CN108461815B - ECO-based solid polyelectrolyte and preparation method thereof - Google Patents
ECO-based solid polyelectrolyte and preparation method 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
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Abstract
The invention discloses an ECO-based solid polyelectrolyte which is characterized in that: the solid polyelectrolyte comprises epichlorohydrin rubber, lithium salt, polyvinylidene fluoride and fast ion conductor ceramic powder, wherein the mass parts of the components are respectively as follows: 50-80 parts of epichlorohydrin rubber, 5-40 parts of lithium salt, 0-50 parts of polyvinylidene fluoride and 5-30 parts of fast ion conductor ceramic powder. A preparation method of an ECO-based solid polyelectrolyte comprises the following preparation steps: dissolving and dispersing materials; mixing materials; and (4) film forming. The advantages are that: the epichlorohydrin rubber is used as a matrix, and is a rubber material at room temperature, so that the epichlorohydrin rubber has good mechanical properties; the blend with polyvinylidene fluoride can further reduce the regularity of the epichlorohydrin rubber, and the mechanical property of the system can be adjusted by adjusting the addition amount of the polyvinylidene fluoride.
Description
Technical Field
The invention relates to the field of design and preparation of electrolyte materials of lithium ion batteries, relates to an ECO-based solid polyelectrolyte, and further relates to a preparation method of the ECO-based solid polyelectrolyte.
Background
The solid polyelectrolyte battery has the advantages of high specific energy, no liquid leakage, no flammability, simple structure, capability of being made into ultrathin batteries with any shapes, and the like, and is concerned. In 1973, Wright et al discovered that polyether alkali metal salt complexes have higher ionic conductivity, and solid polymer electrolytes based on polyethylene oxide (PEO) were extensively and extensively studied. Because PEO is a crystalline polymer and is crystalline at room temperature, the presence of the crystalline phase results in a low conductivity at room temperature, at 10-7-10- 8The range of S/cm is difficult to be practically applied. People reduce the proportion of a crystallization area by various methods such as blending, grafting, crosslinking, inorganic particle doping and the like to improve the room-temperature conductivity of the material, but all the methods cannot meet the practical requirements.
Therefore, a new technique is sought to solve the above problems.
Disclosure of Invention
The purpose of the invention is: in order to overcome the defects, the ECO-based solid polyelectrolyte and the preparation method thereof are provided.
In order to achieve the purpose, the invention adopts the technical scheme that:
the ECO-based solid polyelectrolyte comprises epichlorohydrin rubber, lithium salt, polyvinylidene fluoride and fast ion conductor ceramic powder, wherein the ECO-based solid polyelectrolyte comprises the following components in parts by weight: 50-80 parts of epichlorohydrin rubber, 5-40 parts of lithium salt, 0-50 parts of polyvinylidene fluoride and 5-30 parts of fast ion conductor ceramic powder.
The chlorine content in the epichlorohydrin rubber is 15-30.
The lithium salt comprises one or more of lithium perchlorate, lithium hexafluoroarsenate, lithium tetrafluoroborate, lithium hexafluorophosphate, lithium trifluoromethanesulfonate, lithium bistrifluoromethanesulfonylimide, lithium bistrifluoromethylsulfonyl imide and lithium bisoxalatoborate.
The weight average molecular weight of the polyvinylidene fluoride is 5.0 multiplied by 104-8.0×106。
The fast ion conductor ceramic powder is Li7La3Zr2O12(LLZO)、LixLa2/3-xTiO3(LLTO)、 Li1+ xAlxTi2-x(PO4)3(LLZO)、LiAlO2(LAO)、Li7-xLa3Zr2-xMxO12(M＝Ta,Nb)(0.25 ﹤X﹤2)(LLZMO)、Li7+xGexP3-xS11(LGPS) and the like.
A preparation method of an ECO-based solid polyelectrolyte comprises the following preparation steps: the method comprises the following steps: dissolution and dispersion of materials: respectively dispersing epichlorohydrin rubber, lithium salt and polyvinylidene fluoride in an N-methyl pyrrolidone solution, stirring until the epichlorohydrin rubber, the lithium salt and the polyvinylidene fluoride are completely dissolved, then dispersing fast ion conductor ceramic powder in the N-methyl pyrrolidone solution, and stirring until the fast ion conductor ceramic powder is uniformly dispersed; step two: mixing materials: quantitatively mixing the four solutions and the dispersion liquid, and stirring until the four solutions and the dispersion liquid are uniformly dispersed; step three: film forming: and pouring the mixed solution on a flat polytetrafluoroethylene plate, baking for 24 hours at 80 ℃, and then placing the sample in a vacuum oven at 80 ℃ for drying for 24 hours to remove the residual solvent, thereby obtaining the solid polymer electrolyte film.
Compared with the prior art, the invention achieves the technical effects that: the solid polymer electrolyte provided by the invention takes the epichlorohydrin rubber as a matrix, and the epichlorohydrin rubber is a rubber material at room temperature, so that the solid polymer electrolyte has good mechanical properties; the epichlorohydrin rubber is copolymerized by epichlorohydrin and ethylene oxide, a large amount of EO units can be well dissolved, and lithium salt is complexed; the random copolymerization of CO units in EO can destroy the regularity of EO units, prevent the EO units from crystallizing and ensure that the EO units have good conductivity at room temperature; in addition, the blend is blended with polyvinylidene fluoride to further reduce the regularity of the epichlorohydrin rubber, and the mechanical property of the system can be adjusted by adjusting the addition amount of the polyvinylidene fluoride; the addition of the fast ion conductor ceramic powder increases the disorder degree of the polymer electrolyte, provides a new ion transmission channel and improves the room temperature conductivity of the system.
Detailed Description
The invention is further described below with reference to the following examples:
the first embodiment is as follows:
the ECO-based solid polyelectrolyte comprises epichlorohydrin rubber, lithium salt, polyvinylidene fluoride and fast ion conductor ceramic powder, wherein the ECO-based solid polyelectrolyte comprises the following components in parts by weight: 50 parts of epichlorohydrin rubber, 30 parts of lithium salt, 15 parts of polyvinylidene fluoride and 5 parts of fast ion conductor ceramic powder.
The chlorine content in the epichlorohydrin rubber was 15.
The lithium salt comprises one or more of lithium perchlorate, lithium hexafluoroarsenate, lithium tetrafluoroborate, lithium hexafluorophosphate, lithium trifluoromethanesulfonate, lithium bistrifluoromethanesulfonylimide, lithium bis (trifluoromethylsulfonyl) imide and lithium bistrifluoromethanesulfonylimide, and is preferably lithium bistrifluoromethanesulfonylimide.
The weight average molecular weight of the polyvinylidene fluoride is 5.0 multiplied by 104-8.0×106。
The fast ion conductor ceramic powder is Li7La3Zr2O12(LLZO)、LixLa2/3-xTiO3(LLTO)、 Li1+ xAlxTi2-x(PO4)3(LLZO)、LiAlO2(LAO)、Li7-xLa3Zr2-xMxO12(M＝Ta,Nb)(0.25 ﹤X﹤2)(LLZMO)、Li7+xGexP3-xS11(LGPS) and the like, preferably Li7La3Zr2O12(LLZO)。
A preparation method of an ECO-based solid polyelectrolyte comprises the following preparation steps: the method comprises the following steps: dissolution and dispersion of materials: respectively dispersing 50 parts of epichlorohydrin rubber, 30 parts of lithium bistrifluoromethanesulfonylimide and 15 parts of polyvinylidene fluoride in N-methylpyrrolidone solution, wherein the N-methylpyrrolidone solution for dissolving the epichlorohydrin rubber is 190 parts, the N-methylpyrrolidone solution for dissolving the lithium bistrifluoromethanesulfonylimide is 10 parts, and the N-methylpyrrolidone solution for dissolving the polyvinylidene fluoride is 100 parts, stirring until the materials are completely dissolved, and then stirring 5 parts of fast ion conductor ceramic powder Li7La3Zr2O12(LLZO) dispersing in 9 parts of N-methylpyrrolidone solution, and stirring until the dispersion is uniform; step two: mixing materials: quantitatively mixing the four solutions and the dispersion liquid, and stirring until the four solutions and the dispersion liquid are uniformly dispersed; step three: film forming: and pouring the mixed solution on a flat polytetrafluoroethylene plate, baking for 24 hours at 80 ℃, and then placing the sample in a vacuum oven at 80 ℃ for drying for 24 hours to remove the residual solvent, thereby obtaining the solid polymer electrolyte film.
The invention also discloses a preparation method of the solid lithium ion battery, which comprises the following steps: the method comprises the following steps: preparing a positive electrode: subjecting LiCoO to condensation2The conductive adhesive comprises epichlorohydrin rubber, conductive carbon black, polyvinylidene fluoride and lithium salt according to a mass ratio of 80: 10: 3: 3: 4, adding solvent N-methyl pyrrolidone, stirring to obtain uniform slurry, and coating the slurry on an aluminum foil by a doctor blade method, wherein the surface density is 10mg/cm2And drying at 105 ℃ for 12 hours, rolling and cutting to obtain the positive pole piece. Drying in a vacuum box at 120 deg.C for 24 hr.
(2) And (3) taking a metal lithium sheet as a negative electrode material, assembling and fastening the positive electrode sheet, the ECO-based solid polyelectrolyte film and the negative electrode sheet, and testing by an Analgi testing system.
Example two:
the ECO-based solid polyelectrolyte comprises epichlorohydrin rubber, lithium salt, polyvinylidene fluoride and fast ion conductor ceramic powder, wherein the ECO-based solid polyelectrolyte comprises the following components in parts by weight: 60 parts of epichlorohydrin rubber, 20 parts of lithium salt, 10 parts of polyvinylidene fluoride and 10 parts of fast ion conductor ceramic powder.
The chlorine content in the epichlorohydrin rubber was 25.
The lithium salt comprises one or more of lithium perchlorate, lithium hexafluoroarsenate, lithium tetrafluoroborate, lithium hexafluorophosphate, lithium trifluoromethanesulfonate, lithium bistrifluoromethanesulfonylimide, lithium bis (trifluoromethylsulfonyl) imide and lithium bis (oxalato) borate, and the preferred lithium salt is lithium bis (trifluoromethylsulfonyl) imide.
The weight average molecular weight of the polyvinylidene fluoride is 5.0 multiplied by 104-8.0×106。
The fast ion conductor ceramic powder is Li7La3Zr2O12(LLZO)、LixLa2/3-xTiO3(LLTO)、 Li1+ xAlxTi2-x(PO4)3(LLZO)、LiAlO2(LAO)、Li7-xLa3Zr2-xMxO12(M＝Ta,Nb)(0.25 ﹤X﹤2)(LLZMO)、Li7+xGexP3-xS11(LGPS) and the like, preferably LixLa2/3-xTiO3(LLTO)。
A preparation method of an ECO-based solid polyelectrolyte comprises the following preparation steps: the method comprises the following steps: dissolution and dispersion of materials: respectively dispersing 60 parts of epichlorohydrin rubber, 20 parts of lithium bis (trifluoromethylsulfonyl) imide and 10 parts of polyvinylidene fluoride in N-methylpyrrolidone solution, wherein the N-methylpyrrolidone solution for dissolving the epichlorohydrin rubber is 190 parts, the N-methylpyrrolidone solution for dissolving the lithium bis (trifluoromethylsulfonyl) imide is 10 parts, the N-methylpyrrolidone solution for dissolving the polyvinylidene fluoride is 100 parts, stirring until the materials are completely dissolved, and then stirring 5 parts of fast ion solutionConductive ceramic powder LixLa2/3-xTiO3(LLTO) is dispersed in 9 parts of N-methyl pyrrolidone solution and stirred until the dispersion is uniform; step two: mixing materials: quantitatively mixing the four solutions and the dispersion liquid, and stirring until the four solutions and the dispersion liquid are uniformly dispersed; step three: film forming: and pouring the mixed solution on a flat polytetrafluoroethylene plate, baking for 24 hours at 80 ℃, and then placing the sample in a vacuum oven at 80 ℃ for drying for 24 hours to remove the residual solvent, thereby obtaining the solid polymer electrolyte film.
The invention also discloses a preparation method of the solid lithium ion battery, which is the same as the first embodiment.
Example three:
the ECO-based solid polyelectrolyte comprises epichlorohydrin rubber, lithium salt and fast ion conductor ceramic powder, wherein the ECO-based solid polyelectrolyte comprises the following components in parts by weight: 80 parts of epichlorohydrin rubber, 5 parts of lithium salt and 15 parts of fast ion conductor ceramic powder.
The chlorine content in the epichlorohydrin rubber was 30.
The lithium salt comprises one or more of lithium perchlorate, lithium hexafluoroarsenate, lithium tetrafluoroborate, lithium hexafluorophosphate, lithium trifluoromethanesulfonate, lithium bistrifluoromethanesulfonylimide, lithium bis (trifluoromethylsulfonyl) imide and lithium bisoxalatoborate, and is preferably lithium trifluoromethanesulfonate.
The weight average molecular weight of the polyvinylidene fluoride is 5.0 multiplied by 104-8.0×106。
The fast ion conductor ceramic powder is Li7La3Zr2O12(LLZO)、LixLa2/3-xTiO3(LLTO)、 Li1+ xAlxTi2-x(PO4)3(LLZO)、LiAlO2(LAO)、Li7-xLa3Zr2-xMxO12(M＝Ta,Nb)(0.25 ﹤X﹤2)(LLZMO)、Li7+xGexP3-xS11(LGPS) and the like, preferably Li1+xAlxTi2-x(PO4)3(LLZO)。
A preparation method of an ECO-based solid polyelectrolyte comprises the following preparation steps: the method comprises the following steps: dissolution and dispersion of materials: respectively dispersing 80 parts of epichlorohydrin rubber and 5 parts of lithium trifluoromethanesulfonate in 190 parts of N-methylpyrrolidone solution and 10 parts of N-methylpyrrolidone solution in which lithium trifluoromethanesulfonate is dissolved, stirring until the materials are completely dissolved, and then stirring 15 parts of fast ion conductor ceramic powder Li1+xAlxTi2-x(PO4)3(LLZO) dispersing in 9 parts of N-methylpyrrolidone solution, and stirring until the dispersion is uniform; step two: mixing materials: quantitatively mixing the four solutions and the dispersion liquid, and stirring until the four solutions and the dispersion liquid are uniformly dispersed; step three: film forming: and pouring the mixed solution on a flat polytetrafluoroethylene plate, baking for 24 hours at 80 ℃, and then placing the sample in a vacuum oven at 80 ℃ for drying for 24 hours to remove the residual solvent, thereby obtaining the solid polymer electrolyte film.
The invention also discloses a preparation method of the solid lithium ion battery, which is the same as the first embodiment.
Compared with the prior art, the invention achieves the technical effects that: the solid polymer electrolyte provided by the invention takes the epichlorohydrin rubber as a matrix, and the epichlorohydrin rubber is a rubber material at room temperature, so that the solid polymer electrolyte has good mechanical properties; the epichlorohydrin rubber is copolymerized by epichlorohydrin and ethylene oxide, a large amount of EO units can be well dissolved, and lithium salt is complexed; the random copolymerization of CO units in EO can destroy the regularity of EO units, prevent the EO units from crystallizing and ensure that the EO units have good conductivity at room temperature; in addition, the blend is blended with polyvinylidene fluoride to further reduce the regularity of the epichlorohydrin rubber, and the mechanical property of the system can be adjusted by adjusting the addition amount of the polyvinylidene fluoride; the addition of the fast ion conductor ceramic powder increases the disorder degree of the polymer electrolyte, provides a new ion transmission channel and improves the room temperature conductivity of the system.
According to the examples, comparative data of tables 1 and 2 can be obtained:
wherein the first is the room temperature conductivity and electrochemical window of the ECO-based solid polymer electrolyte
Watch 1
Wherein the second table is the comparison of discharge specific capacity of the charging of the ECO-based solid polymer electrolyte assembly and the charging of the PEO-based polymer electrolyte assembly
Watch two
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (1)
1. A preparation method of ECO-based solid polyelectrolyte is characterized in that: the preparation method comprises the following preparation steps:
the method comprises the following steps: dissolution and dispersion of materials: respectively dispersing 50 parts of epichlorohydrin rubber, 30 parts of lithium bistrifluoromethanesulfonylimide and 15 parts of polyvinylidene fluoride in N-methylpyrrolidone solution, wherein the N-methylpyrrolidone solution for dissolving the epichlorohydrin rubber is 190 parts, the N-methylpyrrolidone solution for dissolving the lithium bistrifluoromethanesulfonylimide is 10 parts, and the N-methylpyrrolidone solution for dissolving the polyvinylidene fluoride is 100 parts, stirring until the materials are completely dissolved, dispersing five parts of fast ion conductor ceramic powder Li7La3Zr2O12 in 9 parts of the N-methylpyrrolidone solution, and stirring until the materials are uniformly dispersed;
step two: mixing materials: quantitatively mixing the four solutions and the dispersion liquid, and stirring until the four solutions and the dispersion liquid are uniformly dispersed;
step three: film forming: pouring the mixed solution on a flat polytetrafluoroethylene plate, baking for 24 hours at 80 ℃, and then placing the sample in a vacuum oven at 80 ℃ for drying for 24 hours to remove the residual solvent, thus obtaining the solid polymer electrolyte.
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Citations (3)
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| CN1372705A (en) * | 1999-09-02 | 2002-10-02 | 锂能技术公司 | Solid polymer elecrolytes |
| CN102130364A (en) * | 2011-02-12 | 2011-07-20 | 中南大学 | Gel-type polymer electrolyte used for lithium-sulfur secondary battery system and preparation method |
| CN107834104A (en) * | 2017-12-12 | 2018-03-23 | 清陶（昆山）能源发展有限公司 | A kind of composite solid electrolyte and preparation method thereof and the application in solid lithium battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1372705A (en) * | 1999-09-02 | 2002-10-02 | 锂能技术公司 | Solid polymer elecrolytes |
| CN102130364A (en) * | 2011-02-12 | 2011-07-20 | 中南大学 | Gel-type polymer electrolyte used for lithium-sulfur secondary battery system and preparation method |
| CN107834104A (en) * | 2017-12-12 | 2018-03-23 | 清陶（昆山）能源发展有限公司 | A kind of composite solid electrolyte and preparation method thereof and the application in solid lithium battery |
Non-Patent Citations (1)
| Title |
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| "Solid state polymeric electrolytes based on poly(epichlorohydrin)";G.Goulart Silva et al;《Solid State Ionics》;19961231;第93卷;第114页右栏第1段到第116页左栏第1段 * |
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