CN108417818B - Lithium ion battery cathode based on silicon-based material - Google Patents
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Abstract
The invention discloses a silicon-based material-based lithium ion battery cathode, which takes silicon carbide or silicon monoxide as cathode slurry of an active substance, adopts a novel water-based block polymer and takes acrylic acid/styrene/methyl acrylate/styrene block copolymer as a binder, the binder has extremely high adhesion with silicon particles and extremely high elasticity, is beneficial to relieving particle pulverization failure caused by huge volume change of the silicon-based particles in the lithium removal/insertion process, and can improve the liquid absorption rate of an electrolyte, accelerate the lithium ion conduction rate and greatly improve the performance of the silicon-based lithium ion battery cathode.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a silicon-based material-based lithium ion battery cathode.
Background
Lithium batteries are widely used in the fields of electric vehicles, portable electronic products and the like at the present stage because of the advantages of high specific capacity, long cycle life, small self-discharge and the like. However, at present, the problems of short driving mileage, overlong charging time, insufficient battery endurance, excessively fast capacity attenuation and the like of portable electronic products still exist in single charging of electric automobiles, and the specific capacity, specific power density, cycle life and the like of lithium batteries are urgently needed to be further improved.
The electrode of the lithium ion battery mainly comprises an active substance, a conductive agent and a binder. Because the maximum specific capacity of the silicon carbide electrode is as high as 2500mAhg-1The maximum theoretical specific capacity of the silicon monoxide electrode is as high as 1800mAhg-1It is 3 times or more than that of graphite materials which are already in commercial use, and therefore, is considered to be the most potential active material of the next generation lithium ion battery. However, the volume deformation of the silicon-based electrode in the charge-discharge cycle process causes the capacity of the silicon-based electrode to be rapidly attenuated, and the cycle performance of the silicon-based electrode is far less than the normal use standard.
Polyvinylidene fluoride (PVDF) is a binder mainly used in the positive and negative electrodes of lithium batteries for a long time, has good electrochemical, chemical and thermal stability and high mechanical strength, meets the basic requirements of serving as an electrode binder and is widely used. However, recent studies have found that PVDF has poor viscoelasticity and thus is used in a large amount (close to 10%) in an electrode, and PVDF itself has poor electron and ion conductivity, thus increasing the electron and ion conduction resistance in the electrode. In addition, the poor cohesiveness and elasticity of the electrolyte easily cause the separation of the active material from the conductive agent in the process of volume change during charging and discharging, so that the battery capacity is attenuated too fast. In addition, the dissolution of PVDF requires the use of relatively toxic and relatively expensive methyl pyrrolidone (NMP) as a solvent. In addition, the slow drying process of the NMP easily causes the enrichment of PVDF on the surface of the electrode, which leads to the increase of the interface resistance.
Disclosure of Invention
The invention provides a lithium ion battery cathode based on a silicon-based material, aiming at the technical problems that the specific capacity is low when graphite is used as a lithium ion battery cathode active material and the graphite cannot be used as an electric appliance with high performance requirements in the prior art.
The specific technical scheme of the invention is as follows:
the silicon-based material-based lithium ion battery negative electrode is characterized in that the lithium ion battery negative electrode is prepared by coating negative electrode slurry on copper foil, the thickness of the negative electrode slurry is 50-300 microns, and the formula of the negative electrode slurry is as follows: 60.0 to 96.0 weight portions of silicon carbide or silicon monoxide, 1.0 to 20.0 weight portions of conductive agent, 1.0 to 7.5 weight portions of binder, 1.0 to 7.5 weight portions of thickening agent and 30.0 to 400.0 weight portions of dispersion medium;
the binder is an acrylic/styrene/methyl acrylate/styrene block copolymer.
Furthermore, the specific capacity of the silicon carbide is 420-2500mAh/g, and the specific capacity of the silicon monoxide is 460-1800 mAh/g.
Further, the structural expression of the block copolymer is R-AAn1-b-Stn2-b-MAn3-b-Stn4(ii) a Wherein R is an isopropanoyl group, an acetoxy group, a 2-nitriloacetic acid group or a 2-aminoacetoxy group; AAn1Wherein AA is a methacrylic acid monomer unit or an acrylic acid monomer unit, n1 is the average polymerization degree of AA, and n1 is 10-40; stn2Wherein St is a styrene monomer unit, n2 is the average polymerization degree of St, and n2 is 15 to 8000; MA (MA)n3Wherein MA is a methyl acrylate unit, n3 is the average polymerization degree of MA, and n3 is 50-8000; stn4Wherein St is a styrene monomer unit, n4 is the average polymerization degree of St, and n4 is 15 to 8000.
Further, the thickening agent is sodium carboxymethyl cellulose or polyacrylic acid.
Further, the dispersion medium is deionized water or distilled water or pure water.
Further, the conductive agent is conductive graphite, conductive carbon black, ketjen black, graphene, carbon nanotubes or SP-Li.
The invention has the following beneficial effects:
the invention adopts the acrylic acid/styrene/methyl acrylate/styrene block copolymer as the adhesive of the silicon carbide or silicon monoxide electrode, and the styrene hard segment in the copolymer block can be used as the physical crosslinking point of the polymer, thereby being capable of keeping the stability of the polymer network structure. The polymethyl acrylate soft segment can provide enough elasticity, can greatly relieve the huge volume change of the silicon-based particles in the charge-discharge cycle process, and finally improves the battery performance together.
Drawings
FIG. 1 is a test chart of the energy density of the negative electrode of the silicon carbide lithium ion battery obtained in example 1;
FIG. 2 is a test chart of energy density of a negative electrode of a silicon carbide lithium ion battery obtained in a comparative example;
FIG. 3 is a graph showing the power density of the negative electrode of the SiO lithium-ion battery obtained in example 2.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and preferred embodiments, and the objects and effects of the present invention will become more apparent, and the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The preparation of the acrylic acid/styrene/methyl acrylate/styrene block copolymers of the examples described below is described in patent 201610671015X.
The lithium ion battery cathode slurry is prepared by the following processing technology: adding water into a thickening agent, magnetically stirring for 30-120 minutes, and putting a conductive agent and silicon carbide or silicon oxide particles into a planetary high-energy ball mill for dry milling for 30-120 minutes; secondly, transferring the material obtained in the step one to a rotation revolution stirrer, adding all the adhesives with the weight according to the formula and the dispersion medium with the weight of 1/4-1/2 into the stirrer, stirring at a high speed for 5-30 minutes, and removing bubbles for 2-10 minutes after stirring; and thirdly, adding the residual 3/4-1/2 formula weight of dispersion medium into the material prepared in the step two, stirring at a high speed for 5-30 minutes, and removing bubbles for 1-5 minutes after stirring to obtain the lithium ion battery cathode slurry. The magnetic stirring speed is 20-100r/min, the ball milling speed is 200-.
Example 1
And coating the lithium ion battery negative electrode slurry on copper foil to prepare the lithium ion battery negative electrode, wherein the thickness is 50 microns. The slurry comprises the following raw materials in parts by weight: 60 parts of silicon carbide, 20 parts of conductive agent, 7.5 parts of binder, 7.5 parts of thickening agent and 30 parts of dispersion medium, wherein the specific capacity of the silicon carbide is 2500 mAh/g; the conductive agent is conductive graphite KS 6; the thickening agent is sodium carboxymethyl cellulose; the adhesive is acrylic acid/styrene/methyl acrylate/styrene block copolymer with the structure of R-AA10-b-St15-b-MA8000-b-St15(ii) a The dispersion medium is deionized water.
The lithium ion battery cathode slurry is prepared by the following processing technology: adding water into a thickening agent, magnetically stirring for 120 minutes, and putting a conductive agent and silicon carbide particles into a planetary high-energy ball mill for dry milling for 120 minutes; secondly, transferring the material obtained in the first step to a rotation revolution stirrer, adding all the adhesives with the weight according to the formula and the dispersion medium with the weight according to the formula of 1/2 into the stirrer, stirring at a high speed for 30 minutes, and removing bubbles for 5 minutes after stirring; and thirdly, adding the dispersion medium with the residual 1/2 formula weight into the material prepared in the second step, stirring at a high speed for 20 minutes, and removing bubbles for 3 minutes after stirring to obtain the lithium ion battery cathode slurry. The magnetic stirring speed is 100r/min, the ball milling speed is 500r/min, the high-speed stirring speed is 2500r/min, and the defoaming speed is 1000 r/min.
The high-energy density type lithium ion battery cathode is prepared by the formula, a 2032 type button half-cell is prepared by adopting a metal lithium sheet as a counter electrode and the obtained lithium ion battery cathode, and the high-energy type cathode has an energy density of 650mAh/g after 100 cycles of charge and discharge at 0.1C, and is shown in figure 1.
Comparative example 1
The binder in example 1 is replaced by commercial binder styrene-butadiene latex from acrylic acid/styrene/methyl acrylate/styrene block copolymer, and other components and proportions are unchanged, so as to prepare the negative electrode of the commercial lithium ion battery, and design comparative example 1.
And coating the lithium ion battery negative electrode slurry on copper foil to prepare the lithium ion battery negative electrode, wherein the thickness is 50 microns. The slurry comprises the following raw materials in parts by weight: 60 parts of silicon carbide, 20 parts of conductive agent, 7.5 parts of binder, 7.5 parts of thickening agent and 30 parts of dispersion medium. The specific capacity of the silicon carbide is 2500 mAh/g; the conductive agent is conductive graphite KS 6; the thickening agent is sodium carboxymethyl cellulose; the binder is commercial binder styrene-butadiene latex; the dispersion medium is deionized water.
The lithium ion battery cathode slurry is prepared by the following processing technology: adding water into a thickening agent, magnetically stirring for 60 minutes, and putting a conductive agent and silicon carbide particles into a planetary high-energy ball mill for dry milling for 60 minutes; secondly, transferring the material obtained in the first step to a rotation revolution stirrer, adding all the adhesives with the weight according to the formula and the dispersion medium with the weight according to the formula of 1/2 into the stirrer, stirring for 15 minutes at a high speed, and removing bubbles for 2 minutes after stirring; and thirdly, adding the dispersion medium with the residual 1/2 formula weight into the material prepared in the second step, stirring at a high speed for 10 minutes, and removing bubbles for 1 minute after stirring to obtain the lithium ion battery cathode slurry. The magnetic stirring speed is 50r/min, the ball milling speed is 350r/min, the high-speed stirring speed is 1500r/min, and the defoaming speed is 500 r/min.
The commercial lithium ion battery cathode is prepared according to the formula, a 2032 type button half-cell is prepared by adopting a metal lithium sheet as a counter electrode and the obtained lithium ion battery cathode, and the energy density of 420mAh/g is obtained after 100 cycles of charge and discharge at the multiplying power of 0.1C, as shown in figure 2.
Example 2
And coating the lithium ion battery negative electrode slurry on copper foil to prepare the lithium ion battery negative electrode, wherein the thickness is 300 microns. The slurry comprises the following raw materials in parts by weight: 96 parts of silicon monoxide, 1 part of conductive agent, 7.5 parts of binder, 1 part of thickening agent and 400 parts of dispersion medium. The theoretical specific capacity of the silicon monoxide is 1800 mAh/g; the conductive agent is conductive graphite SFG 6; the thickener is polyacrylic acid; the adhesive is acrylic acid/styrene/methyl acrylate/styrene block copolymer with the structure of R-AA40-b-St8000-b-MA15-b-St800(ii) a The dispersion medium is distilled water.
The lithium ion battery cathode slurry is prepared by the following processing technology: adding water into a thickening agent, magnetically stirring for 120 minutes, and putting a conductive agent and silicon monoxide into a planetary high-energy ball mill for dry milling for 120 minutes; secondly, transferring the material obtained in the first step to a rotation revolution stirrer, adding all the adhesives with the weight according to the formula and the dispersion medium with the weight according to the formula of 1/2 into the stirrer, stirring at a high speed for 30 minutes, and removing bubbles for 5 minutes after stirring; and thirdly, adding the dispersion medium with the residual 1/2 formula weight into the material prepared in the second step, stirring at a high speed for 20 minutes, and removing bubbles for 3 minutes after stirring to obtain the lithium ion battery cathode slurry. The magnetic stirring speed is 100r/min, the ball milling speed is 500r/min, the high-speed stirring speed is 2500r/min, and the defoaming speed is 1000 r/min.
The high-power-density lithium ion battery cathode is prepared by the formula, a 2032 type button half-cell is prepared by adopting a metal lithium sheet as a counter electrode and the obtained lithium ion battery cathode, and the obtained power cathode has the energy density of 800mAh/g under the multiplying power of 2C, which is shown in figure 3.
Example 3
And coating the lithium ion battery negative electrode slurry on copper foil to prepare the lithium ion battery negative electrode, wherein the thickness is 200 microns. The slurry comprises the following raw materials in parts by weight: 75 parts by weight of silicon monoxide, 10 parts by weight of conductive agent, 1 part by weight of binder, 5 parts by weight of thickening agent and 200 parts by weight of dispersion medium. The theoretical specific capacity of the silicon monoxide is 460 mAh/g; the conductive agent is Keqin black EC-300J; the thickener is polyacrylic acid; the adhesive is acrylic acid/styrene/methyl acrylate/styrene block copolymer with the structure of R-AA30-b-St15-b-MA500-b-St500(ii) a The dispersion medium is pure water.
The lithium ion battery cathode slurry is prepared by the following processing technology: adding water into a thickening agent, magnetically stirring for 120 minutes, and putting a conductive agent and silicon monoxide into a planetary high-energy ball mill for dry milling for 120 minutes; secondly, transferring the material obtained in the first step to a rotation revolution stirrer, adding all the adhesives with the weight according to the formula and the dispersion medium with the weight according to the formula of 1/2 into the stirrer, stirring at a high speed for 30 minutes, and removing bubbles for 5 minutes after stirring; and thirdly, adding the dispersion medium with the residual 1/2 formula weight into the material prepared in the second step, stirring at a high speed for 20 minutes, and removing bubbles for 3 minutes after stirring to obtain the lithium ion battery cathode slurry. The magnetic stirring speed is 100r/min, the ball milling speed is 500r/min, the high-speed stirring speed is 2500r/min, and the defoaming speed is 1000 r/min.
The high-power-density lithium ion battery cathode is prepared by the formula, a 2032 type button half-cell is prepared by adopting a metal lithium sheet as a counter electrode and the obtained lithium ion battery cathode, and the obtained power cathode has the energy density of 440mAh/g after 100 cycles of charging and discharging under the multiplying power of 0.1C.
Example 4
And coating the lithium ion battery negative electrode slurry on copper foil to prepare the lithium ion battery negative electrode, wherein the thickness is 100 microns. The slurry comprises the following raw materials in parts by weight: 95 parts of silicon carbide, 20 parts of conductive agent, 7.5 parts of binder, 7.5 parts of thickening agent and 400 parts of dispersion medium. The specific capacity of the silicon monoxide is 420 mAh/g; the conductive agent is SP-Li; thickeningThe agent is polyacrylic acid; the adhesive is acrylic acid/styrene/methyl acrylate/styrene block copolymer with the structure of R-AA20-b-St500-b-MA230-b-St1500(ii) a The dispersion medium is pure water.
The lithium ion battery cathode slurry is prepared by the following processing technology: adding water into a thickening agent, magnetically stirring for 120 minutes, and putting a conductive agent and silicon carbide into a planetary high-energy ball mill for dry milling for 120 minutes; secondly, transferring the material obtained in the first step to a rotation revolution stirrer, adding all the adhesives with the weight according to the formula and the dispersion medium with the weight according to the formula of 1/2 into the stirrer, stirring at a high speed for 30 minutes, and removing bubbles for 5 minutes after stirring; and thirdly, adding the dispersion medium with the residual 1/2 formula weight into the material prepared in the second step, stirring at a high speed for 20 minutes, and removing bubbles for 3 minutes after stirring to obtain the lithium ion battery cathode slurry. The magnetic stirring speed is 100r/min, the ball milling speed is 500r/min, the high-speed stirring speed is 2500r/min, and the defoaming speed is 1000 r/min.
The high-energy-density lithium ion battery cathode is prepared by the formula, a 2032 type button half-cell is prepared by using a metal lithium sheet as a counter electrode and the obtained lithium ion battery cathode, and the obtained power cathode has an energy density of 400mAh/g after being charged and discharged for 100 cycles at a multiplying power of 0.1C.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the invention and is not intended to limit the invention, which has been described in detail with reference to the foregoing examples, but it will be apparent to those skilled in the art that various changes in the form and details of the embodiments may be made and equivalents may be substituted for elements thereof. All modifications, equivalents and the like which come within the spirit and principle of the invention are intended to be included within the scope of the invention.
Claims (6)
1. The silicon-based material-based lithium ion battery negative electrode is characterized in that the lithium ion battery negative electrode is prepared by coating negative electrode slurry on copper foil, the thickness of the negative electrode slurry is 50-300 microns, and the formula of the negative electrode slurry is as follows: 60.0 to 96.0 weight portions of silicon carbide or silicon monoxide, 1.0 to 20.0 weight portions of conductive agent, 1.0 to 7.5 weight portions of binder, 1.0 to 7.5 weight portions of thickening agent and 30.0 to 400.0 weight portions of dispersion medium;
the adhesive is acrylic acid/styrene/methyl acrylate/styrene block copolymer, and the structural expression of the adhesive is R-AAn1-b-Stn2-b-MAn3-b-Stn4(ii) a Wherein R is an isopropanoyl group, an acetoxy group, a 2-nitriloacetic acid group or a 2-aminoacetoxy group; AAn1Wherein AA is a methacrylic acid monomer unit or an acrylic acid monomer unit, n1 is the average degree of polymerization of AA, n1= 10-40; stn2Wherein St is a styrene monomer unit, n2 is the average degree of polymerization of St, n2= 15-8000; MA (MA)n3Wherein MA is a methyl acrylate unit, n3 is the average degree of polymerization of MA, n3= 50-8000; stn4Wherein St is a styrene monomer unit, n4 is an average polymerization degree of St, and n4= 15-8000.
2. The silicon-based material-based lithium ion battery negative electrode as defined in claim 1, wherein the specific capacity of the silicon carbide is 420-2500mAh/g, and the specific capacity of the silicon monoxide is 460-1800 mAh/g.
3. The silicon-based material-based lithium ion battery negative electrode of claim 1 or 2, wherein the thickener is sodium carboxymethylcellulose or polyacrylic acid.
4. The silicon-based material-based lithium ion battery negative electrode according to claim 1 or 2, wherein the dispersion medium is pure water.
5. The silicon-based material-based lithium ion battery negative electrode according to claim 4, wherein the dispersion medium is deionized water or distilled water.
6. The silicon-based material-based lithium ion battery negative electrode according to claim 1 or 2, wherein the conductive agent is conductive graphite, conductive carbon black, ketjen black, graphene, carbon nanotubes, or SP-Li.
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| CN112531171A (en) * | 2020-12-02 | 2021-03-19 | 萝北瑞喆烯碳新材料有限公司 | Graphene-coated silicon carbide negative electrode material and preparation method thereof |
| CN112625197A (en) * | 2020-12-02 | 2021-04-09 | 惠州亿纬锂能股份有限公司 | Multi-block binder and preparation method and application thereof |
| CN112920354B (en) * | 2021-01-28 | 2022-10-28 | 远景动力技术(江苏)有限公司 | Block polymers and lithiation and methods of making and using the same |
| CN112786888B (en) * | 2021-01-28 | 2022-06-21 | 远景动力技术(江苏)有限公司 | Binder, negative electrode slurry, negative electrode and lithium ion battery |
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