CN111180637A - Sodium ion battery diaphragm and preparation method and application thereof - Google Patents
Sodium ion battery diaphragm and preparation method and application thereof Download PDFInfo
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- CN111180637A CN111180637A CN202010013181.7A CN202010013181A CN111180637A CN 111180637 A CN111180637 A CN 111180637A CN 202010013181 A CN202010013181 A CN 202010013181A CN 111180637 A CN111180637 A CN 111180637A
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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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- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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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- 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
Abstract
The invention relates to a sodium ion battery diaphragm and a preparation method and application thereof, belonging to the technical field of sodium ion batteries. The invention aims to provide a sodium ion battery diaphragm with high liquid absorption rate and high conductivity. The sodium ion battery diaphragm is prepared from the following components in percentage by weight: 85-99% of sodium type perfluorinated sulfonic acid resin and 1-15% of sodium montmorillonite. The composite diaphragm is obtained by compounding the sodium type perfluorinated sulfonic acid resin and the sodium-based montmorillonite in a specific ratio, so that the sodium ion conductivity of the diaphragm is increased, the liquid absorption rate of an electrolyte membrane is improved, and the diaphragm shows high battery capacity and circulation stability when used for a sodium ion battery. The sodium ion battery diaphragm disclosed by the invention is simple in preparation method, low in cost, safe and environment-friendly, and can be applied to industrialization.
Description
Technical Field
The invention relates to a sodium ion battery diaphragm and a preparation method and application thereof, belonging to the technical field of sodium ion batteries.
Background
From the perspective of fossil fuel depletion and greenhouse effect, there is an urgent need to shift the production of electricity from traditional fossil fuels to renewable clean energy sources. By integration with battery technology, energy storage and conservation can be achieved and is widely used in a variety of applications. Rechargeable lithium ion batteries have been leading in the power market for portable electronic devices over the last three decades and are being applied to electric vehicles as technology develops. However, due to the increase in market demand and the shortage and uneven distribution of lithium resources, the widespread use of lithium batteries is threatened by the rapid rise in cost. Recently, a range of alkali metal ion batteries, including sodium (Na), potassium (K), magnesium (Mg) and aluminum (Al), have naturally attracted considerable attention.
Among them, sodium ion batteries are one of the best technologies for large-scale energy storage applications due to the unlimited and widespread sodium resources. The diaphragm plays an important role in isolating the positive electrode and the negative electrode of the battery, preventing short circuit, storing electrolyte, allowing the quick shuttling of sodium ions and the like. However, the separator of the sodium ion battery has received much less attention than the positive and negative electrode materials of the sodium ion battery with concentrated hot spots. Polyolefin separators that have been commercialized to date have failed to meet the energy storage requirements of high-safety large-scale sodium ion batteries due to their inherent poor wettability to sodium ion battery electrolytes (EC/PC, EC/DMC) and low thermal stability.
Currently, the most studied sodium ion battery separators mainly include three types, namely glass fiber filter paper, organic polymer non-woven fabrics and polyolefin composite separators. Glass fiber filter paper is fibrous non-woven filter paper prepared from inorganic materials, has large thickness, is not suitable for batteries with high energy density, is expensive and has low tensile strength. The polyolefin composite membrane is formed by compounding organic or inorganic materials with the existing commercial polyolefin membrane, and has the advantages of thin thickness, small resistance, poor wettability and low thermal stability. There are also some researchers using ion exchange membranes for sodium ion batteries to replace the conventional sodium ion separator, and these ion exchange membranes show more excellent electrochemical properties than the conventional liquid electrolyte after absorbing the electrolyte solvent. However, the membrane prepared by sodium modification of the ion exchange resin is poor in cycle stability when used in a sodium ion battery. Therefore, the development of new battery separators has been selected to meet the requirements of sodium ion batteries.
The perfluoro-sulfonic acid resin (Nafion-H) is the strongest known solid super acid and has the characteristics of good heat resistance, high chemical stability, high mechanical strength and the like. At present, the perfluorosulfonic acid membrane is a proton exchange membrane which is most applied in the development and development of proton exchange membrane fuel cells, and has good proton conductivity and chemical stability, but the principles of the fuel cells are completely different from those of sodium ion cells, the requirements on diaphragms are different, and the perfluorosulfonic acid membrane can not achieve good effects when being directly used for the sodium ion cells.
Patent CN108232262A discloses a high-barrier and high-tolerance composite proton exchange membrane and a preparation method thereof, the membrane is composed of 99-99.5% of ion exchange resin and 0.5-5% of orientation layer, wherein the ion exchange resin can be perfluorosulfonic acid resin, and the orientation layer can be modified montmorillonite. However, the patent is to compound sodium-based montmorillonite modified by an intercalating agent and ion exchange resin to form a film, the method is complex, and the film is a fuel cell film, does not have high liquid absorption rate and conductivity of a sodium ion battery, and is not suitable for the fuel cell.
Disclosure of Invention
In view of the above defects, the technical problem to be solved by the invention is to provide a sodium ion battery diaphragm with high liquid absorption rate and conductivity.
The invention relates to a sodium ion battery diaphragm which comprises the following components in percentage by weight: 85-99% of sodium type perfluorinated sulfonic acid resin and 1-15% of sodium montmorillonite.
Preferably, the thickness of the sodium ion battery diaphragm is 20-50 μm.
Preferably, the thickness of the sodium-ion battery separator is 30 μm.
The invention solves the second technical problem by providing the preparation method of the sodium-ion battery diaphragm.
The preparation method of the sodium ion battery diaphragm comprises the following steps:
1) mixing the sodium type perfluorinated sulfonic acid resin solution and the sodium-based montmorillonite dispersion liquid, and stirring at normal temperature to obtain mixed slurry; wherein, in the sodium type perfluorinated sulfonic acid resin solution, the mass fraction of solute is 5-20%, in the sodium montmorillonite dispersion, the mass fraction of dispersoid is 0.5-5%;
2) and preparing the mixed slurry into a membrane to obtain the sodium-ion battery diaphragm.
Preferably, the solvent of the sodium-type perfluorosulfonic acid resin solution is a high boiling point solvent.
Preferably, the high boiling point solvent is N, N dimethylformamide, N dimethylacetamide, N-methylpyrrolidone, or dimethylsulfoxide.
Preferably, the preparation method of the sodium-type perfluorosulfonic acid resin comprises the following steps: mixing H-type perfluorosulfonic acid powder with a NaOH solution with the concentration of 1-3 mol/L according to the mass ratio of 1: 8-12, stirring and reacting at 70-90 ℃ for 20-30H, taking out, washing and drying to obtain the sodium-type perfluorosulfonic acid resin.
Preferably, the preparation method of the sodium-type perfluorosulfonic acid resin comprises the following steps: mixing H-type perfluorosulfonic acid powder with a NaOH solution with the concentration of 2mol/L according to the mass ratio of 1:10, and stirring and reacting at 80 ℃ for 24 hours.
Preferably, the preparation method of the sodium montmorillonite dispersion liquid comprises the following steps: dispersing sodium-based montmorillonite in an acetone solvent, and performing ball milling for 3-5 h at the rotation speed of 450-500 rpm to obtain a sodium-based montmorillonite dispersion liquid.
The invention also provides application of the sodium-ion battery diaphragm in a sodium-ion battery.
The sodium ion battery diaphragm has good liquid absorption rate and conductivity, and can show high battery capacity and cycling stability when being used for a sodium ion battery.
Compared with the prior art, the invention has the following beneficial effects:
the composite diaphragm is obtained by compounding the sodium type perfluorinated sulfonic acid resin and the sodium-based montmorillonite in a specific ratio, so that the sodium ion conductivity of the diaphragm is increased, the liquid absorption rate of an electrolyte membrane is improved, and the diaphragm shows high battery capacity and circulation stability when used for a sodium ion battery.
The sodium ion battery diaphragm disclosed by the invention is simple in preparation method, low in cost, safe and environment-friendly, and can be applied to industrialization.
Drawings
FIG. 1 shows the cycle performance (current 1A g) of the separators prepared in examples 1 to 5 of the present invention-1)。
Detailed Description
The invention relates to a sodium ion battery diaphragm which is prepared from the following components in percentage by weight: 85-99% of sodium type perfluorinated sulfonic acid resin and 1-15% of sodium montmorillonite.
The sodium-type perfluorosulfonic acid resin is a resin in which a sulfonic acid group in the perfluorosulfonic acid resin is sodium-converted into sodium sulfonate. Because the perfluorosulfonic acid has good proton conductivity, the material has good sodium ion conductivity after being subjected to sodium treatment. Therefore, the sodium-modified perfluorosulfonic acid membrane, i.e., the sodium-type perfluorosulfonic acid resin, can be used not only as a separator but also as a carrier for Na ion transfer.
The sodium-based montmorillonite has good expansibility, adsorbability and cation exchange property, and is a layered structure which enables sodium ions to have good conductivity among layers of the sodium-based montmorillonite.
The sodium-type perfluorosulfonic acid resin and the sodium-based montmorillonite are compounded to prepare the composite diaphragm, and the sodium-based montmorillonite is doped into the sodium-type perfluorosulfonic acid membrane and supplements with each other, so that the sodium ion conductivity of the sodium-type perfluorosulfonic acid membrane is increased, the liquid absorption rate of an electrolyte membrane is improved, and the diaphragm shows high battery capacity and circulation stability when used for a sodium ion battery.
Preferably, the thickness of the sodium ion battery diaphragm is 20-50 μm.
Preferably, the thickness of the sodium-ion battery separator is 30 μm.
The preparation method of the sodium ion battery diaphragm comprises the following steps:
1) mixing the sodium type perfluorinated sulfonic acid resin solution and the sodium-based montmorillonite dispersion liquid, and stirring at normal temperature to obtain mixed slurry; wherein, in the sodium type perfluorinated sulfonic acid resin solution, the mass fraction of solute is 5-20%, in the sodium montmorillonite dispersion, the mass fraction of dispersoid is 0.5-5%;
2) and preparing the mixed slurry into a membrane to obtain the sodium-ion battery diaphragm.
Preferably, the solvent of the sodium-type perfluorosulfonic acid resin solution is a high boiling point solvent.
Preferably, the high boiling point solvent is N, N dimethylformamide, N dimethylacetamide, N-methylpyrrolidone, or dimethylsulfoxide.
Preferably, the preparation method of the sodium-type perfluorosulfonic acid resin comprises the following steps: mixing H-type perfluorosulfonic acid powder with a NaOH solution with the concentration of 1-3 mol/L according to the mass ratio of 1: 8-12, stirring and reacting at 70-90 ℃ for 20-30H, taking out, washing and drying to obtain the sodium-type perfluorosulfonic acid resin.
The structure of the sodium-type perfluorosulfonic acid resin prepared preferably is as follows:
among them, n is preferably 6 to 10.
Preferably, the preparation method of the sodium-type perfluorosulfonic acid resin comprises the following steps: mixing H-type perfluorosulfonic acid powder with a NaOH solution with the concentration of 2mol/L according to the mass ratio of 1:10, and stirring and reacting at 80 ℃ for 24 hours.
Preferably, the preparation method of the sodium montmorillonite dispersion liquid comprises the following steps: dispersing sodium-based montmorillonite in an acetone solvent, and performing ball milling for 3-5 h at the rotation speed of 450-500 rpm to obtain a sodium-based montmorillonite dispersion liquid.
The sodium ion battery diaphragm has good liquid absorption rate and conductivity, and can show high battery capacity and cycling stability when being used for a sodium ion battery.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention. The H-type perfluorosulfonic acid powder is a conventional commercially available acid-type perfluorosulfonic acid resin, i.e., a perfluorosulfonic acid resin as it is commonly referred to. Na-montmorillonite is also a conventional commercially available sodium montmorillonite. Both of the above two commercially available products are suitable for this scheme.
Example 1
(1) Mixing and stirring 20g H type perfluorosulfonic acid powder and 200g of 2mol/L NaOH solution, placing the mixture in a constant-temperature water bath kettle at 80 ℃, stirring the mixture for 24 hours, washing off redundant NaOH with deionized water, and drying the mixture to obtain Na type perfluorosulfonic acid powder.
(2) Dissolving Na type perfluorosulfonic acid powder in an N, N-dimethylacetamide solvent according to the mass fraction of the Na type perfluorosulfonic acid powder being 5%, heating and stirring the mixture at the temperature of 80 ℃ in a water bath to dissolve the Na type perfluorosulfonic acid powder, and obtaining Na type perfluorosulfonic acid solution (namely PFSA-Na solution) with the mass fraction being 5%.
(3) According to the mass fraction of Na-montmorillonite of 0.5%, Na-montmorillonite is dispersed in acetone solvent and ball milled for 3h at the rotating speed of 500rpm, and Na-montmorillonite dispersion liquid with the mass fraction of 0.5% is obtained.
(4) According to mass ratio: sodium-type perfluorosulfonic acid resin: 99 percent; sodium montmorillonite: 1 percent; and (3) adding the Na-based montmorillonite dispersion liquid in the step (3) into the PFSA-Na solution in the step (2), and mixing and stirring for 1h at normal temperature.
(5) The uniform slurry prepared above was uniformly coated on a glass plate by a doctor blade method, and the thickness of the separator was controlled to 30 μm.
(6) The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 2
(1) Mixing and stirring 20g H type perfluorosulfonic acid powder and 200g of 2mol/L NaOH solution, placing the mixture in a constant-temperature water bath kettle at 80 ℃, stirring the mixture for 24 hours, washing off redundant NaOH with deionized water, and drying the mixture to obtain Na type perfluorosulfonic acid powder.
(2) According to the mass fraction of the Na-type perfluorosulfonic acid powder being 10%, the Na-type perfluorosulfonic acid powder is dissolved in N, N-dimethylacetamide solvent, and is heated and stirred to be dissolved under the condition of water bath at 80 ℃, so that Na-type perfluorosulfonic acid solution (namely PFSA-Na solution) with the mass fraction of 10% is obtained.
(3) Taking Na-montmorillonite to disperse in an acetone solvent according to the mass fraction of the Na-montmorillonite of 5 percent, and ball-milling for 4 hours at the rotating speed of 500rpm to obtain montmorillonite dispersion liquid with the mass fraction of 3 percent.
(4) According to mass ratio: sodium-type perfluorosulfonic acid resin: 90 percent; sodium montmorillonite: 10 percent; and (3) adding the Na-based montmorillonite dispersion liquid in the step (3) into the PFSA-Na solution in the step (2), and mixing and stirring for 1h at normal temperature.
(5) The uniform slurry prepared above was uniformly coated on a glass plate by a doctor blade method, and the thickness of the separator was controlled to 30 μm.
(6) The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 3
(1) Mixing and stirring 20g H type perfluorosulfonic acid powder and 200g of 2mol/L NaOH solution, placing the mixture in a constant-temperature water bath kettle at 80 ℃, stirring the mixture for 24 hours, washing off redundant NaOH with deionized water, and drying the mixture to obtain Na type perfluorosulfonic acid powder.
(2) Taking Na type perfluorosulfonic acid powder as 20 percent by mass, dissolving the Na type perfluorosulfonic acid powder in N, N dimethylacetamide solvent, heating and stirring the mixture to dissolve the mixture at the temperature of 80 ℃ in water bath to obtain Na type perfluorosulfonic acid solution (namely PFSA-Na solution) with the mass percent of 20 percent.
(3) According to the mass percentage of Na-montmorillonite being 5%, Na-montmorillonite is dispersed in acetone solvent, and ball milling is carried out for 5h at the rotating speed of 500rpm, thus obtaining montmorillonite dispersion liquid with mass percentage of 5%.
(4) According to mass ratio: sodium-type perfluorosulfonic acid resin: 85 percent; sodium montmorillonite: 15 percent; and (3) adding the Na-based montmorillonite dispersion liquid in the step (3) into the PFSA-Na solution in the step (2), and mixing and stirring for 1h at normal temperature.
(5) The uniform slurry prepared above was uniformly coated on a glass plate by a doctor blade method, and the thickness of the separator was controlled to 30 μm.
(6) The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 4
(1) Mixing and stirring 20g H type perfluorosulfonic acid powder and 200g of 2mol/L NaOH solution, placing the mixture in a constant-temperature water bath kettle at 80 ℃, stirring the mixture for 24 hours, washing off redundant NaOH with deionized water, and drying the mixture to obtain Na type perfluorosulfonic acid powder.
(2) According to the mass fraction of the Na-type perfluorosulfonic acid powder being 20%, the Na-type perfluorosulfonic acid powder is dissolved in N, N-dimethylacetamide solvent, and is heated and stirred to be dissolved under the condition of water bath at 80 ℃, so that a Na-type perfluorosulfonic acid solution (namely a PFSA-Na solution) with the mass fraction of 20% is obtained.
(3) Taking Na-montmorillonite to disperse in an acetone solvent according to the mass fraction of the Na-montmorillonite of 5 percent, and ball-milling for 5 hours at the rotating speed of 500rpm to obtain montmorillonite dispersion liquid with the mass fraction of 5 percent.
(4) According to mass ratio: sodium-type perfluorosulfonic acid resin: 75 percent; sodium montmorillonite: 25 percent; and (3) adding the Na-based montmorillonite dispersion liquid in the step (3) into the PFSA-Na solution in the step (2), and mixing and stirring for 1h at normal temperature.
(5) The uniform slurry prepared above was uniformly coated on a glass plate by a doctor blade method, and the thickness of the separator was controlled to 30 μm.
(6) The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 5
(1) Mixing and stirring 20g H type perfluorosulfonic acid powder and 200g of 2mol/L NaOH solution, placing the mixture in a constant-temperature water bath kettle at 80 ℃, stirring the mixture for 24 hours, washing off redundant NaOH with deionized water, and drying the mixture to obtain Na type perfluorosulfonic acid powder.
(2) Dissolving 20g of Na-type perfluorosulfonic acid powder in 80g N N dimethylacetamide solvent, heating and stirring the mixture to dissolve the Na-type perfluorosulfonic acid powder in a water bath at 80 ℃ to obtain a Na-type perfluorosulfonic acid solution with the mass fraction of 20%.
(3) The uniform slurry prepared above was uniformly coated on a glass plate by a doctor blade method, and the thickness of the separator was controlled to 30 μm.
(4) The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
The electric conductivity at room temperature, liquid absorption rate and the negative electrode of the separators of examples and comparative examples were measured using hard carbon as the positive electrode and sodium sheet as the negative electrode at 1A g-1The discharge capacity at current was obtained, and the results are shown in Table 1.
TABLE 1
Cycling stability of different sodium ion membranes (Current 1A g)-1) See fig. 1. As can be seen from fig. 1, the battery using the separator of example 3 exhibited the optimal electrochemical stability, the number of charge and discharge cycles thereof was also up to 1000 cycles, and no significant capacity fade was exhibited. The cycling stability of examples 1, 2 was slightly poor, only between 400 and 600 cycles. But still much more excellent than examples 5 and 4. This demonstrates that the separator of the present invention can indeed improve the electrochemical performance of the battery.
Claims (10)
1. The sodium ion battery diaphragm is characterized by comprising the following components in percentage by weight: 85-99% of sodium type perfluorinated sulfonic acid resin and 1-15% of sodium montmorillonite.
2. The sodium ion battery separator of claim 1, wherein: the thickness of the sodium ion battery diaphragm is 20-50 mu m.
3. The sodium ion battery separator of claim 1, wherein: the thickness of the sodium ion battery diaphragm is 30 mu m.
4. A method for preparing a sodium-ion battery separator as claimed in any one of claims 1 to 3, comprising the steps of:
1) mixing the sodium type perfluorinated sulfonic acid resin solution and the sodium-based montmorillonite dispersion liquid, and stirring at normal temperature to obtain mixed slurry; wherein, in the sodium type perfluorinated sulfonic acid resin solution, the mass fraction of solute is 5-20%, in the sodium montmorillonite dispersion, the mass fraction of dispersoid is 0.5-5%;
2) and preparing the mixed slurry into a membrane to obtain the sodium-ion battery diaphragm.
5. The method for preparing a sodium-ion battery separator according to claim 4, wherein: the solvent of the sodium-type perfluorinated sulfonic acid resin solution is a high-boiling point solvent.
6. The method for preparing a sodium-ion battery separator according to claim 5, characterized in that: the high boiling point solvent is N, N dimethylformamide, N dimethylacetamide, N-methylpyrrolidone or dimethyl sulfoxide.
7. The method for preparing a sodium-ion battery separator according to claim 4, wherein: the preparation method of the sodium type perfluorinated sulfonic acid resin comprises the following steps: mixing H-type perfluorosulfonic acid powder with a NaOH solution with the concentration of 1-3 mol/L according to the mass ratio of 1: 8-12, stirring and reacting at 70-90 ℃ for 20-30H, taking out, washing and drying to obtain the sodium-type perfluorosulfonic acid resin.
8. The method for preparing a sodium-ion battery separator according to claim 7, characterized in that: the preparation method of the sodium type perfluorinated sulfonic acid resin comprises the following steps: mixing H-type perfluorosulfonic acid powder with a NaOH solution with the concentration of 2mol/L according to the mass ratio of 1:10, and stirring and reacting at 80 ℃ for 24 hours.
9. The method for preparing a sodium-ion battery separator according to claim 4, wherein: the preparation method of the sodium-based montmorillonite dispersion liquid comprises the following steps: dispersing sodium-based montmorillonite in an acetone solvent, and performing ball milling for 3-5 h at the rotation speed of 450-500 rpm to obtain a sodium-based montmorillonite dispersion liquid.
10. Use of the sodium ion battery separator of any one of claims 1 to 3 in a sodium ion battery.
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