CN115101889A - Preparation method of silicon dioxide compounded polyacrylonitrile lithium battery diaphragm - Google Patents

Preparation method of silicon dioxide compounded polyacrylonitrile lithium battery diaphragm Download PDF

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CN115101889A
CN115101889A CN202210803466.XA CN202210803466A CN115101889A CN 115101889 A CN115101889 A CN 115101889A CN 202210803466 A CN202210803466 A CN 202210803466A CN 115101889 A CN115101889 A CN 115101889A
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polyacrylonitrile
silicon dioxide
lithium battery
mixed solution
pan
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梅顺齐
刘腾
陈龙
郑权
张百威
罗威
徐巧
陈振
张智明
汪佩
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Wuhan Textile University
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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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
    • 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
    • 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
    • H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
    • 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
    • H01M50/431—Inorganic material
    • H01M50/434—Ceramics
    • 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
    • H01M50/44—Fibrous material
    • 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
    • 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
    • H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Composite Materials (AREA)
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Abstract

A preparation method of a silicon dioxide compounded polyacrylonitrile lithium battery diaphragm comprises the steps of adding Polyacrylonitrile (PAN) and silicon dioxide (SiO 2) into N, N-dimethylformamide according to a required proportion, fully mixing to obtain a mixed solution, carrying out centrifugal spinning on the mixed solution to obtain Polyacrylonitrile (PAN) -silicon dioxide (SiO 2) nanofibers, collecting the nanofibers, and pressing the nanofibers at normal temperature to obtain the lithium battery diaphragm, wherein the mass sum of the Polyacrylonitrile (PAN) and the silicon dioxide (SiO 2) accounts for 19-21% of the total mass of the mixed solution, and the mass ratio of the Polyacrylonitrile (PAN) to the silicon dioxide (SiO 2) in the mixed solution is 96.5-97.5: 2.5-3.5. The silicon dioxide-compounded polyacrylonitrile lithium battery diaphragm prepared by the method has high thermal stability, the liquid absorption rate and the porosity are improved, and the working efficiency of the lithium battery is high.

Description

Preparation method of silicon dioxide compounded polyacrylonitrile lithium battery diaphragm
Technical Field
The invention belongs to the technical field of lithium battery materials, and particularly relates to a preparation method of a silicon dioxide-compounded polyacrylonitrile lithium battery diaphragm.
Background
Lithium ion batteries are widely used due to their advantages of high energy density, excellent cycle performance, high voltage, low charge loss, no memory effect, low pollution, and good safety. The diaphragm is used as one of the important components of the lithium ion battery, the diaphragm has the functions of isolating the positive electrode and the negative electrode, preventing the lithium ions from transferring through micropores while the open circuit is prevented, the size and the number of the micropores of the diaphragm determine the porosity of the diaphragm, and the porosity of the diaphragm influences the performances of internal resistance, multiplying power, high-temperature storage, circulation and the like of the battery.
Chinese patent: the invention with application publication number CN11026 of 5610A discloses a method for preparing a lithium battery diaphragm by using a centrifugal electrostatic spinning method, wherein a polyacrylonitrile fiber film is prepared by using the centrifugal electrostatic spinning method and then is subjected to suction filtration treatment in a SiO2 solution, although the liquid absorption rate and the heat shrinkage rate of the prepared lithium battery diaphragm are improved, the porosity, the liquid absorption rate and the heat stability are not greatly improved, and the requirement of high performance of a lithium battery cannot be met. Therefore, the prior art has the problems of poor porosity, poor liquid absorption rate and poor thermal stability of the lithium battery diaphragm and low working efficiency of the lithium battery.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of a silicon dioxide-compounded polyacrylonitrile lithium battery diaphragm, which improves the porosity, the liquid absorption rate and the thermal stability.
In order to achieve the above purpose, the invention provides the following technical scheme:
a preparation method of a silicon dioxide compounded polyacrylonitrile lithium battery diaphragm sequentially comprises the following steps:
s1 polyacrylonitrile PAN, silicon dioxide SiO 2 Adding the mixture into N, N-dimethylformamide according to a required proportion, and fully mixing to obtain a mixed solution, wherein the mixed solution comprises Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 The mass sum of the mixed solution accounts for 19 to 21 percent of the total mass of the mixed solution, and the mixed solution contains Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 The mass ratio of (A) to (B) is 96.5-97.5: 2.5-3.5;
s2, firstly, carrying out centrifugal spinning on the mixed solution obtained in the step S1 to obtain polyacrylonitrile PAN-silicon dioxide SiO 2 And collecting the nano fibers, and pressing the nano fibers at normal temperature to obtain the lithium battery diaphragm.
In step S2, the polyacrylonitrile PAN-silica SiO 2 The diameter of the nanofiber is 300-400 nm.
In step S2, the lithium battery separator has a thickness of 40-50 μm.
In step S2, the rotation speed of the centrifugal spinning is 4100-.
In step S1, the mixing is specifically stirring for 7.5-8.5h at 78-82 ℃.
In step S2, the pressure of the normal-temperature pressing is 9-11MPa, and the duration is 25-35 min.
In step S2, the polyacrylonitrile PAN-silica SiO 2 The collection of the nano-fibers is specifically that the nano-fibers obtained by centrifugal spinning are stood for 5-15min and then overlapped for 4-5 times along the orientation of the nano-fibers.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a preparation method of a polyacrylonitrile lithium battery diaphragm compounded with silicon dioxide, which comprises the steps of firstly preparing Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 Adding the mixture into N, N-dimethylformamide according to a required proportion, fully mixing to obtain a mixed solution, and then carrying out centrifugal spinning on the mixed solution to obtain polyacrylonitrile PAN-silica SiO 2 Collecting the nano fiber, and pressing at normal temperature to obtain lithium battery diaphragm, Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 The mass sum of the mixed solution accounts for 19 to 21 percent of the total mass of the mixed solution, and the mixed solution contains Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 The mass ratio of the SiO to the mixed solution is 96.5-97.5:2.5-3.5, and SiO is compounded in the mixed solution of the method 2 On one hand, the viscosity and the surface tension of the mixed solution are reduced, so that the nano fiber is stretched to be finer during centrifugal spinning, the diameter of the nano fiber is smaller, the porosity of the diaphragm is improved, lithium ions are transferred in the diaphragm more smoothly, and the working efficiency of the lithium battery is improved, on the other hand, the silicon dioxide SiO is not only used 2 The thermal stability of the diaphragm is improved, and the SiO is generated by the silicon dioxide 2 Has rich pore structure, can store a large amount of electrolyte, and silicon dioxide SiO 2 Has better affinity with the electrolyte, and improves the liquid absorption rate of the diaphragm. Therefore, the silicon dioxide-compounded polyacrylonitrile lithium battery diaphragm prepared by the invention has high thermal stability, improves the liquid absorption rate and porosity, and improves the working efficiency of the lithium battery.
Drawings
FIG. 1 is a graph showing the diameter distribution of nanofibers in a test example of the present invention.
FIG. 2 is a graph showing the diameter distribution of nanofibers according to comparative example 1 of the present invention.
FIG. 3 shows the results of the ion conductivity measurements of the test examples of the present invention and comparative examples 1 and 2.
FIG. 4 is the results of electrochemical oxidation limit analysis of the test examples of the present invention and comparative example 1.
FIG. 5 shows the results of electrochemical oxidation limit analysis of comparative example 2 in the present invention.
FIG. 6 is an electrochemical impedance spectrum of a test example of the present invention and comparative examples 1 to 3.
FIG. 7 shows the thermal stability performance of the test examples of the present invention and comparative example 1.
Detailed Description
The invention is further described with reference to the drawings and the detailed description.
A preparation method of a silicon dioxide compounded polyacrylonitrile lithium battery diaphragm sequentially comprises the following steps:
s1 polyacrylonitrile PAN, silicon dioxide SiO 2 Adding the mixture into N, N-dimethylformamide according to a required proportion, and fully mixing to obtain a mixed solution, wherein the mixed solution comprises Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 The mass sum of the mixed solution accounts for 19 to 21 percent of the total mass of the mixed solution, and the mixed solution contains Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 The mass ratio of (A) to (B) is 96.5-97.5: 2.5-3.5;
s2, carrying out centrifugal spinning on the mixed solution obtained in the step S1 to obtain polyacrylonitrile PAN-silica SiO 2 And collecting the nano fibers, and pressing the nano fibers at normal temperature to obtain the lithium battery diaphragm.
In step S2, the polyacrylonitrile PAN-silica SiO 2 The diameter of the nanofiber is 300-400 nm.
In step S2, the thickness of the lithium battery separator is 40-50 μm.
In step S2, the rotation speed of the centrifugal spinning is 4100-.
In step S1, the mixing is specifically carried out by stirring for 7.5-8.5h at 78-82 ℃.
In step S2, the pressure of the normal-temperature pressing is 9-11MPa, and the duration is 25-35 min.
In step S2, the polyacrylonitrile PAN-silica SiO 2 The collection of the nano-fiber is specifically that the nano-fiber obtained by centrifugal spinning is stood for 5-15min and then is overlapped for 4-5 times along the orientation of the nano-fiber.
Example 1:
a preparation method of a silicon dioxide compounded polyacrylonitrile lithium battery diaphragm specifically comprises the following steps:
s1 polyacrylonitrile PAN, silicon dioxide SiO 2 Adding the mixture into N, N-dimethylformamide according to a required proportion, and stirring the mixture for 9 hours in a magnetic stirrer at the temperature of 80 ℃ to obtain a mixed solution, wherein the polyacrylonitrile PAN and the silicon dioxide SiO 2 The mass sum accounts for 20 percent of the total mass of the mixed solution, and the mass ratio of polyacrylonitrile PAN to silicon dioxide SiO2 in the mixed solution is 97: 3;
s2, injecting the mixed solution obtained in the step S1 into a centrifugal spinning machine, adjusting the rotating speed of the centrifugal spinning machine to be 4200r/min, collecting the mixed solution with the distance of 30cm, and obtaining polyacrylonitrile PAN-silica SiO with the diameter of 300-400nm 2 A nanofiber;
and S3, standing the nanofibers obtained in the step S2 for 10min, then overlapping the nanofibers along the orientation of the nanofibers for 4 times to obtain nanofiber films, and pressing the nanofiber films for 35min at normal temperature under the pressure of 10MPa by using a hot press to obtain the lithium battery diaphragm with the thickness of 45 microns.
Example 2:
the difference from example 1 is that:
in step S1, the polyacrylonitrile PAN and the silicon dioxide SiO 2 The mass sum accounts for 19 percent of the total mass of the mixed solution, and the mass ratio of polyacrylonitrile PAN to silicon dioxide SiO2 in the mixed solution is 96.5: 3.5;
in step S2, the rotating speed of the centrifugal spinning machine is 4100r/min, and the collecting distance is 30 cm;
in step S3, the lithium battery separator with a thickness of 50 μm is obtained by overlapping the nanofibers for 5 times along the orientation and pressing at normal temperature for 25 min.
Example 3:
the difference from example 1 is that:
in step S1, the polypropyleneAlkenenitrile PAN, silicon dioxide SiO 2 The mass sum accounts for 19 percent of the total mass of the mixed solution, and the mass ratio of Polyacrylonitrile (PAN) to silicon dioxide (SiO 2) in the mixed solution is 97.5: 2.5;
in step S2, the rotating speed of the centrifugal spinning machine is 4300r/min, and the collecting distance is 32 cm;
in step S3, the lithium battery separator with a thickness of 40 μm is obtained by overlapping the nanofibers for 4 times along the orientation and pressing at normal temperature for 30 min.
And (3) performance testing:
the following performance tests were carried out using the lithium battery separator obtained in example 1 as a test example, using a separator obtained from a mixed solution a having a mass fraction of 20% (mixed solution B to which only polyacrylonitrile PAN was added) as a comparative example 1 (other preparation steps were the same as in example 1), and using a commercially available Celgard 2400 lithium battery separator as a comparative example 2:
1. nanofiber diameter testing
The diameters of 200 nanofibers in the test example and the comparative example 1 are randomly measured under a 1000-fold electron microscope and are subjected to summary statistics, the statistical results of the test example and the comparative example 1 are respectively shown in fig. 1 and fig. 2, as can be seen from fig. 1 and fig. 2, the diameter of the nanofiber in the comparative example 1 is between 400 and 500nm, and the diameter of the nanofiber in the test example is between 300 and 400 nm.
2. Porosity and imbibition testing
The porosity and the liquid absorption rate of the test examples and comparative examples 1 and 2 are detected, and the detection results are shown in table 1:
TABLE 1 porosity and imbibition test results
Figure DEST_PATH_IMAGE001
。
As can be seen from Table 1, the porosity and the liquid absorption of the test examples are significantly higher than those of the comparative examples 1 and 2.
3. Ion conductivity test
The ionic conductivity test was conducted on the test examples and comparative examples 1 and 2, and the results are shown in FIG. 3. from FIG. 3, it can be seen that the ionic conductivity of the test examples was 1.22mS/cm, which is significantly higher than that of comparative example 1, 1.18mS/cm, and that of comparative example 2, which is 0.79mSIs/cm, this is due to SiO 2 Has good affinity to electrolyte, SiO 2 The unsaturated Si-O bond and the hydroxyl group in (b) increase the absorption and retention capacity of the electrolyte.
4. Electrochemical oxidation limit analysis
In a battery system with lithium iron phosphate as a positive electrode and lithium metal as a negative electrode, electrochemical oxidation limit analysis is carried out on a test example and comparative examples 1 and 2 by using a linear sweep voltammetry, the electrochemical oxidation limit analysis result of the test example and the comparative example 1 is shown in figure 4, the electrochemical oxidation limit analysis result of the comparative example 2 is shown in figure 5, the corresponding voltage when the current sharply increases is the oxidation limit of the diaphragm, and the oxidation limit of the diaphragm of the test example is 5.4V and is obviously greater than 5.2V of the comparative example 1 and 4.3V of the comparative example 2.
5. Interfacial resistance analysis
In a battery system with lithium iron phosphate as a positive electrode and lithium metal as a negative electrode, an electrochemical impedance spectroscopy EIS of a test example and comparative examples 1 and 2 is detected, as shown in FIG. 6, the semi-circle diameter in a Nyquist plot shows the interface resistance of the diaphragm and the lithium metal, the interface resistance of the test example is 150ohm, which is obviously greater than 160ohm of the comparative example 1 and 300ohm of the comparative example 2, because the lithium battery diaphragm prepared by the centrifugal spinning technology has higher electrolyte absorptivity, the lithium ion migration resistance is reduced, and because SiO is used as a raw material, the electrochemical impedance spectroscopy EIS of the test example and the comparative examples 1 and 2 is obtained by detection, and the interface resistance is obviously greater than 160ohm of the comparative example 1 and 300ohm of the comparative example 2 2 Has better affinity with electrolyte, reduces the interface impedance to a certain extent, further improves the migration rate of lithium ions and the liquid retention capacity of a lithium battery diaphragm, and simultaneously SiO 2 And impurities generated by electrode reaction can be adsorbed, so that the interface stability is enhanced.
6. First charge and discharge performance and cycle performance test
In a battery system with lithium iron phosphate as a positive electrode and lithium metal as a negative electrode, the first charge-discharge performance of the battery provided with the test example and the diaphragms of the comparative examples 1 and 2 is detected under the multiplying power of 0.2C, and the detection result is as follows: the residual discharge specific capacity of the test example is 158.7mAh/g, which is obviously higher than 158.1mAh/g of comparative example 1 and 158.6mAh/g of comparative example 2. After 50 times of circulation under the multiplying power of 0.2C, the battery provided with the test example and the diaphragms of the comparative examples 1 and 2 is tested for the circulation performance, and the test result is as follows: the residual discharge specific capacity and the capacity retention rate of the test example are 153 mAh/g and 96.4 percent respectively, which are slightly higher than 151mAh/g and 95.5 percent of the comparative example 1 and 151mAh/g and 95.2 percent of the comparative example 3.
7. Thermal stability test
The thermal stability of the test example, comparative example 1, when heated to 150 c is shown in fig. 7. as can be seen from fig. 7, the separator of comparative example 1 has significant shrinkage, while the separator of test example has no shrinkage, indicating good thermal stability.

Claims (7)

1. A preparation method of a polyacrylonitrile lithium battery diaphragm compounded with silicon dioxide is characterized by comprising the following steps:
the preparation method comprises the following steps in sequence:
s1 polyacrylonitrile PAN, silicon dioxide SiO 2 Adding the mixture into N, N-dimethylformamide according to a required proportion, and fully mixing to obtain a mixed solution, wherein the mixed solution comprises Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 The mass sum of the mixed solution accounts for 19 to 21 percent of the total mass of the mixed solution, and the mixed solution contains Polyacrylonitrile (PAN) and silicon dioxide (SiO) 2 The mass ratio of (A) to (B) is 96.5-97.5: 2.5-3.5;
s2, carrying out centrifugal spinning on the mixed solution obtained in the step S1 to obtain polyacrylonitrile PAN-silica SiO 2 And collecting the nano fibers, and pressing the nano fibers at normal temperature to obtain the lithium battery diaphragm.
2. The preparation method of the silicon dioxide compounded polyacrylonitrile lithium battery diaphragm as claimed in claim 1 or 2, characterized in that: in step S2, the polyacrylonitrile PAN-silica SiO 2 The diameter of the nanofiber is 300-400 nm.
3. The preparation method of the silicon dioxide compounded polyacrylonitrile lithium battery diaphragm as claimed in claim 1 or 2, characterized in that: in step S2, the thickness of the lithium battery separator is 40-50 μm.
4. The preparation method of the silicon dioxide compounded polyacrylonitrile lithium battery diaphragm as claimed in claim 1 or 2, characterized in that: in step S2, the rotation speed of the centrifugal spinning is 4100-.
5. The preparation method of the silicon dioxide compounded polyacrylonitrile lithium battery diaphragm as claimed in claim 1 or 2, characterized in that: in step S1, the mixing is specifically stirring for 7.5-8.5h at 78-82 ℃.
6. The preparation method of the silicon dioxide compounded polyacrylonitrile lithium battery diaphragm as claimed in claim 1 or 2, characterized in that: in step S2, the pressure of the normal-temperature pressing is 9-11MPa, and the time duration is 25-35 min.
7. The preparation method of the silicon dioxide-compounded polyacrylonitrile lithium battery diaphragm as claimed in claim 1 or 2, is characterized in that: in step S2, the polyacrylonitrile PAN-silica SiO 2 The collection of the nano-fibers is specifically that the nano-fibers obtained by centrifugal spinning are stood for 5-15min and then overlapped for 4-5 times along the orientation of the nano-fibers.
CN202210803466.XA 2022-07-07 2022-07-07 Preparation method of silicon dioxide compounded polyacrylonitrile lithium battery diaphragm Pending CN115101889A (en)

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Citations (5)

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Publication number Priority date Publication date Assignee Title
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CN110265610A (en) * 2019-06-26 2019-09-20 广东工业大学 A kind of lithium battery diaphragm and preparation method thereof
CN114032670A (en) * 2021-10-22 2022-02-11 武汉纺织大学 Preparation method of high-temperature-resistant composite polyimide lithium ion battery diaphragm

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103971950A (en) * 2013-01-28 2014-08-06 海洋王照明科技股份有限公司 Electrochemical power source membrane, preparation method of electrochemical power source membrane and electrochemical battery or capacitor
CN106521717A (en) * 2015-09-11 2017-03-22 五邑大学 Preparation method of porous carbon fiber with high specific surface area
CN109449355A (en) * 2018-10-29 2019-03-08 郑州大学 A kind of battery modified polyacrylonitrile non-woven fabrics/aerosil composite diaphragm and preparation method thereof
CN110265610A (en) * 2019-06-26 2019-09-20 广东工业大学 A kind of lithium battery diaphragm and preparation method thereof
CN114032670A (en) * 2021-10-22 2022-02-11 武汉纺织大学 Preparation method of high-temperature-resistant composite polyimide lithium ion battery diaphragm

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
MELTEM YANILMAZ等: "SiO2/polyacrylonitrile membranes via centrifugal spinning as a separator for Li-ion batteries", 《JOURNAL OF POWER SOURCES》 *
张百威等: "纤维基锂离子电池隔膜制备技术研究进展", 《化工新型材料》 *

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