CN108808080B - Nano composite gel electrolyte, lithium secondary battery and preparation method thereof - Google Patents
Nano composite gel electrolyte, lithium secondary battery 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 relates to a nano composite gel electrolyte, a lithium secondary battery and a preparation method thereof, wherein the gel electrolyte is formed by introducing hydrophobic modified nano particles into a liquid electrolyte and forming a three-dimensional network through hydrogen bond interaction between the hydrophobic modified nano particles and surface modified molecules thereof and electrolyte solvent molecules so as to gelatinize the liquid electrolyte. The ionic conductivity of the gel electrolyte is close to that of the electrolyte of the same type, and is about 10‑3S/cm. The addition of the hydrophobic modified nano particles can effectively improve the lithium ion transference number of electrolyte and reduce the interface impedance between the electrolyte and lithium metal. In addition, compared with the same type of pure electrolyte, the gel electrolyte has better compatibility and cycling stability with the lithium metal electrode. The gel electrolyte can be compounded on the diaphragm by a direct coating or coating swelling method, and the preparation process is simple and convenient for production.
Description
Technical Field
The invention relates to the field of lithium metal secondary batteries, in particular to a nano composite gel electrolyte, a lithium secondary battery and a preparation method thereof.
Background
With the development of society, environmental protection and energy conservation are more and more concerned by people. Lithium ion batteries are one of the most popular chemical energy sources due to their higher energy density, longer cycle life and lower environmental impact. Lithium ion batteries have a profound effect on the daily life of people, and the carbon cathode lithium ion batteries used in commercialization are almost close to the theoretical capacity of the carbon cathode lithium ion batteries, so that the carbon cathode lithium ion batteries are difficult to meet the increasingly high application requirements in the aspects of portable electronic equipment, electric automobiles, large-scale energy storage and the like. Therefore, there is still an urgent need for a battery having higher energy density and higher safety.
Metallic lithium has the highest theoretical energy density (3860 mAh/g) and the lowest electrochemical potential (3.04V relative to a standard hydrogen electrode). Therefore, lithium metal batteries are one of the most promising next-generation energy storage devices, and can meet the requirements of high-energy-consumption devices. However, there is still a significant problem when lithium metal is used directly as a battery negative electrode. These problems include: the circulation and rate performance are poor, and the safety is difficult to guarantee. The main reason is that lithium metal is extremely unstable in the currently used electrolyte, dendrite growth is caused by large polarization and strong electric field under high rate, and the commonly used diaphragm has low mechanical strength and is easy to puncture, so that a series of safety problems can be caused. The replacement of the liquid electrolyte with a solid electrolyte having a higher mechanical strength not only overcomes the disadvantages of the liquid electrolyte, but also provides the possibility for developing new chemical batteries. However, poor contact between the solid electrolyte and the electrodes results in large interfacial resistance, which is not favorable for the performance of the solid electrolyte.
Disclosure of Invention
The present invention has been made in view of the above problems, and it is an object of the present invention to provide a nanocomposite gel electrolyte, a lithium secondary battery including the same, and a method for preparing the same, wherein the gel electrolyte has high ionic conductivity and good compatibility with positive and negative electrodes, and can effectively prolong the cycle life of a lithium battery, and the nanocomposite gel can reduce the interfacial impedance between a solid electrolyte and electrodes.
The technical scheme for realizing the invention is as follows: a nano composite gel electrolyte consists of hydrophobic modified nano particles and electrolyte, wherein the mass fraction of the hydrophobic modified nano particles in the nano composite gel electrolyte is 3-30%, and the nano composite gel electrolyte is used for being spaced between a battery diaphragm and a positive electrode and a negative electrode.
The hydrophobic modified nano particles are nano Al2O3Nano SiO2Nano ZnO and nano SnO2Or nano TiO2The hydrophobically modified nanoparticle has a size of 5 to 500 nm.
The hydrophobic modified nano-particles are modified by utilizing a silane coupling agent, wherein the silane coupling agent is one or more of hexamethyldisiloxane, polydimethylsiloxane, dimethyl siloxane, octamethylcyclotetrasiloxane, monomethyltrichlorosilane, dimethyldichlorosilane and methacryloxypropyltrimethoxysilane.
The modification method comprises the following steps: ultrasonically dispersing the nanoparticles and the silane coupling agent in ethanol, wherein the mass fractions of the nanoparticles and the silane coupling agent in the ethanol are 1-10% and 1-15%, respectively, stirring for 3-12 h at 60-90 ℃, separating the product by using a centrifugal or filtration mode, washing the product by using ethanol, and finally performing vacuum drying.
The electrolyte comprises lithium salt and an organic solvent I, wherein the lithium salt is LiClO4、LiPF6One or more of LiOH, LiTFSI, LiFSI or LiNFSI; the organic solvent I is one or more of propylene carbonate, ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate or methyl propyl carbonate.
The lithium secondary battery comprises a positive pole piece, a negative pole piece, a diaphragm and a nano composite gel electrolyte, wherein the nano composite gel electrolyte consists of hydrophobic modified nano particles and electrolyte and is used for being spaced between the battery diaphragm and the positive and negative poles.
A lithium secondary battery, the structure of which comprises: a positive electrode sheet including a positive electrode current collector and a positive electrode active material; a negative electrode tab including a negative current collector and a negative active material; a diaphragm; a nanocomposite gel electrolyte for spacing between the separator and the positive and negative pole pieces.
The positive pole piece is obtained by coating a positive active substance on an aluminum foil, wherein the positive active substance is a nickel-cobalt-aluminum ternary material, a nickel-cobalt-manganese ternary material, lithium cobaltate, lithium nickelate, lithium manganate, lithium iron phosphate or phosphorus, sulfur or lithium polysulfide.
The negative pole piece is obtained by compounding a negative active material on a copper foil, wherein the negative active material is lithium metal, and the compounding mode is electroplating or rolling.
The separator may be a porous PE film, a porous PP/PE/PP composite film, an inorganic solid electrolyte film, or a polymer solid electrolyte film.
The preparation method of the lithium secondary battery comprises the following steps:
(a) adding the hydrophobic modified nano particles into an organic solvent II, and fully stirring to form colloidal slurry;
(b) coating the colloidal slurry prepared in the step (a) on two sides of a diaphragm, and performing vacuum drying to obtain the diaphragm coated with the nano particle coating;
(c) assembling the battery cell according to the positive pole piece, the diaphragm coated with the nano particle coating prepared in the step (b) and the negative pole piece in sequence;
(d) and injecting electrolyte into the battery cell to swell the nano particle coating into gel electrolyte, and then packaging the battery cell.
In the step (a), the mass fraction of the hydrophobically modified nanoparticles in an organic solvent II is 3-30%, and the organic solvent II is one or more of dimethylbenzene, methanol, ethanol, isopropanol, dioxane or N-methylpyrrolidone; the thickness of the coating of the colloidal slurry in the step (b) is 10-100 μm, and the temperature of vacuum drying is 25-100 ℃.
The preparation method of the lithium secondary battery comprises the following steps:
(e) adding the hydrophobic modified nano particles into the electrolyte, and fully stirring to form the nano composite gel electrolyte;
(f) coating the nano composite gel electrolyte prepared in the step (e) on a diaphragm on two sides; obtaining a separator coated with a gel electrolyte;
(g) and (f) assembling and packaging the battery cell according to the positive pole piece, the diaphragm coated with the gel electrolyte and the negative pole piece in sequence.
The mass fraction of the hydrophobic nano particles in the nano composite gel electrolyte in the step (e) is 3-30%, and the thickness of the nano composite gel electrolyte coated in the step (f) is 5-50 μm.
The invention has the beneficial effects that: the gel electrolyte is formed by introducing hydrophobic modified nano particles into a liquid electrolyte and forming a three-dimensional network through the hydrogen bond action between the hydrophobic modified nano particles and surface modified molecules thereof and electrolyte solvent molecules so as to gelatinize the liquid electrolyte. The addition of the hydrophobic modified nano particles can effectively improve the lithium ion transference number of electrolyte, reduce the interface impedance gel between the electrolyte and lithium, and ensure that the ionic conductivity of the electrolyte is close to that of pure electrolyte of the same type, namely about 10-3S/cm; compared with pure electrolyte of the same type, the productThe gel electrolyte and the lithium metal electrode have better compatibility and cycling stability; compared with the pure electrolyte of the same type, the gel electrolyte has lower interfacial impedance between the gel electrolyte and the lithium metal electrode.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
The composite material comprises a separator 1, a nanocomposite gel electrolyte 2, a positive electrode active material 3, a negative electrode active material 4, a positive electrode current collector 5 and a negative electrode current collector 6.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A lithium secondary battery, the structure of which comprises:
(1) a positive electrode sheet including a positive electrode current collector 5 and a positive electrode active material 3;
(2) a negative electrode tab including a negative electrode current collector 6 and a negative electrode active material 4;
(3) a diaphragm 1;
(4) and the nano composite gel electrolyte 2 is used for spacing between the diaphragm 1 and the positive pole piece and the negative pole piece.
The lithium secondary battery is prepared as follows:
(1) hydrophobic Al2O3Preparing nano particles: will be provided withAl2O3Ultrasonically dispersing the nano particles and the silane coupling agent in ethanol, stirring for 6 hours at 70 ℃, separating a product by using a centrifugal or filtration mode, washing the product by using the ethanol, and finally drying in vacuum.
(2) Coating a nickel-cobalt-manganese ternary material NCM523 serving as a positive electrode material on an aluminum foil to prepare a positive electrode piece;
(3) compounding lithium metal on copper foil in an electroplating or rolling mode to prepare a negative pole piece;
(4) mixing Al2O3And adding the nano particles into the electrolyte, and fully stirring to prepare the cementing slurry. The mass fraction of the nano particles in the slurry is 15%, and the lithium salt used in the electrolyte is LiClO4The organic solvent is propylene carbonate;
(5) coating the gel electrolyte prepared in the step (3) on a porous PE diaphragm on two sides, wherein the coating thickness of each side is 20 micrometers;
(6) and assembling and packaging the battery cell according to the sequence of the positive pole piece, the diaphragm coated with the gel electrolyte and the negative pole piece.
The basic steps of examples 2 to 5 are the same as those of example 1, except for the use of the positive electrode material, the type of nanoparticles, the mass fraction of nanoparticles, the types of lithium salts and organic solvents in the electrolyte, the type of separator, and the coating thickness of the gel electrolyte. In particular, see the following table:
TABLE 1 parameters of examples 2 to 5
Example 6
The lithium secondary battery is prepared as follows:
(1) hydrophobic SiO2Preparing nano particles: mixing SiO2Ultrasonically dispersing the nano particles and the silane coupling agent in ethanol, stirring for 6 hours at 70 ℃, separating a product by using a centrifugal or filtration mode, washing the product by using the ethanol, and finally drying in vacuum.
(2) Coating a nickel-cobalt-manganese ternary material NCM523 serving as a positive electrode material on an aluminum foil to prepare a positive electrode piece;
(3) compounding lithium metal on copper foil in an electroplating or rolling mode to prepare a negative pole piece;
(4) hydrophobic nano SiO2Adding the particles into an organic solvent, and fully stirring to prepare a nanoparticle precursor slurry, wherein the mass fraction of the nanoparticles in the organic solvent is 6%, and the organic solvent used by the precursor slurry is ethanol.
(5) Coating the two sides of the nanoparticle precursor slurry prepared in the step (3) on a PE diaphragm, wherein the coating thickness is 30 mu m, and then carrying out vacuum drying to obtain a nanoparticle-coated diaphragm;
(6) assembling a battery core according to the sequence of a positive pole piece, a diaphragm coated with nano particles and a negative pole piece, injecting a proper amount of electrolyte into the battery core, and packaging the battery core, wherein lithium salt in the electrolyte is LiPF6The organic solvent is propylene carbonate.
The basic steps of examples 7 to 10 are the same as those of example 6, except for the used positive electrode material, the type of nanoparticles, the precursor slurry solvent, the mass fraction of nanoparticles in the precursor slurry, the type of separator, the coating thickness of the precursor slurry, and the types of lithium salt and organic solvent in the electrolyte. In particular, see the following table:
TABLE 2 parameters of examples 7 to 9
The above examples were subjected to a charge-discharge test to calculate the discharge capacity retention rate, and the charge-discharge rate was 0.5C.
The nano-composite gel prepared in all the examples is assembled into a Li-Li symmetrical non-blocking battery, the transference number of lithium ions and the interface impedance of the gel electrolyte to lithium are measured, and pure electrolyte is used as comparison.
Table 3 shows that the charge-discharge cycle times of the examples 1-10 with the capacity retention rate lower than 90% are compared with those of the corresponding pure electrolyte
TABLE 4 transference number of lithium ions in nanocomposite gel electrolyte in examples 1-10
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A nanocomposite gel electrolyte characterized by: the nano composite gel electrolyte consists of hydrophobic modified nano particles and electrolyte, wherein the mass fraction of the hydrophobic modified nano particles in the nano composite gel electrolyte is 3-30% and is used for being spaced between a battery diaphragm and a positive electrode and a negative electrode;
the hydrophobic modified nano-particles are modified by utilizing a silane coupling agent, wherein the silane coupling agent is one or more of hexamethyldisiloxane, polydimethylsiloxane, dimethyl siloxane, octamethylcyclotetrasiloxane, monomethyltrichlorosilane, dimethyldichlorosilane and methacryloxypropyltrimethoxysilane; the hydrophobic modified nano particles are nano Al2O3Nano ZnO and nano SnO2Or nano TiO2The hydrophobically modified nanoparticles have a size of 5 to 500 nm;
the modification method comprises the following steps: ultrasonically dispersing the nanoparticles and the silane coupling agent in ethanol, wherein the mass fractions of the nanoparticles and the silane coupling agent in the ethanol are 1-10% and 1-15%, respectively, stirring for 3-12 h at 60-90 ℃, separating the product by using a centrifugal or filtration mode, washing the product by using ethanol, and finally performing vacuum drying.
2. The nanocomposite gel electrolyte according to claim 1, characterized in that: the electrolyte comprises lithium salt and an organic solvent I, wherein the lithium salt is LiClO4、LiPF6LiOH, LiTFSI, LiFSI or LiNFSIOne or more of the above-mentioned raw materials; the organic solvent I is one or more of propylene carbonate, ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate or methyl propyl carbonate.
3. A lithium secondary battery prepared using the nanocomposite gel electrolyte of any one of claims 1 to 2, characterized in that: the lithium secondary battery comprises a positive pole piece, a negative pole piece, a diaphragm and a nano composite gel electrolyte, wherein the nano composite gel electrolyte consists of hydrophobic modified nano particles and electrolyte and is used for being spaced between the battery diaphragm and the positive and negative poles.
4. A method for preparing a lithium secondary battery according to claim 3, characterized by comprising the steps of:
(a) adding the hydrophobic modified nano particles into an organic solvent II, and fully stirring to form colloidal slurry;
(b) coating the colloidal slurry prepared in the step (a) on two sides of a diaphragm, and performing vacuum drying to obtain the diaphragm coated with the nano particle coating;
(c) assembling the battery cell according to the positive pole piece, the diaphragm coated with the nano particle coating prepared in the step (b) and the negative pole piece in sequence;
(d) and injecting electrolyte into the battery cell to swell the nano particle coating into gel electrolyte, and then packaging the battery cell.
5. The method of manufacturing a lithium secondary battery according to claim 4, characterized in that: in the step (a), the mass fraction of the hydrophobically modified nanoparticles in an organic solvent II is 3-30%, and the organic solvent II is one or more of dimethylbenzene, methanol, ethanol, isopropanol, dioxane or N-methylpyrrolidone; the thickness of the coating of the colloidal slurry in the step (b) is 10-100 μm, and the temperature of vacuum drying is 25-100 ℃.
6. A method for preparing a lithium secondary battery according to claim 3, characterized by comprising the steps of:
(e) adding the hydrophobic modified nano particles into the electrolyte, and fully stirring to form the nano composite gel electrolyte;
(f) coating the nano composite gel electrolyte prepared in the step (e) on a diaphragm on two sides; obtaining a separator coated with a gel electrolyte;
(g) and (f) assembling and packaging the battery cell according to the positive pole piece, the diaphragm coated with the gel electrolyte and the negative pole piece in sequence.
7. The method of manufacturing a lithium secondary battery according to claim 6, characterized in that: the mass fraction of the hydrophobic nano particles in the nano composite gel electrolyte in the step (e) is 3-30%, and the thickness of the nano composite gel electrolyte coated in the step (f) is 5-50 μm.
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| CN109888265B (en) * | 2019-01-28 | 2021-08-10 | 南京师范大学 | Hydrogel-derived silicon-titanium alloy interconnection network material and preparation method and application thereof |
| CN110212241A (en) * | 2019-06-12 | 2019-09-06 | 哈尔滨工业大学 | A kind of solid electrolyte membrane and its preparation process and application |
| CN111196888B (en) * | 2020-01-06 | 2020-12-11 | 浙江大学 | Gel polymer electrolyte doped with modified particles and preparation method and application thereof |
| CN111435757B (en) * | 2020-04-02 | 2021-10-15 | 珠海冠宇电池股份有限公司 | Composite polymer electrolyte, preparation method thereof and lithium battery |
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