CN114552118A - Cellulose-based sodium-ion battery diaphragm and preparation method thereof - Google Patents
Cellulose-based sodium-ion battery diaphragm and preparation method thereof Download PDFInfo
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- CN114552118A CN114552118A CN202210087640.5A CN202210087640A CN114552118A CN 114552118 A CN114552118 A CN 114552118A CN 202210087640 A CN202210087640 A CN 202210087640A CN 114552118 A CN114552118 A CN 114552118A
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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
- H01M10/054—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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/44—Fibrous material
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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
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Abstract
The invention belongs to the technical field of sodium ion batteries, and discloses a cellulose-based sodium ion battery diaphragm and a preparation method thereof. The method comprises the following steps: 1) uniformly dispersing the plant fiber slurry and the glass fiber solution to obtain a composite slurry; 2) and (3) papermaking the composite slurry to obtain the cellulose-based sodium-ion battery diaphragm. The method provided by the invention not only improves the mechanical strength, heat resistance and liquid absorption of the diaphragm, but also increases the sodium ion conductivity of the diaphragm, so that the diaphragm shows excellent cycle stability and rate capability when applied to a sodium ion battery. The preparation method is simple, low in cost, safe and environment-friendly, and can be suitable for industrial large-scale production.
Description
Technical Field
The invention belongs to the technical field of sodium ion batteries, and particularly relates to a cellulose-based sodium ion battery diaphragm and a preparation method thereof.
Background
The lithium ion battery has the advantages of high working voltage, high specific energy density, small self-discharge, long cycle life, rapid charge and discharge and the like, and is widely applied to the fields of portable equipment, electric automobiles, smart power grids and the like as an energy storage and power system. However, the shortage and the uneven distribution of lithium resources inevitably restrict the large-scale application of lithium ion batteries. Therefore, it is imperative to develop a secondary battery that can replace lithium ion batteries. Sodium-ion batteries are considered a promising alternative to lithium-ion batteries because of the greater sodium reserves in earth than lithium, while they have a similar operating principle as lithium-ion batteries.
Like lithium ion batteries, sodium ion batteries are mainly composed of a positive electrode, a negative electrode, a current collector, an electrolyte, a diaphragm and a battery case. In recent years, research on sodium ion batteries has focused on materials of positive and negative electrodes, and attention to separators of sodium ion batteries has been very little. The diaphragm is used as a key component of the sodium ion battery, and plays a role in isolating the positive plate from the negative plate in the battery, blocking electrons in a circuit from passing during charging and discharging, and allowing sodium ions in electrolyte to freely pass through. Polyolefin battery separators, including polyethylene and polypropylene separators, which are currently commercialized, have poor wettability to sodium ion battery electrolytes and low thermal stability, and are therefore not well suited for sodium ion batteries.
Sodium ion battery separators which are researched more at home and abroad are mainly divided into three types: polyolefin composite diaphragm, organic polymer non-woven fabric and glass fiber filter paper. The polyolefin composite separator is obtained by compounding an organic or inorganic material with an existing commercial polyolefin separator, and has the advantages of thin thickness, low resistance, poor wettability and poor thermal stability. Glass fiber filter paper is fibrous non-woven filter paper made of inorganic materials, has large thickness, is expensive, has low tensile strength, and is not suitable for large-scale use. At present, a sodium ion battery diaphragm commonly used in a laboratory is generally a glass fiber diaphragm, a thicker glass fiber diaphragm easily causes overlarge internal resistance of the battery, so that the performance of the battery is reduced, and poor mechanical strength can cause local short circuit to cause safety problems.
Disclosure of Invention
Aiming at the problems of a glass fiber diaphragm commonly used for a sodium ion battery, the invention provides a cellulose-based sodium ion battery diaphragm and a preparation method thereof. The method is simple, low in cost, safe and environment-friendly, and capable of realizing large-scale production, and the prepared cellulose-based sodium ion battery diaphragm has high ionic conductivity and good electrolyte wettability, mechanical property and cycle performance.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a cellulose-based sodium-ion battery diaphragm comprises the following steps:
1) uniformly dispersing the plant fiber slurry and the glass fiber solution to obtain a composite slurry;
2) and (3) papermaking the composite slurry to obtain the cellulose-based sodium-ion battery diaphragm.
The beating degree of the plant fiber slurry is 72-91 DEG SR.
The cellulose-based raw material of the plant fiber pulp in the step 1) is one or a mixture of bamboo pulp and northern softwood pulp, and the softwood pulp is preferred.
The plant fiber slurry is obtained by pulping a cellulose-based raw material, and is specifically obtained by pulping the cellulose-based raw material by using a trough type pulping machine.
The glass fiber solution is obtained by dispersing glass fibers in a sulfuric acid solution; the sulfuric acid solution is a sulfuric acid solution with the pH of 2.5-3.5, and preferably a sulfuric acid solution with the pH of 3; the mass concentration of the glass fiber in the glass fiber solution is 1-3%.
The dispersion means defibering in a standard fiber defibrator, and the rotational speed of the defibering is 8000-12000 revolutions, preferably 9000-11000 revolutions.
The mass ratio of the oven dry mass of the plant fiber slurry to the glass fiber in the step 1) is 1: 9-9: 1, preferably 7: 3-3: 7, more preferably 6.5: 3.5-5.5: 4.5.
the concentration of the plant fiber slurry is 5-15 wt%.
When dispersing, water can be added according to the needs, and the volume mass ratio of the added amount of the water to the glass fiber is (1.5-2.5) L: (0.5-1) g.
The papermaking quantitative amount of the papermaking paper in the step 2) is 30-50g/m2；
After papermaking, a handsheet was obtained, and the handsheet was dried to obtain a separator.
The drying temperature is 80-100 ℃, and the drying time is 10-15 min.
The cellulose-based sodium ion battery diaphragm is manufactured by mixing softwood pulp or bamboo pulp and glass fiber according to a preset mass ratio and is manufactured by papermaking, and the thickness of the obtained diaphragm is 90-120 mu m.
Compared with the prior art, the invention has the following beneficial effects:
(1) the diaphragm of the invention has good electrolyte wettability, thermal stability and better mechanical property. The invention is beneficial to the transmission of sodium ions in the charging and discharging process by adjusting the aperture of the diaphragm, thereby improving the ionic conductivity of the diaphragm. The diaphragm assembled sodium-ion battery prepared by the method shows excellent cycle stability and rate capability.
(2) The raw materials selected by the bamboo cultivation method are green and sustainable, on one hand, the integrated utilization of wood resources can be enhanced, on the other hand, the bamboo planted at one time can be continuously used for several years due to the short growth period of the bamboo, and the bamboo cultivation method accords with the integrated circulation development mode of the wood pulp.
(3) The cellulose-based sodium ion battery diaphragm is simple in preparation method, low in cost, safe and environment-friendly, and can be applied to industrialization.
Drawings
FIG. 1 is a graph of the cycle performance at 1C of cellulose-based sodium ion battery separators prepared in examples 1-3;
FIG. 2 is a graph of the cycle performance at 1C for cellulose-based sodium ion battery separators prepared in examples 3-7;
FIG. 3 is a tensile property stress-strain curve of cellulose-based sodium ion battery separators prepared in examples 3-7;
FIG. 4 is a scanning electron microscope image of a cellulose-based sodium ion battery separator prepared in example 6;
FIG. 5 is the cycle performance at 10C of the cellulose-based sodium ion battery separator prepared in example 6;
fig. 6 is a graph showing rate performance of the cellulose-based sodium-ion battery separator prepared in example 6.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
In the embodiment, the plant fiber pulp is obtained by pulping a cellulose-based raw material to a certain pulping degree by using a groove type pulping machine.
Example 1
Bleached sulfate northern softwood pulp and glass fiber are used as raw materials, and the weight ratio of absolute dry to mass is 1: 1 weighing 72 DEG SR softwood pulp (7.85g, wood pulp concentration of 10 wt%) and 2% wt. glass fiber solution (39.25g), mixing, adding a proper amount of clear water (about 2L), defibering in a standard fiber dissociator for 10000 turns, pouring the dispersed mixed slurry into a rapid Kaiser method paper sheet forming machine, stirring, standing, draining, vacuumizing to obtain handsheets (papermaking quantitative of 50 g/m)2) And then drying for 10min at 90 ℃ under vacuum to finish papermaking and obtain the diaphragm. The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 2
Bleached sulfate northern softwood pulp and glass fiber (the diameter is 0.5-2 mu m, and the length is 0.5-5 mm) are used as raw materials, and the weight ratio of absolute dry to mass is 1: 1, respectively weighing 91-degree SR softwood pulp (7.85g, the concentration of wood pulp is 10 wt%) and 2 wt% glass fiber solution (39.25g), mixing, adding a proper amount of clear water, defibering in a standard fiber dissociator for 10000 revolutions, pouring the dispersed mixed slurry into a rapid Kaiser method paper sheet forming machine, obtaining handsheets after the processes of stirring, standing, draining and vacuumizing, and then drying for 10min under vacuum at 90 ℃ to finish papermaking. The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 3
Bleached sulfate northern softwood pulp and glass fiber are used as raw materials, and the weight ratio of absolute dry to mass is 1: 1, respectively weighing 80-degree SR softwood pulp (7.85g, the concentration of wood pulp is 10 wt%) and 2 wt% glass fiber solution (39.25g), mixing, adding a proper amount of clear water, defibering in a standard fiber dissociator for 10000 revolutions, pouring the dispersed mixed slurry into a rapid Kaiser method paper sheet forming machine, obtaining handsheets after the processes of stirring, standing, draining and vacuumizing, and then drying for 10min under vacuum at 90 ℃ to finish papermaking. The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 4
Bleached sulfate northern softwood pulp and glass fiber are used as raw materials, and the weight ratio of absolute dry to glass fiber is 3: 7 weighing 80-degree SR softwood pulp (4.71g, the concentration of wood pulp is 10 wt%) and 2 wt% glass fiber solution (54.95g) respectively, mixing, adding a proper amount of clear water, defibering in a standard fiber dissociator for 10000 revolutions, pouring the dispersed mixed slurry into a rapid Kaiser method paper sheet forming machine, obtaining handsheets after the processes of stirring, standing, draining and vacuumizing, and then drying for 10min under vacuum at 90 ℃ to finish papermaking. The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 5
Bleached sulfate northern softwood pulp and glass fiber are used as raw materials, and the weight ratio of absolute dry to mass is 4: 6, respectively weighing 80-degree SR softwood pulp (6.28g, the concentration of wood pulp is 10 wt%) and 2 wt% glass fiber solution (47.1g), mixing, adding a proper amount of clear water, defibering in a standard fiber dissociator for 10000 revolutions, pouring the dispersed mixed slurry into a rapid Kaiser paper forming machine, stirring, standing, draining, vacuumizing to obtain handsheets, and then drying at 90 ℃ for 10min in vacuum to finish papermaking. The prepared diaphragm is pressed into a 16mm round piece by a punching machine and is placed for standby.
Example 6
Bleached sulfate northern softwood pulp and glass fiber are used as raw materials, and the weight ratio of absolute dry to the weight ratio of 6: 4, respectively weighing 80-degree SR softwood pulp (9.42g, the concentration of wood pulp is 10 wt%) and 2 wt% glass fiber solution (31.4g), mixing, adding a proper amount of clear water, defibering in a standard fiber dissociator for 10000 revolutions, pouring the dispersed mixed slurry into a rapid Kaiser paper forming machine, obtaining handsheets after the processes of stirring, standing, draining and vacuumizing, and then drying for 10min at 90 ℃ in vacuum to finish papermaking. The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
Example 7
Bleached sulfate northern softwood pulp and glass fiber are used as raw materials, and the weight ratio of absolute dry to mass is 7: 3, respectively weighing 80-degree SR softwood pulp (10.99g, the concentration of wood pulp is 10 wt%) and 2 wt% glass fiber solution (23.55g), mixing, adding a proper amount of clear water, defibering in a standard fiber dissociator for 10000 revolutions, pouring the dispersed mixed slurry into a rapid Kaiser paper sheet forming machine, stirring, standing, draining, vacuumizing to obtain handsheets, and then drying at 90 ℃ for 10min in vacuum to finish papermaking. The prepared separator was pressed into a 16mm circular piece with a punch and placed for use.
The thickness, tensile strength, room temperature conductivity, air permeability, porosity, and liquid absorption of the cellulose-based sodium ion battery separator prepared in example were measured, and the results are shown in table 1. Vanadium sodium phosphate is used as a positive electrode, a sodium sheet is used as a negative electrode, and the sodium ion battery diaphragm prepared in the embodiment is assembled into a sodium ion battery, the discharge specific capacity of the sodium ion battery diaphragm is tested under 1C (1C-115 mA/g) for 200 cycles, the discharge specific capacity of the sodium ion battery diaphragm is tested under 10C for 1000 cycles in the embodiment 6, and the specific capacities under different multiplying powers are shown in the attached drawings.
FIG. 1 is a graph of the cycle performance at 1C of cellulose-based sodium ion battery separators prepared in examples 1-3;
FIG. 2 is a graph of the cycle performance at 1C for cellulose-based sodium ion battery separators prepared in examples 3-7;
FIG. 3 is a tensile property stress-strain curve of cellulose-based sodium ion battery separators prepared in examples 3-7;
FIG. 4 is a scanning electron microscope image of a cellulose-based sodium ion battery separator prepared in example 6;
FIG. 5 is the cycle performance at 10C of the cellulose-based sodium ion battery separator prepared in example 6;
fig. 6 is a graph showing rate performance of the cellulose-based sodium-ion battery separator prepared in example 6.
As can be seen from fig. 1 and 2, the battery using the separator of example 6 exhibited the most excellent cycle stability and reversible specific capacity. The composite diaphragm combines the advantages of cellulose and glass fiber, and the adjustment of the diaphragm aperture is beneficial to the transmission of sodium ions in the charge and discharge process, thereby improving the ionic conductivity of the diaphragm. In addition, the cycle stability of the battery has a great relationship with the mechanical strength of the separator, and the separator of example 6 has both good ionic conductivity and tensile strength. As can be seen from the SEM image of example 6 in FIG. 4, the cellulose in the pulp covers a large number of glass fiber holes, so that the pore size distribution of the diaphragm is adjusted, and the mechanical property of the diaphragm is effectively improved. The porosity and the liquid absorption rate of the diaphragm of the example 6 are tested, and the porosity is about 46%, the liquid absorption rate is about 351%, and meanwhile, the diaphragm has good wetting performance on the electrolyte. Therefore, the battery using the separator of example 6 exhibited excellent rate performance without much attenuation even after the number of charge and discharge times reached 1000.
Table 1 example separator performance
The above-mentioned embodiments are merely exemplary embodiments of the present invention, which are described in detail and specific, but should not be construed as limiting the scope of the present invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be covered by the scope of the present invention.
Claims (9)
1. A preparation method of a cellulose-based sodium-ion battery diaphragm is characterized by comprising the following steps: the method comprises the following steps:
1) uniformly dispersing the plant fiber slurry and the glass fiber solution to obtain a composite slurry;
2) making the composite slurry into paper to obtain a cellulose-based sodium-ion battery diaphragm;
the beating degree of the plant fiber slurry is 72-91 DEG SR; the mass ratio of the oven dry mass of the plant fiber slurry to the glass fiber in the step 1) is 1: 9-9: 1.
2. the method for preparing the cellulose-based sodium-ion battery separator according to claim 1, wherein: the cellulose-based raw material of the plant fiber pulp in the step 1) is one or a mixture of bamboo pulp and northern softwood pulp;
the mass ratio of the oven dry mass of the plant fiber slurry to the glass fiber in the step 1) is 7: 3-3: 7.
3. the method for preparing the cellulose-based sodium-ion battery separator according to claim 2, wherein:
the cellulose-based raw material of the plant fiber pulp in the step 1) is a northern softwood pulp board;
the mass ratio of the oven dry mass of the plant fiber slurry to the glass fiber in the step 1) is 6.5: 3.5-5.5: 4.5.
4. the method for preparing the cellulose-based sodium-ion battery separator according to claim 1, wherein:
the glass fiber solution is obtained by dispersing glass fibers in a sulfuric acid solution; the sulfuric acid solution is a sulfuric acid solution with the pH value of 2.5-3.5; the mass concentration of the glass fiber in the glass fiber solution is 1-3%;
the concentration of the plant fiber slurry is 5-15 wt%.
5. The method for preparing the cellulose-based sodium-ion battery separator according to claim 1, wherein:
the dispersion refers to defibering in a standard fiber dissociator, and the rotational speed of the defibering is 8000-12000 revolutions;
the papermaking quantitative amount of the papermaking paper in the step 2) is 30-50g/m2；
After papermaking, a handsheet was obtained, and the handsheet was dried to obtain a separator.
6. The method for preparing the cellulose-based sodium-ion battery separator according to claim 5, wherein: the dispersion refers to defibering in a standard fiber dissociator, and the rotational speed of the defibering is 9000-11000 revolutions;
the drying temperature is 80-100 ℃, and the drying time is 10-15 min.
7. The method for preparing the cellulose-based sodium-ion battery separator according to claim 5, wherein:
the thickness of the diaphragm is 90-120 mu m.
8. A cellulose-based sodium-ion battery separator obtained by the preparation method of any one of claims 1-6.
9. Use of a cellulose-based sodium-ion battery separator as claimed in claim 8, characterized in that: the cellulose-based sodium ion battery diaphragm is used for a sodium ion battery.
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