CN114566713B - Electrolyte, preparation method thereof and method for preparing sodium ion battery by using electrolyte - Google Patents
Electrolyte, preparation method thereof and method for preparing sodium ion battery by using electrolyte Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H—ELECTRICITY
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- 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
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Abstract
The invention belongs to the technical field of sodium ion batteries. The invention provides an electrolyte and a preparation method thereof. The preparation method comprises the following steps: dissolving sodium salt in an ether solvent to obtain a solution; and adding dimethyl sulfoxide and fluoroether into the solution to obtain the electrolyte. The invention also provides a method for preparing the sodium ion battery by using the electrolyte. After the electrolyte is applied to the graphite anode material of the sodium ion battery for 60 circles, the graphite anode material still has 259.0 mAh.g ‑1 The reversible specific capacity of the electrolyte is improved by 93 percent compared with the electrolyte without dimethyl sulfoxide and fluoroether; and the preparation method is simple, easy to operate and suitable for industrial application.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to electrolyte, a preparation method thereof and a method for preparing a sodium ion battery by using the electrolyte.
Background
At present, commercialization of lithium ion batteries has been very successful, but the global lithium resource competition is becoming increasingly hotter, the dependence on lithium resources is eliminated, and a new battery system is not yet developed. Sodium is considered as the most promising alternative resource because of its similar chemical properties to lithium and its richer reserves, lower cost and better safety. The first generation of sodium ion batteries have been first released in the Nide era, commercializing sodium ion batteries, but there are many drawbacks. For example, since the relative atomic mass of sodium is much higher than that of lithium, the theoretical specific capacity of sodium ion batteries is less than 1/2 of that of lithium ion batteries; sodium ions are more difficult to intercalate and deintercalate in the battery material because the radius of sodium ions is 70% larger than the radius of lithium ions.
Graphite is the negative electrode material commonly used in lithium ion batteries, but inWhen using conventional carbonate-based electrolytes in sodium ion batteries, sodium ions are difficult to de-intercalate in the graphite layer, which is an important limitation in using graphite as the negative electrode material in sodium ion batteries. The current research shows that the use of ether solvent instead of traditional ester solvent in electrolyte can realize the stable deintercalation of sodium ions in graphite, thereby reaching about 150 mAh.g -1 But for commercial rechargeable batteries the energy density is still to be further improved. Therefore, how to improve the electrolyte of the sodium ion battery and further improve the charge and discharge performance of the sodium ion battery, and the preparation of the sodium ion battery with high energy density, high rate performance, long cycle life and high safety factor becomes a hot spot of current research.
Disclosure of Invention
The invention aims to provide an electrolyte, a preparation method thereof and a method for preparing a sodium ion battery by using the electrolyte, aiming at the defects in the prior art, so as to solve the problem of low energy density of the current graphite cathode applied to the sodium ion battery and improve the charge and discharge performance of a graphite cathode material in the sodium ion battery.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of electrolyte, which comprises the following steps:
1) Dissolving sodium salt in an ether solvent to obtain a solution;
2) And adding dimethyl sulfoxide and fluoroether into the solution to obtain the electrolyte.
Preferably, the sodium salt in the step 1) is sodium hexafluorophosphate, sodium perchlorate or sodium trifluoromethylsulfonate; the ether solvent is ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether or diethyl ether.
As a preferred alternative to this, step 2) the fluoroether is 1, 2-tetrafluoroethyl-2, 2-trifluoroethyl ether 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether or 1, 2-tetrafluoroethyl ether.
Preferably, the concentration of the solution in step 1) is 1 to 5mol/L.
Preferably, the volume ratio of the dimethyl sulfoxide to the solution in the step 2) is 0.01-5:10; the volume ratio of the fluoroether to the solution is 0.01-5:10.
The invention also provides electrolyte obtained by the preparation method.
The invention also provides a method for preparing the sodium ion battery from the electrolyte, which comprises the following steps:
(1) Mixing spherical graphite, acetylene black, carboxymethyl cellulose and water, and performing ball milling to obtain pasty slurry;
(2) Coating the pasty slurry on a copper foil, and sequentially drying and rolling to obtain an electrode slice;
(3) In an inert atmosphere, the electrolyte, the electrode sheet, the separator and the sodium sheet are assembled into a sodium ion battery.
Preferably, the weight ratio of the spherical graphite, the acetylene black and the carboxymethyl cellulose in the step (1) is 7-9:0.5-2:0.5-2; the mixing time is 8-12 min; the ball milling speed is 200-600 r/min, and the ball milling time is 4-8 h.
Preferably, the drying temperature in the step (2) is 40-80 ℃, and the drying time is 43-53 h; the roll pressure is 5-15 MPa.
Preferably, the inert atmosphere in the step (3) is an argon atmosphere.
The beneficial effects of the invention include the following points:
1) The preparation method of the electrolyte is simple, easy to operate and suitable for industrial application.
2) The electrolyte prepared by the invention is applied to the graphite anode material of the sodium ion battery, and the electrolyte still has 259 mAh.g after 60 circles of circulation -1 The reversible specific capacity of the electrolyte is improved by 93 percent compared with the electrolyte without dimethyl sulfoxide and fluoroether.
Drawings
FIG. 1 is a CV test curve of a sodium ion battery of comparative example 1;
FIG. 2 is a CV test curve of the sodium ion battery of example 1;
FIG. 3 is the rate capability of the sodium ion batteries of example 1 and comparative example 1 at the same number of cycles at different current densities;
FIG. 4 is the cycling performance of the sodium ion batteries of example 1 and comparative example 1 at a current density of 0.1A/g.
Detailed Description
The invention provides a preparation method of electrolyte, which comprises the following steps:
1) Dissolving sodium salt in an ether solvent to obtain a solution;
2) And adding dimethyl sulfoxide and fluoroether into the solution to obtain the electrolyte.
In the present invention, the sodium salt in step 1) is preferably sodium hexafluorophosphate, sodium perchlorate or sodium trifluoromethylsulfonate; the ether solvent is preferably ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether or diethyl ether.
In the present invention, the fluoroether of step 2) is preferably 1, 2-tetrafluoroethyl-2, 2-trifluoroethyl ether 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether or 1, 2-tetrafluoroethyl ether.
In the present invention, the concentration of the solution in step 1) is 1 to 5mol/L, preferably 2 to 4mol/L, more preferably 2.5 to 3.5mol/L, and still more preferably 3mol/L.
In the present invention, the volume ratio of the dimethyl sulfoxide to the solution in the step 2) is 0.01-5:10, preferably 0.5-4.5:10, more preferably 1-4:10, and even more preferably 2-3:10; the volume ratio of the fluoroether to the solution is 0.01-5:10, preferably 0.5-4.5:10, more preferably 1-4:10, and even more preferably 2-3:10.
The invention also provides electrolyte obtained by the preparation method.
The invention also provides a method for preparing the sodium ion battery from the electrolyte, which comprises the following steps:
(1) Mixing spherical graphite, acetylene black, carboxymethyl cellulose and water, and performing ball milling to obtain pasty slurry;
(2) Coating the pasty slurry on a copper foil, and sequentially drying and rolling to obtain an electrode slice;
(3) In an inert atmosphere, the electrolyte, the electrode sheet, the separator and the sodium sheet are assembled into a sodium ion battery.
In the present invention, the spheroidal graphite of step (1) is preferably untreated commercial spheroidal graphite; the water is preferably deionized water.
In the invention, the weight ratio of the spherical graphite, the acetylene black and the carboxymethyl cellulose in the step (2) is 7-9:0.5-2:0.5-2, preferably 7.2-8.8:0.7-1.8:0.7-1.8, and more preferably 7.5-8.5:1-1.5:1-1.5; the mixing time is 8-12 min, preferably 9-11 min, and more preferably 10min; the mixing mode is preferably manual slow stirring; the ball milling speed is 200-600 r/min, preferably 300-500 r/min, more preferably 350-450 r/min, and even more preferably 400r/min; the ball milling time is 4 to 8 hours, preferably 5 to 7 hours, more preferably 5.5 to 6.5 hours, and still more preferably 6 hours.
In the present invention, the drying temperature in the step (3) is 40 to 80 ℃, preferably 50 to 70 ℃, more preferably 55 to 65 ℃, and even more preferably 60 ℃; the drying time is 43 to 53 hours, preferably 45 to 51 hours, more preferably 47 to 49 hours, and still more preferably 48 hours; the roll pressure is 5 to 15MPa, preferably 7 to 13MPa, more preferably 9 to 11MPa, and even more preferably 10MPa.
In the present invention, the inert atmosphere in the step (3) is preferably an argon atmosphere.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Sodium hexafluorophosphate is fully dissolved in diethylene glycol dimethyl ether to obtain a solution with the concentration of 2 mol/L. To 10mL of the solution were added 0.2mL of dimethyl sulfoxide and 0.1mL of 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether to obtain a dual additive electrolyte.
8g of untreated commercial spheroidal graphite, 1g of acetylene black, 1g of carboxymethyl cellulose and 20g of deionized water were mixed, manually stirred slowly for 10min, then transferred to a planetary ball mill, ball-milled at a rate of 400r/min for 6h, the obtained pasty slurry was coated on copper foil, dried at 60 ℃ for 48h, then subjected to roll pressing under a pressure of 10MPa, and cut to obtain electrode sheets.
And in an argon atmosphere, assembling the electrolyte, the electrode plate, the diaphragm and the sodium plate of the dual additive into the sodium ion battery.
Example 2
Sodium perchlorate is fully dissolved in ethylene glycol dimethyl ether to obtain a solution with the concentration of 1 mol/L. To 10mL of the solution were added 0.01mL of dimethyl sulfoxide and 5mL of 1, 2-tetrafluoroethyl-2, 2-trifluoroethyl ether to obtain a dual additive electrolyte A.
7g of untreated commercial spheroidal graphite, 0.5g of acetylene black, 0.5g of carboxymethyl cellulose and 15g of deionized water were mixed, stirred for 8 minutes, then transferred to a planetary ball mill, ball-milled at a rate of 200r/min for 4 hours, the obtained paste slurry was coated on a copper foil, dried at 40 ℃ for 43 hours, then roll-pressed at a pressure of 5MPa, and cut to obtain electrode sheets.
In an argon atmosphere, the dual-additive electrolyte a, electrode sheet, separator and sodium sheet were assembled into a sodium ion battery.
Example 3
Sodium triflate is fully dissolved in diethyl ether to obtain a solution with the concentration of 5mol/L. To 10mL of the solution were added 5mL of dimethyl sulfoxide and 0.01mL of 1, 2-tetrafluoroethyl ethyl ether to obtain a dual additive electrolyte B.
9g of spheroidal graphite, 2g of acetylene black, 2g of carboxymethyl cellulose and 30g of deionized water are mixed, manually stirred at a slow speed for 12min, then transferred to a ball mill, ball-milled at a speed of 600r/min for 8h, the obtained pasty slurry is coated on copper foil, dried at 80 ℃ for 53h, then subjected to roll pressing under 15MPa pressure, and cut to obtain an electrode slice.
And in an argon atmosphere, assembling the electrolyte B, the electrode plate, the diaphragm and the sodium plate of the dual additive into a sodium ion battery.
Comparative example 1
Sodium hexafluorophosphate is fully dissolved in diethylene glycol dimethyl ether to obtain a solution with the concentration of 2mol/L, and the solution is marked as electrolyte without additives.
A sodium ion battery was prepared by replacing the dual additive electrolyte of example 1 with an equal amount of additive-free electrolyte, and the other operations and parameters were the same as in example 1.
Comparative example 2
Sodium perchlorate is fully dissolved in ethylene glycol dimethyl ether to obtain a solution with the concentration of 1mol/L, and the solution is marked as electrolyte A without additives.
A sodium ion battery was prepared by replacing the dual additive electrolyte a of example 2 with an equal amount of additive-free electrolyte a, and the other operations and parameters were the same as in example 2.
Comparative example 3
Sodium triflate was dissolved thoroughly in diethyl ether to give a 5mol/L solution labeled as additive-free electrolyte B.
A sodium ion battery was prepared by replacing the dual additive electrolyte B of example 3 with an equal amount of additive-free electrolyte B, and the other operations and parameters were the same as in example 3.
The sodium ion batteries of example 1 and comparative example 1 were subjected to a CV test, a rate performance test at different current densities, and a cycle performance test at a current density of 0.1A/g, and the results are shown in fig. 1 to 4.
From FIGS. 1 to 4, it can be seen that the electrolyte using the dual additive of example 1 can intercalate more Na at low voltage than the electrolyte using the no additive of comparative example 1 + The method comprises the steps of carrying out a first treatment on the surface of the The electrolyte of example 1 was double-additive with corresponding capacities of 233.8 mAh.g at current densities of 0.1A/g, 0.2A/g, 0.5A/g, 1A/g, 2A/g, respectively, at the same number of cycles -1 、163.9mAh·g -1 、141.9mAh·g -1 、121.4mAh·g -1 And 108.4 mAh.g -1 The method comprises the steps of carrying out a first treatment on the surface of the When the current density is recovered to 0.1A/g, the capacity can still be recovered to 180 mAh.g -1 And is stable and free from attenuation, and sufficiently exhibits high specific capacity and excellent rate performance. The electrolyte of comparative example 1, after 60 cycles at a current density of 0.1A/g, had a reversible specific capacity of 134.2 mAh.g -1 Dual additive electrolyte of example 1The inverse specific capacity is 259 mAh.g -1 After that, the capacity still tends to rise, and the reversible specific capacity is improved by 93%.
At the same cycle number, the corresponding capacities of the dual additive electrolyte A of example 2 were 235.4 mAh.g when the current densities were 0.1A/g, 0.2A/g, 0.5A/g, 1A/g, and 2A/g, respectively -1 、164.2mAh·g -1 、143.1mAh·g -1 、122.5mAh·g -1 And 108.9 mAh.g -1 The method comprises the steps of carrying out a first treatment on the surface of the When the current density is recovered to 0.1A/g, the capacity can still be recovered to 182 mAh.g -1 And is stable and free from attenuation, and sufficiently exhibits high specific capacity and excellent rate performance. The reversible specific capacity of the additive-free electrolyte A of comparative example 2 after 60 cycles at a current density of 0.1A/g was 134.7 mAh.g -1 The reversible specific capacity of the dual additive electrolyte A of example 2 was 258.9 mAh.g -1 After that, the capacity still tends to rise, and the reversible specific capacity is improved by 92.2%.
At the same cycle number, the corresponding capacities of the dual additive electrolyte B of example 3 were 226.5 mAh.g when the current densities were 0.1A/g, 0.2A/g, 0.5A/g, 1A/g, and 2A/g, respectively -1 、152.3mAh·g -1 、132.2mAh·g -1 、112.5mAh·g -1 And 95.2 mAh.g -1 The method comprises the steps of carrying out a first treatment on the surface of the When the current density is recovered to 0.1A/g, the capacity can still be recovered to 172 mAh.g -1 And is stable and free from attenuation, and sufficiently exhibits high specific capacity and excellent rate performance. The reversible specific capacity of the additive-free electrolyte B of comparative example 3 after 60 cycles at a current density of 0.1A/g was 132.1 mAh.g -1 The reversible specific capacity of the dual additive electrolyte B of example 3 was 252mAh g -1 After that, the capacity still has a trend of rising, and the reversible specific capacity is improved by 90.8%.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (7)
1. A method for preparing a sodium ion battery by using electrolyte, which is characterized by comprising the following steps:
(1) Mixing spherical graphite, acetylene black, carboxymethyl cellulose and water, and performing ball milling to obtain pasty slurry;
(2) Coating the pasty slurry on a copper foil, and sequentially drying and rolling to obtain an electrode slice;
(3) Assembling the electrolyte, the electrode plate, the diaphragm and the sodium plate into a sodium ion battery in an inert atmosphere;
the preparation method of the electrolyte comprises the following steps:
1) Dissolving sodium salt in an ether solvent to obtain a solution;
2) Dimethyl sulfoxide and fluoroether are added into the solution to obtain electrolyte;
the volume ratio of the dimethyl sulfoxide to the solution in the step 2) is 0.01-5:10; the volume ratio of the fluoroether to the solution is 0.01-5:10.
2. The method of claim 1, wherein the sodium salt of step 1) is sodium hexafluorophosphate, sodium perchlorate, or sodium trifluoromethylsulfonate; the ether solvent is ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether or diethyl ether.
3. A method according to claim 1 or 2, characterized in that, step 2) the fluoroether is 1, 2-tetrafluoroethyl-2, 2-trifluoroethyl ether 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether or 1, 2-tetrafluoroethyl ether.
4. A method according to claim 3, wherein the concentration of the solution in step 1) is 1 to 5mol/L.
5. The method of claim 1, wherein the weight ratio of the spheroidal graphite, the acetylene black and the carboxymethyl cellulose in the step (1) is 7-9:0.5-2:0.5-2; the mixing time is 8-12 min; the ball milling speed is 200-600 r/min, and the ball milling time is 4-8 h.
6. The method of claim 1, wherein the drying temperature in step (2) is 40-80 ℃ and the drying time is 43-53 h; the roll pressure is 5-15 MPa.
7. The method of claim 1, wherein the inert atmosphere of step (3) is an argon atmosphere.
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