CN116014079A - Lignin water-based composite battery binder and preparation method and application of silicon-based negative plate thereof - Google Patents
Lignin water-based composite battery binder and preparation method and application of silicon-based negative plate thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a lignin water-based composite battery binder, a preparation method and application of a silicon-based negative plate thereof. The binder of the silicon-based negative electrode plate is a three-component water-based composite binder of polyacrylic acid PAA, sulfonated lignin SL and sodium polythiooctoate PTA-Na, PAA/SL/TA-Na solution is prepared, then silicon-based active material and conductive material are added and mixed to prepare negative electrode slurry, and finally the negative electrode slurry is coated on a substrate and subjected to high-temperature polymerization, drying and thermal esterification to obtain the negative electrode plate. The covalent bond-dynamic bond in the lignin water-based composite binder can provide strong mechanical strength to inhibit the volume expansion of the silicon-based material, and can dissipate stress through reversible fracture and repair of the dynamic bond, so that the volume effect of the silicon-based negative electrode is effectively relieved, and the technical problem of poor cycle performance of the silicon-based negative electrode is solved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a lignin water-based composite battery binder, a preparation method and application of a silicon-based negative plate thereof.
Background
Lithium Ion Batteries (LIBs) have become important energy storage devices for portable devices such as cell phones, notebook computers, and cameras. Along with the continuous improvement of the requirements of people on high-power energy storage devices, the graphite carbon cathode material serving as a lithium ion battery at present can not meet the use requirements of high energy density and high power density. In the aspect of the novel lithium ion battery anode material, the theoretical specific capacity of the silicon anode material is up to 4200mAh/g, which is 11 times that of the traditional graphite anode (372 mAh/g). In addition, the silicon anode material is a potential anode material of the next generation of high-energy-density lithium ion battery because of abundant resource and low cost. Among them, silicon oxide is considered as a very promising silicon-based negative electrode material for lithium ion batteries, which has a smaller expansion and a theoretical specific capacity of 2043mAh/g as compared with silicon. However, the silicon-based negative electrode still has some problems in practical application, and the silicon-based negative electrode can have huge volume expansion in the process of lithium intercalation, so that the active material is broken and crushed, and the active component and the current collector fall off, thereby influencing the coulombic efficiency, the circulation and the rate capability of the battery.
The problems can be improved by changing the size of the silicon-based material, hybridizing the composite material, designing a new binder and the like, but designing the binder is one of the most convenient and economical methods. The binder serves to maintain a tight connection between the active material, the conductive agent and the current collector, maintaining the integrity of the electrode. The traditional binder is mainly linear polymer with rich polar groups, but the interaction sites between the binder and the silicon-based material are few, and the stress caused by the volume expansion of the silicon-based material is difficult to bear, so that the active material is cracked and crushed, the electrical contact is not good, and the SEI growth is unstable. In addition, the existing adhesive mostly uses solvents with strong polarity, such as N-methyl pyrrolidone, N-dimethyl amide, dimethyl sulfoxide and the like, the solvents with strong polarity have high toxicity, and meanwhile, the preparation of the crosslinked network adhesive is complex and is not beneficial to large-scale application. However, the water-based adhesive has the problems of insufficient mechanical strength, poor adhesion and poor effect of inhibiting the expansion of the silicon-based material, and cannot meet the requirements of the lithium ion battery with high energy density, high capacity and long service life. Therefore, it is necessary to develop a water-based adhesive with high mechanical strength, strong adhesiveness and good expansion inhibiting effect on silicon-based materials, so as to realize that the lithium ion battery using the silicon-based negative electrode sheet has excellent cycling stability.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a lignin water-based battery binder; the invention further aims to provide a silicon-based negative electrode plate based on the lignin water-based battery binder; the invention further aims to provide application of the silicon-based negative plate in a lithium ion battery.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
the invention provides a silicon-based negative electrode plate based on a lignin water-based battery binder, which is characterized by comprising a silicon-based active material, a lignin water-based battery binder and a conductive agent, wherein the lignin water-based battery binder comprises polyacrylic acid, sulfonated lignin and sodium polythiooctoate.
The invention also provides a preparation method of the silicon-based negative electrode plate based on the lignin water-based battery binder, which is characterized by comprising the following steps: and dissolving polyacrylic acid, sulfonated lignin, sodium lipoic acid, a silicon-based active material and a conductive material in water, uniformly mixing to obtain negative electrode slurry, scraping the negative electrode slurry on a substrate, and finally drying and thermally esterifying at high temperature to obtain the negative electrode plate.
Preferably, the mass ratio of the polyacrylic acid, the sulfonated lignin and the sodium lipoic acid is (1-100): 1:1.
Preferably, the water is used in an amount of 30mL/g based on the amount of the raw materials of the lignin-based electrode binder composed of polyacrylic acid, sulfonated lignin and sodium lipoic acid.
Preferably, the preparation method of the polyacrylic acid comprises the following steps: and (3) dissolving acrylic acid in water, adding an ammonium persulfate initiator, continuously stirring at 60 ℃ for 12 hours, washing the obtained polymer for 2-3 times after the reaction is finished, removing unreacted monomers and the initiator, and drying the obtained polyacrylic acid at 50 ℃ to remove water.
Preferably, polyacrylic acid, sulfonated lignin and sodium lipoic acid are used for forming raw materials of the lignin-based battery binder, the active material, the conductive material and the raw materials of the lignin-based battery binder are mixed according to the mass ratio of (6-7): (1-2), the silicon-based active material is at least one of silicon, silicon oxide and silicon-carbon composite material, and the conductive material is conductive carbon black.
Preferably, the mixing is carried out with stirring at 30-1000 rpm for 1-10 hours.
Preferably, the negative electrode slurry is used at a concentration of 1.0-2.5 mg/cm 2 The active material surface loading of (2) is knife coated on a substrate, wherein the substrate is a copper foil substrate.
Preferably, the high temperature drying is thermal esterified to vacuum drying at 150-200 ℃.
The invention also provides application of the silicon-based negative electrode substrate based on the lignin water-based battery binder to preparation of a lithium ion battery.
The lignin water-based battery binder can also be applied to preparing positive plates or negative plates of other batteries.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a preparation method of a silicon-based negative electrode plate based on lignin water-based battery binder, which comprises the steps of dissolving polyacrylic acid, sulfonated lignin, sodium lipoic acid, a silicon-based active material and a conductive material in water, uniformly mixing to obtain negative electrode slurry, then scraping the negative electrode slurry on a substrate, and finally drying and thermally esterifying at high temperature to obtain the negative electrode plate. The invention utilizes polyhydroxy of lignin and carboxyl of polyacrylic acid to form covalent ester bond, thus obtaining rigid three-dimensional structure, and then introduces dynamic disulfide bond of flexible sodium polythiooctoate, and hydrogen bond formed between carboxyl and lignin hydroxyl to form double dynamic bond; the covalent bond-dynamic bond combination can provide strong mechanical strength to inhibit the volume expansion of the silicon-based material when the silicon-based material is in volume expansion, and simultaneously, stress dissipation is carried out through fracture and repair of the dynamic bond. The peel strength of the silicon-based negative electrode plate based on the lignin water-based adhesive reaches 4.9N, has strong adhesion, effectively inhibits the volume effect of the silicon-based negative electrode plate during charge and discharge, and improves the cycle performance of the silicon-based negative electrode plate.
Drawings
FIG. 1 is a graph of peel strength analysis of a silicon-based negative plate;
FIG. 2 is a graph of cycling performance of a silicon oxide negative half cell at a current density of 0.2A/g.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, were conventional, and the experimental materials used in the following examples, unless otherwise specified, were commercially available from conventional sources.
Example 1 preparation of a silicon-based negative electrode sheet based on PAA/SL/TA-Na-150 Binder
1. Preparation of polyacrylic acid (PAA): weighing 10ml of Acrylic Acid (AA), putting the Acrylic Acid (AA) into a reaction bottle filled with 100ml of water, adding 0.01g of ammonium persulfate initiator, continuously stirring for 12 hours at 60 ℃, washing the obtained polymer with absolute ethyl alcohol for 3 times after the reaction is finished, removing unreacted monomers and initiator, drying the obtained polyacrylic acid at 50 ℃ by using a forced air drying box to remove water, and drying for later use;
2. preparation of sodium lipoic acid (TA-Na): measuring 5g of lipoic acid, adding the lipoic acid into a sodium hydroxide-absolute ethyl alcohol solution (the molar ratio of the lipoic acid to the sodium hydroxide is 1:1.2), reacting to generate precipitate, washing the precipitate with absolute ethyl alcohol for multiple times, and drying to obtain sodium lipoic acid;
3. preparing a silicon-based negative plate: the polyacrylic acid, sulfonated lignin and sodium lipoic acid obtained are mixed according to the following ratio of 1:1:1, 0.02g of deionized water which is mixed with 600 mu L of deionized water to prepare PAA/SL/TA-Na solution, 0.14g of silicon oxide and 0.04g of conductive carbon black which are ball-milled to obtain particle size of 500nm are added, and then the mixture is stirred for 10 hours at a speed of 800rpm to carry out slurry mixing, and the slurry after the uniform mixing is 1.5mg/cm 2 The active material load of the polymer is flatly coated on a copper foil, and the copper foil is dried for 10 hours at a high temperature of 150 ℃ to cause each component to generate thermal esterification, so as to prepare a pole piece, and the sodium lipoic acid is polymerized to form the sodium polythiooctoate in the thermal esterification process. And cutting the dried pole piece into a wafer with the diameter of 14mm to serve as a negative pole piece of the button cell for standby.
Comparative example 1 preparation of a silicon-based negative electrode sheet based on PAA/SL/TA-Na-60 Binder
The preparation method of PAA and TA-Na is the same as that of example 1, and the preparation of the silicon-based negative electrode plate is as follows: the polyacrylic acid, sulfonated lignin and sodium lipoic acid obtained are mixed according to the following ratio of 1:1:1, 0.02g of PAA/SL/TA-Na solution is prepared by mixing the materials into 600 mu L of deionized water, 0.14g of silicon oxide and 0.04g of conductive carbon black are added after ball milling, and then the mixture is stirred for 10 hours at the speed of 800rpm for slurry mixing, and the slurry after uniform mixing is 1.5mg/cm 2 The active material load of the polymer is flatly coated on copper foil, and the polymer is dried for 10 hours at 60 ℃ to obtain the pole piece. And cutting the dried pole piece into a wafer with the diameter of 14mm to serve as a negative pole piece of the button cell for standby.
Comparative example 2 preparation of a PAA/SL-150 Binder-based silicon-based negative electrode sheet
The PAA preparation method is the same as in example 1, preparation of silicon-based negative electrode sheet: the polyacrylic acid and sulfonated lignin obtained are prepared according to the following steps of 1:1, 0.02g of deionized water is weighed and mixed into 600 mu L of deionized water to prepare PAA/SL solution, 0.14g of silicon oxide and 0.04g of conductive carbon black are added after ball milling, and then the mixture is stirred for 10 hours at the speed of 800rpm to carry out slurry mixing, and the slurry after uniform mixing is 1.5mg/cm 2 The active material load of the polymer is flatly coated on copper foil, and the polymer is dried at a high temperature of 150 ℃ for 10 hours for thermal esterification to obtain the pole piece. And cutting the dried pole piece into a wafer with the diameter of 14mm to serve as a negative pole piece of the button cell for standby.
Comparative example 3 preparation of a PAA/SL-60 Binder-based silicon-based negative electrode sheet
The PAA preparation method is the same as in example 1, preparation of silicon-based negative electrode sheet: the polyacrylic acid and sulfonated lignin obtained are prepared according to the following steps of 1:1, 0.02g of deionized water is weighed and mixed into 600 mu L of deionized water to prepare PAA/SL solution, 0.14g of silicon oxide and 0.04g of conductive carbon black are added after ball milling, and then the mixture is stirred for 10 hours at the speed of 800rpm to carry out slurry mixing, and the slurry after uniform mixing is 1.5mg/cm 2 The active material load of the polymer is flatly coated on copper foil, and the polymer is dried for 10 hours at 60 ℃ to obtain the pole piece. And cutting the dried pole piece into a wafer with the diameter of 14mm to serve as a negative pole piece of the button cell for standby.
Comparative example 4 preparation of PAA Binder-based silicon-based negative electrode sheet
The PAA preparation method is the same as in example 1, preparation of silicon-based negative electrode sheet: weighing 0.02g of the obtained polyacrylic acid, mixing with 600 mu L of deionized water to prepare PAA solution, adding 0.14g of ball-milled silicon oxide and 0.04g of conductive carbon black, stirring at 800rpm for 10h to mix slurry, and mixing the slurry at a concentration of 1.5mg/cm 2 The active material load of the polymer is flatly coated on copper foil, and the polymer is dried for 10 hours at 60 ℃ to obtain the pole piece. And cutting the dried pole piece into a wafer with the diameter of 14mm to serve as a negative pole piece of the button cell for standby.
Example 1 characterization of Performance of silicon-based negative electrode sheet and half cell thereof
1. Adhesion test
The silicon-based negative electrode sheets of example 1 and comparative examples 1 and 4 were fixed to a peel force tester, respectively, and then 180-degree peel test was performed at a speed of 10 mm/min. The peel test results are shown in fig. 1, and the average peel strength of the adhesive in the example 1 reaches 4.9N, which is higher than 3.5N in the comparative example 4 and 2.5N in the comparative example 1, which indicates that the esterification degree of polyacrylic acid and sulfonated lignin is obviously improved after the adhesive in the example 1 is subjected to high-temperature esterification, the adhesion of a network is enhanced, the integrity of an electrode in a battery cycle can be maintained, and an active material, a conductive material and a copper foil current collector are tightly connected together. While comparative example 1 was not completely esterified, the degree of esterification was low, and the adhesiveness was weak; comparative example 4 has only one-component PAA as adhesive, and the adhesion effect is inferior to example 1.
2. Cyclic performance characterization of silicon-based negative plate half-cell at current density of 0.2A/g
And (3) assembling a half cell: and respectively assembling the silicon-based negative plates with the diameters of 14mm into a lithium ion half battery in a glove box filled with argon and having the water oxygen content of less than 0.1 ppm. The electrolyte system was selected from EC/DEC (v/v=1:1) solutions containing 10wt% FEC and 1wt% VC, and the separator was a commercial polypropylene porous membrane.
The cycle performance characterization of each half cell under the current density of 0.2A/g is shown in figure 2, after the half cell is cycled for 100 circles, the half cell of the embodiment 1 still keeps the discharge specific capacity of 1192mAh/g, and compared with the cycle performance of the comparative example 2, the half cell has better cycle performance, which shows that the addition of the sodium lipoic acid can realize the fracture and repair of dynamic bonds to perform stress dissipation, and the inhibition effect on the expansion of the silicon-based material is enhanced. The cycle performance of example 1 and comparative example 2 is better than that of comparative example 4, which shows that the polyhydroxy three-dimensional structure of lignin per se and carboxyl of polyacrylic acid are esterified and crosslinked to obtain a rigid three-dimensional structure, and the rigid three-dimensional structure can provide strong mechanical strength to inhibit the volume expansion of silicon-based materials when the volume expansion of the materials is carried out. While comparative examples 1 and 3 were poor in cycle performance because of the low degree of esterification, expansion could not be suppressed.
The two tests show that the PAA/SL/TA-Na water-based polymer binder forms a covalent bond-dynamic bond bonding network through high-temperature esterification, can provide strong mechanical strength to inhibit the volume expansion of the silicon-based material, and can simultaneously perform stress dissipation through the fracture and repair of the dynamic bond. The volume effect of the electrode circulation process can be effectively inhibited by applying the adhesive to the silicon-based negative electrode of the lithium ion battery, and the circulation performance of the battery is obviously improved.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (10)
1. The silicon-based negative electrode plate based on the lignin water-based battery binder is characterized by comprising a silicon-based active material, the lignin water-based battery binder and a conductive agent, wherein the lignin water-based battery binder comprises polyacrylic acid, sulfonated lignin and sodium polythiooctoate.
2. The method for preparing the silicon-based negative electrode sheet based on the lignin water-based battery binder, which is disclosed in claim 1, is characterized by comprising the following steps: and dissolving polyacrylic acid, sulfonated lignin, sodium lipoic acid, a silicon-based active material and a conductive material in water, uniformly mixing to obtain negative electrode slurry, scraping the negative electrode slurry on a substrate, and finally drying and thermally esterifying at high temperature to obtain the negative electrode plate.
3. The preparation method of the silicon-based negative electrode sheet based on the lignin water-based battery binder, which is disclosed in claim 2, is characterized in that the mass ratio of polyacrylic acid, sulfonated lignin and sodium lipoic acid is (1-100): 1:1.
4. The method for preparing the silicon-based negative electrode sheet based on the lignin water-based battery binder according to claim 2, wherein the method for preparing the polyacrylic acid is as follows: and (3) dissolving acrylic acid in water, adding an ammonium persulfate initiator, continuously stirring at 60 ℃ for 12 hours, washing the obtained polymer for 2-3 times after the reaction is finished, removing unreacted monomers and the initiator, and drying the obtained polyacrylic acid at 50 ℃ to remove water.
5. The preparation method of the silicon-based negative plate based on the lignin water-based battery binder, which is disclosed in claim 2, is characterized in that polyacrylic acid, sulfonated lignin and sodium lipoic acid are used for forming raw materials of the lignin water-based battery binder, the active material, the conductive material and the raw materials of the lignin water-based battery binder are mixed according to the mass ratio of (6-7): (1-2), the silicon-based active material is at least one of silicon, silicon oxide and silicon carbon composite material, and the conductive material is conductive carbon black.
6. The method for preparing a silicon-based negative electrode sheet based on a lignin water-based battery binder according to claim 2, wherein the mixing is carried out for 1-10 hours with 30-1000 rpm.
7. The method for preparing a silicon-based negative electrode sheet based on lignin water-based battery binder according to claim 2, wherein the negative electrode slurry is 1.0-2.5 mg/cm 2 The active material surface loading of (2) is knife coated on a substrate, wherein the substrate is a copper foil substrate.
8. The method for preparing a silicon-based negative electrode sheet based on a lignin water-based battery binder according to claim 2, wherein the high-temperature drying and thermal esterification is vacuum drying at 150-200 ℃.
9. The application of the silicon-based negative electrode substrate based on the lignin-based aqueous battery binder in the preparation of a lithium ion battery.
10. The lignin-based battery binder of claim 1 for use in preparing a battery.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116804138A (en) * | 2023-08-18 | 2023-09-26 | 广东工业大学 | Polyacrylic acid and sodium lignin sulfonate composite binder for silicon-based negative electrode of lithium ion battery, and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116804138A (en) * | 2023-08-18 | 2023-09-26 | 广东工业大学 | Polyacrylic acid and sodium lignin sulfonate composite binder for silicon-based negative electrode of lithium ion battery, and preparation method and application thereof |
| CN116804138B (en) * | 2023-08-18 | 2023-12-08 | 广东工业大学 | Polyacrylic acid and sodium lignin sulfonate composite binder for silicon-based negative electrode of lithium ion battery, and preparation method and application thereof |
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