CN109273762B - Ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte and preparation method thereof - Google Patents
Ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte and preparation method thereof Download PDFInfo
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Abstract
The invention provides an ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte and a preparation method thereof, and relates to the field of lithium ion battery polymer gel electrolytes, wherein the gel electrolyte comprises the following raw material components in percentage by weight: 30-50% of ionic liquid; 0.5-2% of polyethylene glycol modified aminated graphene; 30 to 50 percent of polymer; 10 to 30 percent of lithium salt. The gel electrolyte obtained by the invention has higher ionic conductivity, electrochemical stability window and good charge-discharge cycle stability at room temperature, so that the electrolyte meets the application requirements of lithium batteries. The preparation method of the gel electrolyte provided by the invention has the advantages of simple preparation process, low cost, strong practicability and easiness in popularization.
Description
Technical Field
The invention relates to the field of lithium ion battery polymer gel electrolyte, in particular to an ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte and a preparation method thereof.
Background
The lithium ion battery, as a device for directly converting chemical energy and electric energy through chemical reaction, has the advantages of high energy density, good weight ratio, low self-discharge property, no memory effect and the like. The energy crisis, the environmental pollution and other problems are getting more and more attention at present. The lithium ion battery mainly comprises three parts, namely a positive electrode material, a negative electrode material and an electrolyte. The electrolyte is used as an important component of the lithium ion battery, and the performance of the electrolyte directly influences the performance of the battery. For traditional liquid electrolyte, hidden troubles such as leakage, explosion and the like exist. Therefore, development of a gel electrolyte having more excellent performance has been an important research point.
The gel polymer electrolyte has the characteristics of ultra-thin property, ultra-light property, design flexibility and the like, and can avoid the dangers of short circuit, needling, combustion and explosion. However, the solid polymer electrolyte has a severe limitation in its application due to its low room temperature ionic conductivity. In order to improve the ionic conductivity of the gel polymer electrolyte, a plasticizer can be added into the solid electrolyte system to melt lithium salt, reduce the crystallinity of the system and promote ion migration. The higher content of the plasticizer can cause the reduction of the mechanical property of the electrolyte, thereby influencing the service performance of the electrolyte. In order to solve the problem, graphene oxide is added into an electrolyte system to improve the ionic conductivity. At present, graphene oxide is mainly added into a single polymer matrix, and the graphene oxide does not form strong interaction with a polymer, so that the ionic conductivity is increased, but the use requirement of an electrolyte cannot be met.
Disclosure of Invention
In view of the above disadvantages of the prior art, an object of the present invention is to provide an ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte and a preparation method thereof, for solving the technical problem that the gel electrolyte adopted by a lithium ion battery in the prior art cannot meet the use requirements.
To achieve the above and other related objects, the present invention provides: in a first aspect, an ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte comprises the following raw material components in percentage by weight:
more preferably, the weight percentage of the ionic liquid is 35-45%.
More preferably, the weight percentage of the polyethylene glycol modified aminated graphene is 1.0% -1.5%.
More preferably, the weight percentage of the polymer is 35% to 45%.
More preferably, the weight percentage of the lithium salt is 15% to 35%.
Preferably, the ionic liquid is selected from one or more of 1-ethyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide salt, 1-butyl-2, 3-dimethylimidazolium bis (trifluoromethylsulfonyl) imide salt and 1-propyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide salt.
Preferably, the lithium salt is selected from LiTFSI, LiPF6、LiClO4、LiBF4、LiCH3SO3、LiCF3SO3One or more of (a).
Preferably, the mass fraction of amino groups of the polyethylene glycol modified aminated graphene is 0.5-2%. Polyethylene glycol modified aminated graphene interface polyethylene glycol groups and lithium ions form a complexing effect, a short-distance transport channel is provided at an interface layer where graphene and polymers are in contact, and migration of the lithium ions is promoted.
Preferably, the polymer is a blend of polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) and P [ MMA-IL ] copolymer. Polyvinylidene fluoride-hexafluoropropylene and P [ MMA-IL ] copolymer form compatible blend to promote lithium ion movement.
Preferably, in the polymer, the mass ratio of the polyvinylidene fluoride-hexafluoropropylene to the P [ MMA-IL ] copolymer is 9: 1-7: 3.
more preferably, in the polymer, the mass ratio of the polyvinylidene fluoride-hexafluoropropylene to the P [ MMA-IL ] copolymer is 8: 2-7: 3.
preferably, the P [ MMA-IL ] copolymer is obtained by a preparation method comprising the steps of: methyl methacrylate and vinyl imidazole are subjected to free radical solution polymerization, then are subjected to ionization reaction with ethyl bromide, and finally are subjected to ion exchange reaction with bis (trifluoromethyl) sulfonyl imide lithium to obtain the P [ MMA-IL ] copolymer.
Preferably, in the preparation method of the P [ MMA-IL ] polymer, the molar ratio of the methyl methacrylate to the vinyl imidazole is 1: 0.5-1: 1.
more preferably, in the process for the preparation of the P [ MMA-IL ] polymer, the molar ratio of methyl methacrylate to vinylimidazole is 1: 0.6-1: 0.8, 1: 0.5-1: 0.6, 1: 0.7-1: 0.8 or 1: 0.8-1: 1.0.
preferably, in the preparation method of the P [ MMA-IL ] polymer, the molar ratio of the bromoethane to the vinyl imidazole is 1: 0.5-1: 1.
more preferably, in the process for the preparation of the P [ MMA-IL ] polymer, the molar ratio of bromoethane to vinylimidazole is 1: 0.6-1: 0.8, 1: 0.5-1: 0.6, 1: 0.7-1: 0.8 or 1: 0.8-1: 1.0.
preferably, in the preparation method of the P [ MMA-IL ] polymer, the molar ratio of the lithium bis (trifluoromethyl) sulfonyl imide to the vinyl imidazole is 1: 0.5-1: 1.
more preferably, in the preparation method of the P [ MMA-IL ] polymer, the molar ratio of the lithium bis (trifluoromethyl) sulfonyl imide to the vinyl imidazole is 1: 0.6-1: 0.8, 1: 0.5-1: 0.6, 1: 0.7-1: 0.8 or 1: 0.8-1: 1.0.
in a second aspect, the present invention provides a method for preparing an ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte as described above, comprising the following steps: dissolving the ionic liquid, the polymer and the lithium salt in an organic solvent according to a weight ratio at room temperature, and heating and stirring to fully dissolve the polymer and the lithium salt to obtain a solution; dissolving the polyethylene glycol modified aminated graphene in an organic solvent, and performing ultrasonic treatment to obtain a dispersion liquid; and mixing the solution with the dispersion liquid, continuously heating and stirring, then pouring into a watch glass, heating and volatilizing the solvent to obtain the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte.
Preferably, the room temperature is 0-30 ℃.
Preferably, the organic solvent is an amide-based organic solvent.
More preferably, the organic solvent is N, N-dimethylformamide.
In a third aspect, the invention provides an application of the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte in a polymer lithium ion battery.
In summary, the invention provides an ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte and a preparation method thereof, and the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte has the following beneficial effects:
the invention utilizes polyethylene glycol modified aminated graphene (rGO-NH)2) The interfacial polyethylene glycol (PEG) group and lithium ions form a complexing effect, a short-distance transport channel can be provided at an interfacial layer where graphene and polymers are in contact, and migration of the lithium ions is promoted; polyethylene glycol modified aminated graphene (rGO-NH)2) The amino group of (a) and polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) form a hydrogen bond; polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) and P [ MMA-IL]The polymers form a compatible blend that facilitates lithium ion movement. The ionic liquid can reduce the crystallinity of an electrolyte system and improve the ionic conductivity.
The gel electrolyte obtained by the invention has higher ionic conductivity, electrochemical stability window and good charge-discharge cycle stability at room temperature, so that the electrolyte meets the application requirements of lithium batteries. The preparation method of the gel electrolyte provided by the invention has the advantages of simple preparation process, low cost, strong practicability and easiness in popularization.
Drawings
Fig. 1 is an ion conductivity analysis diagram of ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte obtained in examples 1 to 4.
Fig. 2 is a diagram of electrochemical stability windows of ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolytes obtained in examples 1 to 4.
Fig. 3 is a charge-discharge curve of a lithium ion battery assembled by the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte obtained in examples 1 to 4 at room temperature.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
It is to be understood that the present invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Example 1
Specific synthetic procedure for P [ MMA-IL ] polymer:
first, a P [ MMA-VIm ] polymer was prepared: 25ml of DMF was weighed into a three-necked flask using a measuring cylinder, and 2.5g of MMA, 2.5g of IVm and 40mg of AIBN were respectively weighed into the three-necked flask. The reaction was carried out at 65 ℃ under a nitrogen atmosphere for 24 h.
Then, P [ MMA-VEImBr ] was prepared. After the reaction was completed, the three-necked flask was taken out and cooled. 3g of bromoethane was weighed into a three-necked flask, and then reacted at 45 ℃ for 24 hours to sufficiently reflect the imidazole group and bromoethane. After the reaction is finished, ether is used as a precipitator to extract the polymer, then the polymer is put into a forced air drying oven to be dried for 4h at the temperature of 80 ℃, and finally dried for 12h at the temperature of 110 ℃ under the vacuum condition to remove DMF, thus obtaining P [ MMA-VEImBr ].
Finally, P [ MMA-IL is prepared]A polymer. Weighing 2.5g P [ MMA-VEImBr]Dissolving the polymer in 40mL of deionized water, simultaneously weighing 5g of LiTFSI and dissolving the LiTFSI in 40mL of deionized water, dropwise adding the deionized water dissolved with the LiTFSI into the deionized water dissolved with the polymer after the polymer is completely dissolved, continuously stirring, and then reacting for 24 hours at the temperature of 30 ℃ to ensure that the TFSI is dissolved-With Br-Ion exchange is performed. After the reaction is finished, the obtained product is washed by a large amount of deionized water, filtered, and then dried in vacuum for 12 hours at 75 ℃ to obtain P [ M ]MA-IL]A polymer.
0.64g of PVDF-HFP, 0.16g P [ MMA-IL ] polymer, 0.8g of methylimidazole bis (trifluoromethanesulfonyl) imide salt and 0.4g of lithium bis (trifluoromethanesulfonyl) imide are dissolved in 20mL of N, N-dimethylformamide at room temperature, stirred to form a uniform solution, transferred to a polytetrafluoroethylene mold, dried at 110 ℃ in a vacuum drying oven for 6 hours, and evaporated to form a film. And then drying the gel electrolyte in a vacuum drying oven at 110 ℃ for 24h to remove the N, N-dimethylformamide to obtain the gel electrolyte. The gel electrolyte film was punched into circular disks with diameters of 16mm and 19 mm. The electrolyte was then tested for ionic conductivity, electrochemical stability window and cell performance.
Example 2
0.64g PVDF-HFP, 0.16g P [ MMA-IL ] was mixed at room temperature]The polymer, 0.8g of methylimidazole bistrifluoromethylsulfonyl imide salt, and 0.4g of lithium bistrifluoromethylsulfonyl imide were dissolved in 20mL of N, N-dimethylformamide and stirred until a homogeneous solution was formed. While 0.01g of rGO-NH will be added2Dissolving the ethylene in N, N-dimethylformamide, carrying out ultrasonic treatment for 30-60 min, mixing with the solution, stirring to form a uniform solution, transferring to a polytetrafluoroethylene mold, drying in a vacuum drying oven at 110 ℃ for 6h, and volatilizing the solvent to form a film. And then drying the gel electrolyte in a vacuum drying oven at 110 ℃ for 24h to remove the N, N-dimethylformamide to obtain the gel electrolyte. The gel electrolyte film was punched into circular disks with diameters of 16mm and 19 mm. The electrolyte was then tested for ionic conductivity, electrochemical stability window and cell performance.
Example 3
0.64g PVDF-HFP, 0.16g P [ MMA-IL ] was mixed at room temperature]The polymer, 0.8g of methylimidazole bistrifluoromethylsulfonyl imide salt, and 0.4g of lithium bistrifluoromethylsulfonyl imide were dissolved in 20mL of N, N-dimethylformamide and stirred until a homogeneous solution was formed. While 0.015g of rGO-NH will be added2Dissolving the ethylene in N, N-dimethylformamide, carrying out ultrasonic treatment for 30-60 min, mixing with the solution, stirring to form a uniform solution, transferring to a polytetrafluoroethylene mold, drying in a vacuum drying oven at 110 ℃ for 6h, and volatilizing the solvent to obtain the final productAnd (3) a membrane. And then drying the gel electrolyte in a vacuum drying oven at 110 ℃ for 24h to remove the N, N-dimethylformamide to obtain the gel electrolyte. The gel electrolyte film was punched into circular disks with diameters of 16mm and 19 mm. The electrolyte was then tested for ionic conductivity, electrochemical stability window and cell performance.
Example 4
0.64g PVDF-HFP, 0.16g P [ MMA-IL ] was mixed at room temperature]The polymer, 0.8g of methylimidazole bistrifluoromethylsulfonyl imide salt, and 0.4g of lithium bistrifluoromethylsulfonyl imide were dissolved in 20mL of N, N-dimethylformamide and stirred until a homogeneous solution was formed. While 0.02g of rGO-NH will be added2Dissolving the ethylene in N, N-dimethylformamide, carrying out ultrasonic treatment for 30-60 min, mixing with the solution, stirring to form a uniform solution, transferring to a polytetrafluoroethylene mold, drying in a vacuum drying oven at 110 ℃ for 6h, and volatilizing the solvent to form a film. And then drying the gel electrolyte in a vacuum drying oven at 110 ℃ for 24h to remove the N, N-dimethylformamide to obtain the gel electrolyte. The gel electrolyte film was punched into circular disks with diameters of 16mm and 19 mm. The electrolyte was then tested for ionic conductivity, electrochemical stability window and cell performance.
And (3) performance testing:
the ionic conductivity, potential window and battery performance of the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte obtained in examples 1 to 4 were tested.
1) Ion conductivity measurement of gel electrolyte:
the gel electrolyte membrane was fixed between two stainless steel electrodes and the blocking electrode was tested for ac impedance at different temperatures. The formula is as follows: σ ═ l/(R)b×A)；
In the formula, σ is the ionic conductivity of the gel electrolyte in S/cm, l is the thickness of the membrane in cm, RbThe bulk resistance value of the gel electrolyte membrane obtained by fitting an alternating current impedance spectrum is represented by omega, A is the cross-sectional area of the stainless steel sheet and is represented by cm2The value is a fixed value of 0.785cm2。
FIG. 1 is a schematic view of an embodimentIon conductivity analysis graphs of ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolytes obtained in examples 1 to 4. From fig. 1, it can be seen that the addition of the polyethylene glycol modified aminated graphene improves the ionic conductivity of the electrolyte. For example, T on the abscissa-1/K-1Is 3.3X 10-3When, with rGO-NH2Is added, the ionic conductivity sigma is 1.27 multiplied by 10-3The S/cm is increased to 1.89 multiplied by 10-3S/cm, i.e. the ordinate log σ (S/cm) in FIG. 1, increases from-2.896 to-2.724. Meanwhile, the ion migration activation energy of the electrolyte is reduced from 2.65KJ/mol to 2.07 KJ/mol. This is mainly due to rGO-NH2The addition of (2) forms a communicated ion conductive path in the system, thereby improving the ion conductivity and reducing the ion migration activation energy.
2) Potential window measurement:
the gel electrolyte was measured for electrochemical stability window using LSV method, and the result is shown in fig. 2. During testing, stainless steel is used as a working electrode, metal lithium is used as a reference electrode and an auxiliary electrode, an electrolyte is clamped between the working electrode and the auxiliary electrode, and a response curve of current along with voltage is measured. Measurements were made at a rate of 10mV/s at room temperature.
Fig. 2 is a diagram of an electrochemical stability window of the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte obtained in examples 1 to 4, wherein the abscissa is potential (potential) and the ordinate is current density (current density). As can be seen from FIG. 2, rGO-NH in examples 2 to 42The addition of the compound improves the oxidative decomposition potential of the lithium ion battery, and has a higher electrochemical stability window.
3) And (3) testing the battery performance:
preparing a positive electrode film: mixing iron aluminum phosphate (LiFePO)4) The acetylene black conductive agent and the polyvinylidene fluoride binder are mixed according to the mass ratio of 8: 1: 1 was dissolved in NMP. After being mixed evenly, the mixture is coated on an aluminum foil by using an automatic coating machine, dried for 6 hours at the temperature of 120 ℃ in vacuum, punched into an electrode slice with the diameter of 10mm by using a punching machine, and weighed for standby.
And (3) preparing the button cell in a glove box by taking the electrode plate as a positive electrode material and a lithium plate as a negative electrode material. And the performance of the battery was tested. And (3) testing conditions are as follows: the test voltage is 2.7-4.2V, and the test multiplying power is 0.1C.
Fig. 3 is a charge-discharge curve of a lithium ion battery assembled by the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte obtained in examples 1 to 4 at room temperature of 30 ℃. As can be seen from FIG. 3, rGO-NH2The discharge capacity of the lithium ion battery is improved by adding the rGO-NH after dozens of charge-discharge cycles2The discharge capacity of the lithium ion battery is still higher than that of the battery without adding rGO-NH2Lithium ion batteries of (1), description rGO-NH2The performance of the lithium ion battery is improved.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. The ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte is characterized by comprising the following raw material components in percentage by weight:
30-50% of ionic liquid;
0.5-2% of polyethylene glycol modified aminated graphene;
30 to 50 percent of polymer;
10 to 30 percent of lithium salt;
the polymer is a blend of polyvinylidene fluoride-hexafluoropropylene and P [ MMA-IL ] copolymer, and the mass ratio of the polyvinylidene fluoride-hexafluoropropylene to the P [ MMA-IL ] copolymer is 9: 1-7: 3;
the mass fraction of amino groups of the polyethylene glycol modified aminated graphene is 0.5-2%.
2. The ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte according to claim 1, wherein: the ionic liquid is selected from one or more of 1-ethyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide salt, 1-butyl-2, 3-dimethylimidazolium bis (trifluoromethylsulfonyl) imide salt and 1-propyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide salt.
3. The ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte according to claim 1, wherein: the lithium salt is selected from LiTFSI and LiPF6、LiClO4、LiBF4、LiCH3SO3、LiCF3SO3One or more of (a).
4. The ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte according to claim 1, wherein: the P [ MMA-IL ] copolymer is obtained by a preparation method comprising the following steps: methyl methacrylate and vinyl imidazole are subjected to free radical solution polymerization, then are subjected to ionization reaction with ethyl bromide, and finally are subjected to ion exchange reaction with bis (trifluoromethyl) sulfonyl imide lithium to obtain the P [ MMA-IL ] copolymer.
5. The ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte according to claim 4, wherein: in the preparation method of the P [ MMA-IL ] copolymer, the molar ratio of the methyl methacrylate to the vinyl imidazole is 1: 0.5-1: 1.
6. the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte according to claim 4, wherein: in the preparation method of the P [ MMA-IL ] copolymer, the molar ratio of the bromoethane to the vinyl imidazole is 1: 0.5-1: 1;
and/or, in the preparation method of the P [ MMA-IL ] copolymer, the molar ratio of the lithium bis (trifluoromethyl sulfonyl) imide to the vinyl imidazole is 1: 0.5-1: 1.
7. a method for preparing the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte according to any one of claims 1-6, characterized in that: the method comprises the following steps:
dissolving the ionic liquid, the polymer and the lithium salt in an organic solvent according to a weight ratio at room temperature, and heating and stirring to fully dissolve the polymer and the lithium salt to obtain a solution;
dissolving the polyethylene glycol modified aminated graphene in an organic solvent, and performing ultrasonic treatment to obtain a dispersion liquid;
and mixing the solution with the dispersion liquid, continuously heating and stirring, then pouring into a watch glass, heating and volatilizing the solvent to obtain the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte.
8. The application of the ionic liquid/polyethylene glycol modified aminated graphene/polymer gel electrolyte according to any one of claims 1 to 6 in a polymer lithium ion battery.
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