the solid electrolyte flexible film with the thickness of 20 microns.
Soaking the obtained solid electrolyte membrane in commercial electrolyte for 10s, taking out the solid electrolyte membrane as a diaphragm and an electrolyte, and mixing the solid electrolyte membrane with commercial high-nickel ternary material LiNi0.8Co0.1Mn0.1O2A lithium ion battery was assembled as a positive electrode and metal lithium as a negative electrode, and electrochemical performance was measured, and a cycle curve at 0.5C-rate is shown in fig. 3, and after 100 cycles, the cycle performance of this sample was lower than that of the sample of example 1.
Example 3
Preparation of 3g of LATP, according to Li1.3Al0.3Ti1.7(PO4)3In a stoichiometric ratio of (A), weighing Li2CO3、TiO2、Al2O3、(NH4)2HPO4Mixing at 360rpm, ball milling for 4 h, and then reacting for 6h at 850 ℃ under an air atmosphere to obtain the LATP material. Ball-milling the obtained LATP material at 500rpm for 4 h, sieving with a 400-mesh sieve, dispersing the sieved powder in 60 mL of DMF, and performing ultrasonic treatment for 60min to form LATP suspension.
4.9g of PAN (with a mass average molecular weight of 150000) is dissolved in 100mL of DMF, and stirred at 80 ℃ under a dry environment for 5 hours, 2.1 g of LiTFSI is added, and stirring is continued at 80 ℃ under a dry environment for 3 hours to obtain a PAN/LiTFSI solution.
Mixing the LATP suspension with the PAN/LiTFSI solution, stirring for 1h, carrying out ultrasonic treatment for 30min, carrying out wet coating, drying at 80 ℃ for 12h, and forming a film to obtain the solid electrolyte flexible film with the thickness of 50 μm. The XRD pattern of the composite membrane shows characteristic peaks of LATP at positions of 14.6 degrees, 21.0 degrees, 24.9 degrees and the like and a bulge peak of PAN at 17.5 degrees as shown in figure 4.
Soaking the obtained solid electrolyte membrane in commercial electrolyte for 10s, taking out the solid electrolyte membrane as a diaphragm and an electrolyte, and mixing the solid electrolyte membrane with commercial high-nickel ternary material LiNi0.8Co0.1Mn0.1O2A lithium ion battery was assembled as a positive electrode and metal lithium as a negative electrode, and electrochemical performance was measured, and a cycle curve at 0.5C magnification is shown in fig. 3, and the cycle performance of this sample was lower than that of the sample of example 1.
Comparative example 1
A commercial diaphragm (Celgard 2500), a commercial electrolyte (Thailand Rong chemical new material Co., Ltd., Zhang Jia gang City), and a commercial high-nickel ternary material LiNi0.8Co0.1Mn0.1O2(Ningbo gold and New materials Co., Ltd.) as a positive electrode, metallic lithium as a negative electrode, and 3 times the amount of the electrolyte added as in example 1. The lithium ion battery is assembled, the electrochemical performance is tested, and the cycle curve at 0.5C multiplying power is shown in figure 3. The initial specific capacity was close to example 1, but both the cycling performance and the coulombic efficiency were lower than example 1.
Claims (10)
1. The solid electrolyte membrane is characterized by comprising the following components in percentage by mass: 40-69% of polyacrylonitrile and lithium bis (trifluoromethanesulfonyl) imide15～30%、Li1.3Al0.3Ti1.7(PO4)3 1～30%。
2. The solid electrolyte membrane according to claim 1, wherein the mass average molecular weight of the polyacrylonitrile is 100000 to 600000.
3. The solid electrolyte membrane according to claim 1 or 2, wherein the Li is1.3Al0.3Ti1.7(PO4)3The preparation method comprises the following steps: according to Li1.3Al0.3Ti1.7(PO4)3In a stoichiometric ratio of (A), weighing Li2CO3、TiO2、Al2O3、(NH4)2HPO4Mixing, ball milling, and reacting at high temperature and air atmosphere.
4. The method for producing a solid electrolyte membrane according to any one of claims 1 to 3, characterized by comprising the steps of:
1) obtaining of LATP suspension: according to Li1.3Al0.3Ti1.7(PO4)3In a stoichiometric ratio of (A), weighing Li2CO3、TiO2、Al2O3、(NH4)2HPO4Mixing, ball-milling and sieving, dispersing the sieved powder in DMF, and performing ultrasonic treatment to form a LATP suspension, which is marked as a solution A;
2) dissolving polyacrylonitrile in DMF, stirring in a dry environment to obtain a PAN/DMF solution, adding lithium bistrifluoromethanesulfonylimide into the PAN/DMF solution, and continuously stirring in the dry environment to obtain a solution B;
3) and mixing the solution A and the solution B, stirring, performing ultrasonic treatment, performing wet coating, and drying to form a film, thus obtaining the solid electrolyte flexible film.
5. The preparation method of the solid electrolyte membrane according to claim 4, wherein the ball milling rotation speed in the step 1) is 300-600 rpm, and the ball milling time is 3-6 h.
6. The method for preparing a solid electrolyte membrane according to claim 4, wherein the reaction is carried out at 850-950 ℃ in an air atmosphere for 6-12 h after the ball milling in the step 1).
7. The method for producing a solid electrolyte membrane according to claim 4, wherein the step 1) is performed by sieving with a 300-500 mesh sieve.
8. The preparation method of the solid electrolyte membrane according to claim 4, wherein the ultrasonic power in the step 1) is 800-1200W, and the ultrasonic time is 30-60 min.
9. The method for producing a solid electrolyte membrane according to claim 4, wherein the solid electrolyte flexible film has a thickness of 20 to 50 μm.
10. Use of the solid electrolyte membrane according to claim 1 or 2 for the production of a lithium battery.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112968179A (en) * | 2021-02-04 | 2021-06-15 | 珠海冠宇电池股份有限公司 | Current collector composite film and solid-state battery |
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| CN109638349A (en) * | 2018-12-04 | 2019-04-16 | 中国科学院山西煤炭化学研究所 | A kind of organic-inorganic nanocomposite solid electrolyte diaphragm and its preparation method and application |
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| KR20180072111A (en) * | 2016-12-21 | 2018-06-29 | 울산과학기술원 | Composite electolyte, method for manufacturing the same, and rechargeable battery comprising the same |
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| CN108539260A (en) * | 2018-04-13 | 2018-09-14 | 中国航发北京航空材料研究院 | With multiple Li+Compound organic solid electrolyte of conduction path and preparation method thereof |
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| 李超乐 等: "PAN-LATP复合固态电解质的制备与性能标准", 《中国科学：化学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112968179A (en) * | 2021-02-04 | 2021-06-15 | 珠海冠宇电池股份有限公司 | Current collector composite film and solid-state battery |
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