CN110828890B - Preparation method of polymer-based solid electrolyte with high room-temperature ionic conductivity - Google Patents
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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Abstract
The invention discloses a preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity. According to the invention, through carrying a large amount of lithium salt polymerizable epoxy monomers, and utilizing the in-situ polymerization of the epoxy monomers and a polymer matrix (polyvinylidene fluoride, polyvinylidene fluoride perfluoropropylene or polyethylene oxide), the crystallinity and the glass transition temperature of the solid electrolyte are reduced, the movement capacity of a molecular chain is improved, and the transmission efficiency of lithium ions in the solid electrolyte is improved. The polymer-based solid electrolyte prepared by the invention has ultrahigh lithium salt loading capacity, ultralow glass transition temperature, excellent ionic conductivity, light weight and good flexibility. After assembly into a lithium ion battery, the operating temperature of the all solid-state lithium ion battery was reduced to 50 ℃.
Description
Technical Field
The invention relates to the technical field of lithium ion solid electrolytes, in particular to a preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity.
Background
The lithium ion battery comprises a liquid Lithium Ion Battery (LIB) and a polymer lithium ion battery (PLB) at present, wherein the liquid lithium ion battery uses a liquid electrolyte, and the polymer lithium ion battery is replaced by a solid polymer electrolyte.
The existing polymer-based solid electrolyte mostly adopts polyvinylidene fluoride (PVDF), polyethylene oxide (PEO) and Polyurethane (PU) as matrixes, is mixed with lithium salt and then is coated to form a film, the lithium salt is uniformly dispersed in the polymer by means of the interaction force formed by an electrolyte active substance and the polymer, and the lithium ion transmission is realized by utilizing the movement of a polymer molecular chain. However, since the glass transition temperature of the polymer is high, the molecular chain movement is difficult at normal temperature, and the crystallinity of the polymer is high, so that the holding amount of lithium salt in the polymer is not high, the ionic conductivity of the polymer-based solid electrolyte at room temperature is low, and the room-temperature electrical performance of the solid battery is also low, which is not beneficial to practical application.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity aiming at the defect of low ionic conductivity of the existing solid electrolyte.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity comprises the following preparation steps:
s1, preparing a matrix solution: dissolving a polymer matrix in a good solvent to prepare a matrix solution with a certain concentration.
S2, preparing a functional monomer solution: dissolving a certain amount of lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) in a functional monomer to form a LiTFSI/functional monomer solution; taking a certain amount of aluminum tris (triflate) ((CF) 3 SO 3 ) 3 Al) is dissolved in the functional monomer to form (CF) 3 SO 3 ) 3 Al/functional monomer solution.
S3, preparing precursor liquid: mixing the LiTFSI/functional monomer solution in S2 with (CF) 3 SO 3 ) 3 And uniformly mixing the Al/functional monomer solution according to a certain proportion to form a mixed solution, and then adding the mixed solution into the polymer matrix solution in the step S1 to be uniformly stirred to prepare a precursor solution.
S4, preparing a solid electrolyte membrane: and (4) coating the precursor solution in the step (S3) on a lithium sheet, and then drying the lithium sheet coated with the precursor solution to obtain the polymer-based solid electrolyte membrane with high room-temperature ionic conductivity.
Further, the polymer matrix of S1 is one or more of polyvinylidene fluoride (PVDF), polyvinylidene fluoride perfluoropropylene (PVDF-HFP) or polyethylene oxide (PEO).
Further, the good solvent of S1 is acetone, N-dimethylformamide or deionized water. Preferably, when the polymer is polyethylene oxide (PEO), deionized water is used as the good solvent. When the polymer matrix is polyvinylidene fluoride (PVDF) or polyvinylidene fluoride perfluoropropylene (PVDF-HFP), acetone is adopted as a good solvent.
Further, the concentration of the base solution in S1 is 10 to 50wt.%. Preferably, S1 the matrix solution concentration is.
Further, the functional monomer S2 is one or more of 1, 3-Dioxolane (DOL), glycidol and propylene oxide.
Further, the molar concentration of LiTFSI in the mixed solution of S3 is 0.5 to 5mol/L (CF) 3 SO 3 ) 3 The molar concentration of Al is 0.5 to 3mmol/L. Preferably, the molar concentration of LiTFSI in the mixed solution of S3 is 2.0mol/L, (CF) 3 SO 3 ) 3 The molar concentration of Al was 2.0mmol/L.
Further, the stirring time in S3 is 3 to 12h, so that the components are uniformly dispersed and reacted. Preferably, the stirring time in S3 is 8h.
Further, the volume ratio of the mixed solution of S3 to the polymer matrix solution is 1. According to the invention, the polymerizable epoxy resin carrying lithium salt is added into the polymer matrix, so that the crystallinity and the glass transition temperature of the polymer-based solid electrolyte can be reduced, and the transmission efficiency of lithium ions in the solid electrolyte can be improved. Preferably, the volume ratio of the mixed solution of S3 to the polymer matrix solution is 1.
And further, the precursor solution S4 is coated on a lithium sheet by a spin coating method, the rotation speed of the spin coating is 1800 to 2300r/min, and the thickness of the spin coating is 10 to 100 mu m.
Further, the drying temperature of S4 is 40 to 50 ℃, and the drying time is 1 to 5h. Preferably, the drying temperature of S4 is 45 ℃, and the drying time is 3h.
Further, the water oxygen index of inert gas in the operating environment of S1-S4 is less than 1ppm.
Compared with the prior art, the beneficial effects are:
the invention creatively adds the polymerizable epoxy monomer carrying a large amount of lithium salt into the matrix of the solid electrolyte, and the solid electrolyte has extremely low crystallinity and glass transition temperature through the polymerization of the epoxy monomer and the uniform dispersion of the epoxy monomer and the polymer matrix (polyvinylidene fluoride (PVDF), polyvinylidene fluoride perfluoropropylene (PVDF-HFP) or polyethylene oxide (PEO)), thereby being beneficial to improving the movement capability of a molecular chain and improving the transmission efficiency of lithium ions in the solid electrolyte. Meanwhile, the polymer matrix provides guarantee for the mechanical strength of the polyepoxy resin. The polymer-based solid electrolyte prepared by the invention has ultrahigh lithium salt loading capacity, ultralow glass transition temperature and excellent ionic conductivity, is light, thin and good in flexibility, and the working temperature of the all-solid-state lithium ion battery is reduced to 50 ℃ after the polymer-based solid electrolyte is assembled into the lithium ion battery.
Detailed Description
The following examples are further explained and illustrated, but the present invention is not limited in any way by the specific examples. Unless otherwise indicated, the methods and equipment used in the examples are conventional in the art and the starting materials used are conventional commercially available materials.
Example 1
The embodiment provides a preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity, which comprises the following steps:
s1, preparing a matrix solution: polyvinylidene fluoride (PVDF) was dissolved in acetone to prepare a 10wt.% polyvinylidene fluoride (PVDF) solution.
S2, preparing a functional monomer solution: dissolving a certain amount of lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) in a 1, 3-Dioxolane (DOL) monomer to prepare a LiTFSI/1, 3-Dioxolane (DOL) solution, and taking aluminum tris (trifluorosulfonate) ((CF) 3 SO 3 ) 3 Al) is dissolved in 1, 3-Dioxolane (DOL) monomer to prepare (CF) 3 SO 3 ) 3 Al/1, 3-Dioxolane (DOL) solution.
S3, preparing precursor liquid: the LiTFSI/1, 3-Dioxopentacyclic (DOL) solution described in S2 and (CF) are added 3 SO 3 ) 3 Mixing Al/1, 3-Dioxolane (DOL) solution uniformly to form a mixed solution, wherein the molar concentration of LiTFSI in the solution is 0.5mol/L, (CF) 3 SO 3 ) 3 And the molar concentration of Al is 0.5mmol/L, and then the mixed solution is added into the polymer matrix solution in the S1 and is uniformly stirred to prepare a precursor solution, wherein the volume ratio of the mixed solution to the polymer matrix solution is 1.
S4, preparing a solid electrolyte membrane: and (3) performing spin coating on the precursor liquid in the S3 on a lithium sheet by using a spin coater at the rotating speed of 2000r/min for 10 mu m of precursor liquid, and then performing heat preservation on the lithium sheet coated with the precursor liquid at 50 ℃ for 1h to obtain the polymer-based solid electrolyte membrane with room temperature and high ionic conductivity.
All the operations are carried out in an inert gas atmosphere.
Example 2
The embodiment provides a preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity, which comprises the following preparation steps:
s1, preparing a matrix solution: polyvinylidene fluoride perfluoropropylene (PVDF-HFP) was dissolved in N, N-dimethylformamide to make a 10wt.% polyvinylidene fluoride (PVDF) solution.
S2, preparing a functional monomer solution: dissolving a certain amount of lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) in a 1, 3-Dioxolane (DOL) monomer to prepare a LiTFSI/1, 3-Dioxolane (DOL) solution, and taking aluminum tris (trifluorosulfonate) ((CF) 3 SO 3 ) 3 Al) is dissolved in 1, 3-Dioxolane (DOL) monomer to prepare (CF) 3 SO 3 ) 3 Al/1, 3-Dioxolane (DOL) solution.
S3, preparing precursor liquid: the LiTFSI/1, 3-Dioxopentacyclic (DOL) solution described in S2 and (CF) are added 3 SO 3 ) 3 Mixing Al/1, 3-Dioxolane (DOL) solution uniformly to form a mixed solution, wherein the molar concentration of LiTFSI in the solution is 5mol/L, (CF) 3 SO 3 ) 3 And the molar concentration of Al is 3mmol/L, and then the mixed solution is added into the polymer matrix solution in the S1 and is uniformly stirred to prepare a precursor solution, wherein the volume ratio of the mixed solution to the polymer matrix solution is 1.
S4, preparing a solid electrolyte membrane: and (4) spin-coating a layer of precursor liquid on the lithium sheet by using the precursor liquid in the S3 at the rotating speed of 2000r/min by using a spin coater, and then keeping the temperature of the lithium sheet coated with the precursor liquid at 40 ℃ for 5 hours to obtain the polymer-based solid electrolyte membrane with the room-temperature high ionic conductivity.
Example 3
The embodiment provides a preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity, which comprises the following preparation steps:
s1, preparing a matrix solution: polyethylene oxide (PEO) was dissolved in deionized water to make a 50wt.% polyethylene oxide (PEO) solution.
S2, preparing a functional monomer solution: dissolving a certain amount of lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) in a propylene oxide monomer to prepare a LiTFSI/propylene oxide solution, and taking aluminum tris (trifluorosulfonate) ((CF) 3 SO 3 ) 3 Al) is dissolved in a propylene oxide monomer to prepare (CF) 3 SO 3 ) 3 Al/propylene oxide solution.
S3, preparing precursor liquid: mixing the LiTFSI/propylene oxide solution in S2 with (CF) 3 SO 3 ) 3 The Al/propylene oxide solution is evenly mixed to form a mixed solution, and the molar concentration of the LiTFSI in the solution is 5mol/L ((CF) 3 SO 3 ) 3 Al) is 3mmol/L, and then the mixed solution is added into the polymer matrix solution in S1 and uniformly stirred to prepare precursor solution, wherein the volume ratio of the mixed solution to the polymer matrix solution is 1.
S4, preparing a solid electrolyte membrane: and (3) spinning a layer of precursor liquid on the lithium sheet by using the spinning machine at the rotating speed of 2000r/min, and then keeping the temperature of the lithium sheet coated with the precursor liquid at 50 ℃ for 1h to obtain the polymer-based solid electrolyte membrane with room temperature and high ionic conductivity.
Example 4
The embodiment provides a preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity, which comprises the following preparation steps:
s1, preparing a matrix solution: polyvinylidene fluoride (PVDF) was dissolved in acetone to prepare a 10wt.% polyvinylidene fluoride (PVDF) solution.
S2, preparing a functional monomer solution: dissolving a certain amount of lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) in a 1, 3-Dioxolane (DOL) monomer to prepare a LiTFSI/1, 3-Dioxolane (DOL) solution, and taking aluminum tris (trifluorosulfonate) ((CF) 3 SO 3 ) 3 Al is dissolved in 1, 3-Dioxypentacyclic (DOL) monomer to prepare (A), (B), (C) and (C)CF 3 SO 3 ) 3 Al)/1, 3-Dioxolane (DOL) solution.
S3, preparing precursor liquid: mixing the solution of LiTFSI/1, 3-Dioxolane (DOL) in S2 with (CF) 3 SO 3 ) 3 Mixing Al/1, 3-Dioxolane (DOL) solution uniformly to form a mixed solution, wherein the molar concentration of LiTFSI in the solution is 2.0mol/L, (CF) 3 SO 3 ) 3 And the molar concentration of Al is 2.0mmol/L, and then the mixed solution is added into the polymer matrix solution in S1 and uniformly stirred to prepare a precursor solution, wherein the volume ratio of the mixed solution to the polymer matrix solution is 1.
S4, preparing a solid electrolyte membrane: and (3) performing spin coating on the precursor liquid in the S3 on a lithium sheet by using a spin coater at the rotating speed of 2000r/min to obtain a precursor liquid with the size of 28 microns, and then performing heat preservation on the lithium sheet coated with the precursor liquid at the temperature of 45 ℃ for 3 hours to obtain the polymer-based solid electrolyte membrane with the room temperature and the high ionic conductivity.
Comparative example 1
This comparative example is identical to example 4 except that it directly combines lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) and aluminum tris (triflate) ((CF) 3 SO 3 ) 3 Al) was added to the polymer matrix without the addition of epoxy monomers.
Comparative example 2
This comparative example is prepared by the same procedure as example 4, except that no LiTFSI/1, 3-Dioxolane (DOL) solution is added.
Comparative example 3
This comparative example was prepared by the same procedure as example 4 except that (CF) was not added 3 SO 3 ) 3 Al/1, 3-Dioxolane (DOL) solution.
Examples of the experiments
1. Polymer-based solid electrolyte Performance detection
The polymer-based solid electrolytes prepared according to example 4 and comparative examples 1 to 3 were tested for lithium salt loading, mechanical strength, glass transition temperature, and ionic conductivity at room temperature, and the test results are shown in table 1:
TABLE 1
| Item | Lithium salt loading | Mechanical Strength (MPa) | Glass transition temperature (. Degree. C.) | Ionic conductivity of |
| Example 4 | 2 | 0.6 | -40 | 7.8×10 -4 |
| Comparative example 1 | 0.5 | 0.2 | -23 | 9.6×10 -5 |
| Comparative example 2 | 1 | 0.4 | -15 | 2.2×10 -4 |
| Comparative example 3 | 5 | 0.3 | -36 | 5.3×10 -4 |
2. Lithium battery performance detection
After assembling the lithium battery with the polymer-based solid electrolyte prepared in example 4 and comparative examples 1 to 3, the working temperature of the lithium battery was measured, and the measurement results are shown in table 2:
TABLE 2
| Item | Working temperature (. Degree.C.) |
| Example 4 | 50 |
| Comparative example 1 | 70 |
| Comparative example 2 | 65 |
| Comparative example 3 | 60 |
As shown in tables 1 and 2, the polymer-based solid electrolyte prepared by the method of the present invention has significantly improved mechanical strength and ionic conductivity, decreased glass transition temperature, and decreased battery operating temperature by 50 ℃.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (7)
1. A preparation method of a polymer-based solid electrolyte with high room-temperature ionic conductivity is characterized by comprising the following preparation steps:
s1, preparing a matrix solution: dissolving a polymer matrix in a good solvent, and preparing a polymer matrix solution with a certain concentration;
s2, preparing a functional monomer solution: dissolving a certain amount of lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) in a functional monomer to form a LiTFSI/functional monomer solution; taking a certain amount of aluminum tris (triflate) ((CF) 3 SO 3 ) 3 Al) in a functional monomer to form (CF) 3 SO 3 ) 3 Al/functional monomer solution;
s3, preparing precursor liquid: mixing the LiTFSI/functional monomer solution in S2 with (CF) 3 SO 3 ) 3 Uniformly mixing Al/functional monomer solution according to a certain proportion to form mixed solution, and then adding the mixed solution into the polymer matrix solution in the step (1) and uniformly stirring to prepare precursor solution;
s4, preparing a solid electrolyte membrane: coating the precursor solution in the step S3 on a lithium sheet, and then drying the lithium sheet coated with the precursor solution to obtain a polymer-based solid electrolyte membrane with room-temperature high ionic conductivity;
wherein, the operations of the steps S1 to S4 are all carried out in an inert gas environment;
s1, the polymer matrix is one or more of polyvinylidene fluoride (PVDF), polyvinylidene fluoride perfluoropropylene (PVDF-HFP) or polyethylene oxide (PEO);
s1, the good solvent is one or more of acetone, N-dimethylformamide and deionized water;
s2, the functional monomer is one or more of 1, 3-Dioxolane (DOL) or propylene oxide and glycidol;
s3, the molar concentration of the LiTFSI in the mixed solution/the functional monomer solution is 0.5 to 5mol/L; in mixed liquor (CF) 3 SO 3 ) 3 Al/functional monomer solution (CF) 3 SO 3 ) 3 The molar concentration of Al is 0.5 to 3mM.
2. The method for preparing a polymer-based solid electrolyte with high ionic conductivity at room temperature as claimed in claim 1, wherein the mass concentration of the matrix S1 is 10 to 50wt.%.
3. The method according to claim 1, wherein the molar concentration of LiTFSI in the mixed solution of S3 is 2.0mol/L; (CF) 3 SO 3 ) 3 The molar concentration of Al is 2.0mM; and in S3, the stirring time is 3 to 12h.
4. The method for preparing a polymer-based solid electrolyte with high ionic conductivity at room temperature according to claim 1, wherein the volume ratio of the mixed solution of S3 to the polymer matrix solution is 1.
5. The method for preparing a polymer-based solid electrolyte with high ionic conductivity at room temperature according to claim 1, wherein the precursor solution of S4 is coated on a lithium plate by a spin coating method; the rotation speed of the spin coating is 1800 to 2300r/min, and the thickness of the spin coating is 10 to 100 mu m.
6. The method for producing a polymer-based solid electrolyte having high ionic conductivity at room temperature as claimed in claim 1, wherein the drying temperature in S4 is from 40 ℃ to 50 ℃ and the drying time is from 1 to 5 hours.
7. The method for preparing a polymer-based solid electrolyte with high ionic conductivity at room temperature according to claim 1, wherein the water oxygen index of the inert gas in the operating environment is less than 1ppm.
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