CN113381123A - SiO (silicon dioxide)2Method for modifying meta-aramid lithium ion battery diaphragm by using nano particles - Google Patents
SiO (silicon dioxide)2Method for modifying meta-aramid lithium ion battery diaphragm by using nano particles Download PDFInfo
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- CN113381123A CN113381123A CN202110723974.2A CN202110723974A CN113381123A CN 113381123 A CN113381123 A CN 113381123A CN 202110723974 A CN202110723974 A CN 202110723974A CN 113381123 A CN113381123 A CN 113381123A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/443—Particulate material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
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Abstract
The invention discloses a SiO2A method for modifying a meta-aramid lithium ion battery diaphragm by using nanoparticles. The method comprises the following steps: slowly placing the meta-aramid fiber lithium ion battery diaphragm in a non-ionic surfactant or silane coupling agent solution, magnetically stirring, deionized water, vacuum drying, and then obtaining the lithium ion battery diaphragmSlowly putting the mixture into a solution of tetraethoxysilane, water, ethanol and ammonia water, stirring, washing by deionized water, and drying in vacuum to obtain the product. The diaphragm prepared by the invention is SiO2The nano particles are uniformly dispersed on the surface and inside of the meta-aramid diaphragm, so that the performance of the lithium ion battery is improved. At the same time, SiO2The addition of the nano particles not only improves the mechanical strength of the battery diaphragm, but also improves the SiO property2The nano particles belong to inorganic substances, have excellent temperature resistance, and can improve the temperature resistance of the battery diaphragm.
Description
Technical Field
The invention relates to a preparation method of a lithium battery composite diaphragm, in particular to a SiO2A preparation method of a meta-aramid lithium battery diaphragm modified by inorganic nanoparticles.
Background
Lithium batteries are widely used not only in portable electronic devices (e.g., mobile phones, laptop computers, digital cameras), but also in hybrid electric vehicles and satellites. With the rapid development of lithium ion batteries in high power applications, the safety and reliability of these batteries becomes critical. In battery systems, the role of the battery separator is to prevent direct contact between the positive and negative electrodes, to avoid short circuits, while promoting ion transport in the battery is one of the most critical components to ensure safe operation of the battery.
At present, commercial battery separators mainly comprise polyolefin separators such as PP (polypropylene), PE (polyethylene) and the like, and the commercial separators can meet the general requirements of lithium ion batteries, such as proper thickness, high mechanical strength, good chemical stability and the like. However, the polyolefin-based separator has disadvantages of low porosity, poor thermal stability, poor electrolyte wettability, etc., which severely limit the electrochemical performance of the lithium ion battery and may cause serious safety problems. The meta-aramid (PMIA) is a high-temperature resistant material with wide application, has extremely high thermal stability (up to 400 ℃), and has excellent self-extinguishing property and chemical corrosion resistance. Therefore, PMIA has received much attention as a novel lithium ion battery separator material. However, since the resin has disadvantages of low mechanical strength and poor wettability with respect to an electrolytic solution, further improvement in performance by modification treatment is required. The inorganic nano silicon dioxide has small grain diameter, large specific surface area, good biocompatibility, surface interface effect of nano material,Small size effect, quantum size effect and the like, and is a common material for modifying the lithium ion battery diaphragm. However, the surface of the nano silicon dioxide is high in energy, is in a thermodynamic unstable state, is very easy to agglomerate, is not easy to be fully mixed with organic matters, is hydrophilic and oleophobic, is difficult to be uniformly dispersed in an organic medium, has poor binding force with an organic matrix, easily causes interface defects, and reduces the performance of the diaphragm. Therefore, many researchers have tried to solve this problem by working with SiO2Nano particles are modified to improve SiO2Bonding with organic matrix to promote SiO2Dispersion of nanoparticles in an organic medium. Zhengxuan et al by using gamma-methacryloxypropyltrimethoxysilane and SiO2Complexing and grafting modification are carried out to the modified SiO2The solution is subjected to electrostatic spraying to obtain nano-scale SiO2 particles, and the nano-SiO particles are subjected to electrostatic spraying by the method2And the lithium battery composite diaphragm is successfully prepared by electrostatic spraying on the ultra-high molecular weight polyethylene diaphragm. The shrinkage rate of the composite membrane is reduced to 1.32% from 7.28%, and the porosity is increased to 61.15% from 37.85%. (Zhengxuan, Liutaiqi. electrostatic spraying method for preparing nano silicon dioxide/ultra-high molecular weight polyethylene lithium ion battery composite diaphragm [ J]New technology and new process, 2019(07):14-18.) Zhang Jiang et al uses pyridinium cation and bis (trifluoromethyl) sulfimide anion with silane coupling agent to SiO2The surface of the nano particle is modified to form a dendritic structure on the surface of the nano particle, so that the surface of the nano particle is provided with a specific functional group, the migration resistance of anions is increased, and the migration number of Li & lt + & gt is increased. (Zhang Yangjiang, Zhang lan, Cheng Yuan, modified nanometer SiO2Particles, method for preparing the same, and nanofiber membrane, gel electrolyte and lithium metal battery [ P ] comprising the same]Chinese CN 108281705A.).
SiO in the above report2Although the nanoparticles can be dispersed in an organic medium, the preparation process is relatively complicated, and relatively more solvents are required, so that the nanoparticles are not suitable for industrial large-scale application.
Disclosure of Invention
The invention aims at the prior SiO2The nanoparticles are easy to agglomerate when PMIA is modified, so that an interface is causedThe defects that the PMIA diaphragm can not be effectively improved and the like, and the method has simple operation, is suitable for large-scale industrial application and can realize SiO2The uniform modification of the nano particles on the PMIA film surface improves the mechanical property of the diaphragm and obtains SiO with good battery cycle performance2A preparation method of an inorganic nanoparticle modified meta-aramid lithium battery diaphragm.
The invention is realized by the following technical scheme: the invention relates to SiO2The method for modifying the meta-aramid lithium ion battery diaphragm by the inorganic nanoparticles comprises the following steps:
(1) adding a nonionic surfactant or silane coupling agent into a solvent, stirring and completely dissolving to obtain a solution A, wherein the mass fraction of the nonionic surfactant or silane coupling agent in the solution A is 0.5-4%;
(2) slowly placing the meta-aramid fiber lithium ion battery diaphragm in the solution A, magnetically stirring for 1-4h, taking out, washing for 3-5 times by using deionized water, and vacuum drying at 60 ℃;
(3) slowly adding ethyl orthosilicate and water into ethanol, then slowly dropwise adding ammonia water to obtain a solution B, stirring for 30s-1min, slowly placing the meta-aramid fiber lithium ion battery diaphragm obtained in the step 2) into the solution B, stirring for 1-4h, taking out, washing for 3-5 times with deionized water, and carrying out vacuum drying at 60 ℃ for 24-48h to obtain SiO2The nano particle modified meta-aramid lithium ion battery diaphragm is characterized in that the volume ratio of substances in the solution B is VTEOS：VWater (W)：VEthanol：VAqueous ammonia＝1：3～4：80～150：1～1.5。
The non-ionic surfactant is one or more of tween 80, tween 60, tween 20, lauryl phosphate, oleyl alcohol, stearyl alcohol, polyglycerol stearate and glycerol oleate, and particularly preferably the non-ionic surfactant is tween 80.
The silane coupling agent is one or more of gamma-Aminopropyltriethoxysilane (APTES), gamma- (methacryloyloxy) propyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane (ethyl) oxysilane and N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, and particularly preferably, the silane coupling agent is gamma-aminopropyltriethoxysilane.
The solvent is one or more of ethanol, methanol and water, and particularly preferably the solvent is ethanol.
The invention has the beneficial effects that:
(1) SiO prepared by the method of the invention2The nano particles can be uniformly dispersed on the surface and inside of the meta-aramid diaphragm, and can give full play to SiO2The advantages of nano particles are not caused by SiO2The agglomeration of the nanoparticles affects the performance of the lithium ion battery.
(2) Nano SiO2The addition of the SiO improves the mechanical strength of the battery diaphragm, improves the electrochemical properties (such as cycle performance and the like) of the lithium ion battery, and the SiO improves the electrochemical properties of the lithium ion battery2The nano particles belong to inorganic substances, have excellent temperature resistance, and can improve the temperature resistance of the battery diaphragm.
Drawings
Fig. 1 is an SEM image of a modified meta-aramid lithium ion battery separator prepared in example 1 of the present invention;
FIG. 2 is a stress-strain graph of the separator according to example 1 of the present invention and the separator according to the comparative example;
fig. 3 and 4 are graphs showing rate and cycle performance of the surface of the battery after the separators prepared in example 1 and comparative example were assembled into the battery.
Detailed Description
The technical scheme of the invention is further explained by combining the specific embodiment and the attached drawings of the specification.
Comparative example 1
PMIA diaphragm prepared by NIPS method is dried, cut into 15.8cm round pieces by a film cutter, assembled into a lithium ion battery in an inert gas glove box and tested for performance. The experimental results show that the ionic conductivity of the battery assembled by the PMIA diaphragm is 0.52mS/cm, and the capacity retention rate is 70.1% after 50 cycles of charge and discharge.
Example 1
Weighing Tween 805 g, adding into 500ml deionized water, stirring, adding meta-aramid fiber (prepared by NIPS method) membrane, and slowly addingStirring for 2 h. And washing, filtering and drying the obtained pretreated diaphragm to obtain the pretreated diaphragm. Taking another beaker, mixing TEOS: water: uniformly mixing ethanol at a volume ratio of 1:1:3:80, stirring for 30s, placing a pretreatment membrane in the mixture, slowly stirring for 2h, taking out, drying, and confirming SiO by SEM picture2Evenly distributed (as shown in figure 1). Finally, the ionic conductivity of the PMIA diaphragm is measured to be 0.78mS/cm, the capacity retention rate of the battery after 50 cycles of charge and discharge is 88.1%, and the performance of the battery is obviously superior to that of the battery assembled by the PMIA diaphragm (see figure 4)
Example 2
Weighing and adding 2010 g of Tween into 500ml of deionized water, stirring uniformly, adding a meta-aramid (prepared by a NIPS method) diaphragm, and slowly stirring for 1 h. And washing, filtering and drying the obtained pretreated diaphragm to obtain the pretreated diaphragm. Taking another beaker, mixing TEOS: water: uniformly mixing ethanol at a volume ratio of 1:1.5:5:120, stirring for 60s, placing a pretreatment diaphragm therein, slowly stirring for 4h, taking out, drying, and confirming SiO by SEM picture2Are uniformly distributed. Finally, the ionic conductivity of the PMIA diaphragm is measured to be 0.75mS/cm, the capacity retention rate of the battery is 87.5 percent after the battery is charged and discharged for 50 circles, and the performance of the battery is obviously superior to that of the battery assembled by the PMIA diaphragm.
Example 3
Weighing 5g of gamma-aminopropyltriethoxysilane, adding the gamma-aminopropyltriethoxysilane into 500ml of ethanol, uniformly stirring, adding a PP diaphragm, and slowly stirring for 2 hours. And washing, filtering and drying the obtained pretreated diaphragm to obtain the pretreated diaphragm. Taking another beaker, mixing TEOS: water: mixing ethanol at a volume ratio of 1:1:4:80, stirring for 30s, adding the pretreatment membrane, slowly stirring for 3h, taking out, drying, and taking out from SEM picture to obtain SiO2Are uniformly distributed. Finally, the ionic conductivity of the PMIA diaphragm is measured to be 0.74mS/cm, the capacity retention rate of the battery is 87.8 percent after the battery is charged and discharged for 50 circles, and the performance of the battery is obviously superior to that of the battery assembled by the PMIA diaphragm.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose of the embodiments 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.
The invention is not the best known technology.
Claims (4)
1. SiO (silicon dioxide)2The preparation method of the nano particle modified meta-aramid lithium ion battery diaphragm is characterized in that,
1) preparing a solution A with the mass fraction of the nonionic surface active or silane coupling agent being 0.5-4%;
2) slowly placing the meta-aramid lithium ion battery diaphragm in the solution A, magnetically stirring for 1-4h, taking out, washing for 3-5 times by using deionized water, and then drying in vacuum;
3) slowly adding ethyl orthosilicate and water into ethanol, then slowly dropwise adding ammonia water to obtain a solution B, stirring for 30s-1min, slowly placing the lithium ion battery diaphragm obtained in the step 2) into the solution B, stirring for 1-4h, taking out, washing for 3-5 times by using deionized water, and drying in vacuum to obtain SiO2Modifying the lithium ion battery diaphragm by the nano particles;
wherein the volume ratio of substances in the solution B is V (tetraethoxysilane): v (water): v (ethanol): ammonia water 1: 3-4: 80-150: 1 to 1.5.
2. The preparation method according to claim 1, wherein the solvent of the solution A is one or more of ethanol, methanol and water.
3. The method according to claim 1, wherein the non-ionic surfactant is one or more of tween 80, tween 60, tween 20, lauryl phosphate, oleyl alcohol, stearyl alcohol, polyglyceryl stearate, and glyceryl oleate.
4. The method according to claim 1, wherein the silane coupling agent is one or more of γ -Aminopropyltriethoxysilane (APTES), γ - (methacryloyloxy) propyltrimethoxysilane, N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane (etha) and N- β - (aminoethyl) - γ -aminopropylmethyldimethoxysilane.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115911752A (en) * | 2023-01-29 | 2023-04-04 | 河北工业大学 | Method for coating meta-aramid fiber lithium ion battery diaphragm with sodium alginate |
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| CN115911752A (en) * | 2023-01-29 | 2023-04-04 | 河北工业大学 | Method for coating meta-aramid fiber lithium ion battery diaphragm with sodium alginate |
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