CN110233286B - In-situ polymerization composite organic solid electrolyte and preparation method and application thereof - Google Patents
In-situ polymerization composite organic solid electrolyte and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an in-situ polymerization composite organic solid electrolyte, a preparation method and application thereof. According to the invention, the inorganic mineral clay is compounded with the polymer, and the branching structure of the polymer reduces the crystallinity, thereby being beneficial to the conduction of lithium ions in an amorphous region; the inorganic mineral clay has a hollow nano-tubular structure, can provide a lithium ion transmission channel, and effectively improves the ionic conductivity of the electrolyte. Moreover, the inorganic mineral clay compounded polymer electrolyte has a higher electrochemical stability window and better thermal stability.
Description
Technical Field
The invention relates to the technical field of all-solid-state lithium ion batteries, in particular to an in-situ polymerization composite organic solid electrolyte and a preparation method and application thereof.
Background
With the acceleration of the modernization process, ecological problems such as energy crisis that the traditional fossil energy is increasingly deficient, serious environmental pollution, global greenhouse effect and the like appear on the global scale. In the face of the increasingly prominent environmental and resource problems, it is urgent to accelerate the development of clean energy, establish an efficient, clean, economic and safe energy system, reduce the dependence of the traditional automobile industry and industry on fossil energy, and realize the sustainable development of new energy. Lithium ion batteries with the advantages of rapid charge and discharge, environmental friendliness and the like become hot spots in the field of new energy.
Most of the electrolytes used in current commercial lithium ion batteries are liquid electrolytes. Such batteries face two very serious problems: firstly, in the process of charging and discharging the battery, the organic solvent can form a solid electrolyte membrane on the positive electrode, so that the electrode is polarized, and the performance of the battery is attenuated; secondly, the organic solvent used in the electrolyte has potential safety hazards such as leakage, combustion and explosion, and the safety problem is great. The solid electrolyte is adopted to replace the liquid electrolyte, so that the safety performance and the cycle life of the lithium ion battery can be effectively improved.
The organic solid electrolyte has good compatibility with the electrode and small interface impedance; the lithium ion battery has good mechanical property, and can effectively inhibit the generation of dendritic crystals of the lithium negative electrode; the preparation method is simple, has good film-forming performance, can improve the energy density of the lithium battery by reducing the thickness of the electrolyte film, and is the solid electrolyte closest to commercial production application. However, the application of organic solid electrolytes is greatly limited by the low ionic conductivity. Researches show that compounding inorganic particles with polymers is one of effective measures for improving the ionic conductivity, for example, the ionic conductivity of polyethylene oxide can be improved by adding nano silica and nano alumina into the polyethylene oxide.
Disclosure of Invention
The invention aims to solve the problem of low ionic conductivity of the existing organic solid electrolyte, and discloses an in-situ polymerization composite organic solid electrolyte and a preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme.
The in-situ polymerized composite organic solid electrolyte consists of polymerizable monomer, photoinitiator, inorganic mineral clay and lithium salt.
Further, the polymerizable monomer is polyethylene glycol acrylate monomethyl ether or polyethylene glycol methacrylate monomethyl ether; the inorganic mineral clay is halloysite.
Further, the lithium salt is lithium perchlorate, lithium hexafluorophosphate or lithium bistrifluoromethanesulfonylimide; the photoinitiator is benzoin dimethyl ether or 2-hydroxy-2-methyl-1 phenyl acetone.
Further, the mass ratio of the polymerizable monomer, the photoinitiator, the inorganic mineral clay and the lithium salt is 1: 0.01: (0.04-0.12): (0.10-0.30).
The invention also provides a preparation method of the in-situ polymerization composite organic solid electrolyte, which comprises the following steps:
(1) adding a photoinitiator and lithium salt into a polymerizable monomer, and stirring and dissolving to obtain a transparent mixed liquid;
(2) adding inorganic mineral clay into the transparent mixed liquid obtained in the step (1), and stirring and mixing to obtain uniformly dispersed slurry;
(3) and (3) coating the slurry obtained in the step (2) on a pole piece, and carrying out free radical polymerization under the illumination of an ultraviolet lamp to obtain the composite organic solid electrolyte.
Further, the steps (1) to (3) are all completed in an inert gas atmosphere.
Further, the stirring in the step (1) is carried out under the condition of keeping out of the sun and is carried out for 3-4 hours; the stirring time in the step (2) is 5-6 h.
Further, the pole piece in the step (3) is a stainless steel sheet.
Further, the power of the ultraviolet lamp in the step (3) is 80W-120W, and the illumination time is 1 h-2 h.
The composite organic solid electrolyte can be used for all-solid-state lithium ion batteries, and the ionic conductivity is as high as 7.1 multiplied by 10-5S cm-1。
Compared with the prior art, the inorganic mineral clay is dispersed in the polymerizable monomer, the uniformly dispersed slurry is coated on the pole piece, the monomer is initiated to be polymerized in situ by adopting ultraviolet light, the preparation method is simple and efficient, and the prepared electrolyte is in good contact with the interface of the pole piece. The monomer is polymerized to form a branched polymer with a main chain of carbon-carbon bond and a side chain of polyethylene glycol monomethyl ether, the branched structure reduces the crystallinity of the polymer to a great extent, increases an amorphous area and is beneficial to the transmission of lithium ions by a polymer chain segment. The inorganic mineral clay halloysite is of a hollow nano tubular structure, the structure provides a lithium ion transmission channel, the transmission paths of lithium ions are increased, and the inorganic mineral clay halloysite can be used for cooperating with a branched polymer to improve the ionic conductivity, so that the capacity and the cycle life of the all-solid-state lithium ion battery are improved.
The invention has the outstanding characteristics and advantages that:
1. the invention compounds the branched polymer and the inorganic mineral clay in situ, the inorganic mineral clay is a hollow nano tubular structure and can provide a lithium ion transmission channel; compared with the traditional crystalline polyethylene oxide, the branched polymer has a larger proportion of amorphous areas, and is beneficial to the conduction of lithium ions in the amorphous areas. The two components act synergistically to improve the ionic conductivity of the solid electrolyte, and the ionic conductivity of the battery using the composite organic solid electrolyte can reach 7.1 multiplied by 10-5S cm-1And the electrochemical stability window reaches 5.22V.
2. The composite organic solid electrolyte is prepared by in-situ polymerization on the pole piece directly, and the obtained electrolyte has good interface contact with the pole piece; the inorganic mineral clay compounded polymer electrolyte has better thermal stability and the thermal decomposition temperature is as high as 341 ℃.
3. The composite organic solid electrolyte is prepared by adopting an ultraviolet light initiated in-situ polymerization method, the raw materials are uniformly mixed, and the electrolyte can be obtained by using an ultraviolet lamp for illumination.
Detailed Description
The following examples further illustrate embodiments of the present invention, but are not intended to limit the invention.
Example 1
The preparation method of the in-situ polymerization composite organic solid electrolyte comprises the following steps:
step one, adding polyethylene glycol acrylate monomethyl ether, benzoin dimethyl ether and lithium bis (trifluoromethanesulfonyl) imide into a glass bottle according to the mass of 1g, 0.01g and 0.30g in an argon glove box, and stirring for 3 hours in a dark place to dissolve solids to obtain transparent liquid;
step two, in an argon glove box, adding 0.04g of halloysite into the transparent liquid obtained in the step one, and stirring for 6 hours to prepare uniformly dispersed slurry;
and step three, coating the slurry prepared in the step two on a stainless steel sheet in an argon glove box, and performing free radical polymerization reaction under a 120W ultraviolet lamp for 1h to obtain the composite organic solid electrolyte.
Assembling the prepared composite organic solid electrolyte into a button cell in an argon glove box, carrying out alternating current impedance test at 30 ℃, and measuring that the ionic conductivity is 7.1 multiplied by 10-5S cm-1。
The prepared composite organic solid electrolyte is subjected to linear sweep voltammetry test, and the electrochemical stability window can reach 5.22V. The prepared composite organic solid electrolyte is subjected to thermogravimetric analysis test, and the thermal decomposition temperature is as high as 341 ℃.
Example 2
The preparation method of the in-situ polymerization composite organic solid electrolyte comprises the following steps:
step one, adding polyethylene glycol acrylate monomethyl ether, 2-hydroxy-2-methyl-1-phenyl acetone and lithium hexafluorophosphate into a glass bottle according to the mass of 1g, 0.015g and 0.20g in an argon glove box, and stirring for 4 hours in a dark place to dissolve solids to obtain transparent liquid;
step two, in an argon glove box, adding 0.05g of halloysite into the transparent liquid obtained in the step one, and stirring for 5 hours to prepare uniformly dispersed slurry;
and step three, coating the slurry prepared in the step two on a stainless steel sheet in an argon glove box, and performing free radical polymerization reaction under a 100W ultraviolet lamp for 2 hours to obtain the composite organic solid electrolyte.
Assembling the prepared composite organic solid electrolyte into a button cell in an argon glove box, carrying out alternating current impedance test at 30 ℃, and measuring that the ionic conductivity is 6.3 multiplied by 10-5S cm-1。
The prepared composite organic solid electrolyte is subjected to linear sweep voltammetry test, and the electrochemical stability window can reach 5.18V. The prepared composite organic solid electrolyte was subjected to thermogravimetric analysis test, and its thermal decomposition temperature was 336 ℃.
Example 3
The preparation method of the in-situ polymerization composite organic solid electrolyte comprises the following steps:
step one, adding polyethylene glycol methyl acrylate monomethyl ether, 2-hydroxy-2-methyl-1 phenyl acetone and lithium perchlorate into a glass bottle according to the mass of 1g, 0.013g and 0.10g in an argon glove box, and stirring for 3.5 hours in a dark place to dissolve solids to obtain transparent liquid;
step two, in an argon glove box, adding 0.07g of halloysite into the transparent liquid obtained in the step one, and stirring for 5 hours to prepare uniformly dispersed slurry;
and step three, coating the slurry prepared in the step two on a stainless steel sheet in an argon glove box, and performing free radical polymerization reaction under a 120W ultraviolet lamp for 1.5 hours to obtain the composite organic solid electrolyte.
Assembling the prepared composite organic solid electrolyte into a button cell in an argon glove box, carrying out alternating current impedance test at 30 ℃, and measuring that the ionic conductivity is 5.2 multiplied by 10-5S cm-1。
The prepared composite organic solid electrolyte is subjected to linear sweep voltammetry test, and the electrochemical stability window can reach 5.21V. The prepared composite organic solid electrolyte is subjected to thermogravimetric analysis test, and the thermal decomposition temperature is 338 ℃.
Example 4
The preparation method of the in-situ polymerization composite organic solid electrolyte comprises the following steps:
step one, adding polyethylene glycol methyl acrylate monomethyl ether, benzoin dimethyl ether and lithium perchlorate into a glass bottle according to the mass of 1g, 0.02g and 0.15g in an argon glove box, and stirring for 4 hours in a dark place to dissolve solids to obtain transparent liquid;
step two, in an argon glove box, adding 0.12g of halloysite into the transparent liquid obtained in the step one, and stirring for 5.5 hours to prepare uniformly dispersed slurry;
and step three, coating the slurry prepared in the step two on a stainless steel sheet in an argon glove box, and performing free radical polymerization reaction under an 80W ultraviolet lamp for 1h to obtain the composite organic solid electrolyte.
Assembling the prepared composite organic solid electrolyte into a button cell in an argon glove box, carrying out alternating current impedance test at 30 ℃, and measuring that the ionic conductivity is 5.7 multiplied by 10-5S cm-1。
The prepared composite organic solid electrolyte is subjected to linear sweep voltammetry test, and the electrochemical stability window can reach 5.16V. The prepared composite organic solid electrolyte is subjected to thermogravimetric analysis test, and the thermal decomposition temperature is 335 ℃.
Example 5
The preparation method of the in-situ polymerization composite organic solid electrolyte comprises the following steps:
step one, adding polyethylene glycol acrylate monomethyl ether, 2-hydroxy-2-methyl-1-phenyl acetone and lithium bis (trifluoromethanesulfonyl) imide into a glass bottle according to the mass of 1g, 0.01g and 0.23g in an argon glove box, and stirring for 3 hours in a dark place to dissolve solids to obtain transparent liquid;
step two, in an argon glove box, adding 0.11g of halloysite into the transparent liquid obtained in the step one, and stirring for 5 hours to prepare uniformly dispersed slurry;
and step three, coating the slurry prepared in the step two on a stainless steel sheet in an argon glove box, and performing free radical polymerization reaction under a 100W ultraviolet lamp for 1h to obtain the composite organic solid electrolyte.
Assembling the prepared composite organic solid electrolyte into a button cell in an argon glove box, carrying out alternating current impedance test at 30 ℃, and measuring that the ionic conductivity is 5.9 multiplied by 10-5S cm-1。
The prepared composite organic solid electrolyte is subjected to linear sweep voltammetry test, and the electrochemical stability window of the composite organic solid electrolyte can reach 5.17V. The prepared composite organic solid electrolyte is subjected to thermogravimetric analysis test, and the thermal decomposition temperature is 337 ℃.
Example 6
The preparation method of the in-situ polymerization composite organic solid electrolyte comprises the following steps:
step one, adding polyethylene glycol methyl acrylate monomethyl ether, 2-hydroxy-2-methyl-1 phenyl acetone and lithium bis (trifluoromethanesulfonyl) imide into a glass bottle according to the mass of 1g, 0.012g and 0.11g in an argon glove box, and stirring for 4 hours in a dark place to dissolve solids to obtain transparent liquid;
step two, in an argon glove box, adding 0.12g of halloysite into the transparent liquid obtained in the step one, and stirring for 5.5 hours to prepare uniformly dispersed slurry;
and step three, coating the slurry prepared in the step two on a stainless steel sheet in an argon glove box, and performing free radical polymerization reaction under a 120W ultraviolet lamp for 1.3h to obtain the composite organic solid electrolyte.
Assembling the prepared composite organic solid electrolyte into a button cell in an argon glove box, carrying out alternating current impedance test at 30 ℃, and measuring that the ionic conductivity is 6.7 multiplied by 10-5S cm-1。
The prepared composite organic solid electrolyte is subjected to linear sweep voltammetry test, and the electrochemical stability window can reach 5.20V. The prepared composite organic solid electrolyte is subjected to thermogravimetric analysis test, and the thermal decomposition temperature is up to 338 ℃.
Comparative example 1
Comparative example 1 is an organic solid electrolyte, not compounded with inorganic mineral clay, and the preparation process is substantially the same as that of example 1 except that step two is omitted, i.e., no halloysite is added, and the resulting solid electrolyte has a low ionic conductivity of only 1.1X 10-5S cm-1And the electrochemical stability window is only 4.9V, and the thermal decomposition temperature is 320 ℃.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any equivalent alterations, modifications or improvements made by those skilled in the art to the above-described embodiments using the technical solutions of the present invention are still within the scope of the technical solutions of the present invention.
Claims (7)
1. An in-situ polymerization composite organic solid electrolyte is characterized in that raw materials comprise a polymerizable monomer, a photoinitiator, inorganic mineral clay and lithium salt;
the monomer is polyethylene glycol acrylate monomethyl ether or polyethylene glycol methacrylate monomethyl ether; the inorganic mineral clay is halloysite;
the photoinitiator is benzoin dimethyl ether or 2-hydroxy-2-methyl-1-phenyl acetone; the lithium salt is lithium perchlorate, lithium hexafluorophosphate or lithium bistrifluoromethanesulfonylimide;
the mass ratio of the polymerizable monomer, the photoinitiator, the inorganic mineral clay and the lithium salt is 1: (0.01-0.02): (0.04-0.12): (0.10 to 0.30);
the in-situ polymerization composite organic solid electrolyte comprises the following steps:
(1) adding a photoinitiator and lithium salt into a polymerizable monomer, and stirring and dissolving to obtain a transparent mixed liquid;
(2) adding inorganic mineral clay into the transparent mixed liquid obtained in the step (1), and stirring and mixing to obtain uniformly dispersed slurry;
(3) and (3) coating the slurry obtained in the step (2) on a pole piece, and carrying out free radical polymerization under the illumination of an ultraviolet lamp to obtain the composite organic solid electrolyte.
2. A method for preparing the in-situ polymerized composite organic solid electrolyte according to claim 1, which comprises the steps of:
(1) adding a photoinitiator and lithium salt into a polymerizable monomer, and stirring and dissolving to obtain a transparent mixed liquid;
(2) adding inorganic mineral clay into the transparent mixed liquid obtained in the step (1), and stirring and mixing to obtain uniformly dispersed slurry;
(3) and (3) coating the slurry obtained in the step (2) on a pole piece, and carrying out free radical polymerization under the illumination of an ultraviolet lamp to obtain the composite organic solid electrolyte.
3. The method for producing a composite organic solid electrolyte according to claim 2, wherein steps (1) to (3) are performed in an inert gas atmosphere.
4. The method for preparing the composite organic solid electrolyte according to claim 2, wherein the power of the ultraviolet lamp in the step (3) is 80W to 120W, and the illumination time is 1h to 2 h.
5. The method for preparing a composite organic solid electrolyte according to claim 2, wherein the stirring in the step (1) is performed for 3 to 4 hours under a condition of keeping out light; the stirring time in the step (2) is 5-6 h.
6. The method for producing a composite organic solid electrolyte according to claim 2, wherein the electrode sheet in the step (3) is a stainless steel sheet.
7. Use of the composite organic solid electrolyte according to claim 1 in an all-solid lithium ion battery.
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| CN113675464A (en) * | 2020-05-15 | 2021-11-19 | 北京卫国创芯科技有限公司 | In-situ polymerized polymer solid electrolyte, battery and preparation method |
| CN111900468B (en) * | 2020-08-11 | 2022-08-30 | 珠海冠宇电池股份有限公司 | Solid electrolyte, preparation method thereof and lithium ion battery |
| CN113540697B (en) * | 2021-06-28 | 2022-09-09 | 合肥国轩高科动力能源有限公司 | Composite diaphragm and preparation method thereof |
| CN113471530B (en) * | 2021-07-28 | 2022-10-25 | 西安交通大学 | Preparation method and application of inorganic clay array |
| CN114512714A (en) * | 2022-01-20 | 2022-05-17 | 贵阳学院 | Composite polymer electrolyte material, preparation method thereof and lithium ion battery |
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