CN111048749B - Negative pole piece, lithium ion battery and manufacturing method thereof - Google Patents
Negative pole piece, lithium ion battery and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a negative pole piece, a lithium ion battery and a manufacturing method thereof.A modified artificial graphite is selected as a negative active material, the artificial graphite is doped with one or more of Cu, Ni and Ag, the surface of the artificial graphite is coated with amorphous carbon pyrolyzed by phenolic resin, and the surface of the artificial graphite is also subjected to heat treatment, so that the large-current discharge capacity of the negative active material, the negative pole piece coated with the negative active material and the lithium ion battery taking the negative pole piece as the negative pole are effectively improved.
Description
Technical Field
The invention relates to the technical field of lithium ion secondary batteries, in particular to a negative pole piece, a lithium ion battery and a manufacturing method thereof.
Background
The lithium ion battery is used as a green and environment-friendly new energy source, has the advantages of good reliability, high safety, small volume, light weight and the like, and is widely applied to the fields of digital products, electric automobiles, military products and the like at present. With the strong support of the country on new energy, the development of the lithium ion battery is very vigorous, but the requirements on the service life, the safety and the low cost of the lithium ion battery are higher and higher, and the lithium ion battery is developed towards the direction of high service life, high safety, high multiplying power and low cost at present.
The negative electrode material is a carrier of lithium ions and electrons during the charging process of the battery and plays a role in storing and releasing energy. In the cost of the battery, the negative electrode material accounts for about 5% -15%, and is one of important raw materials of the lithium ion battery. The negative electrode material comprises a carbon material and a non-carbon negative electrode material, the carbon material comprises a graphite negative electrode and a non-graphite negative electrode, and the graphite negative electrode is widely applied in a plurality of negative electrode materials, but the graphite has the defects: such as the low potential of graphite, forms an interfacial film with the electrolyte and is susceptible to lithium precipitation; the ion migration speed is low, so the charge-discharge multiplying power is low; the graphite having a layered structure is deformed by about 10% during the insertion and extraction of lithium ions, affecting the cycle life of the battery.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a negative pole piece and a preparation method of a lithium ion battery using the negative pole piece.
The purpose of the invention is realized by adopting the following technical scheme:
a preparation method of negative electrode slurry for a lithium ion battery comprises the following steps:
1) fully mixing and grinding carbon powder and metal powder, graphitizing at the high temperature of 2900-; wherein, the metal powder is 0.01 to 0.3 weight percent, the carbon powder is complemented to 100 weight percent, and the metal powder comprises one or more of Cu, Ni and Ag;
2) mixing and crushing the product doped in the step 1) with phenolic resin, heating to 2700-; wherein the phenolic resin accounts for 4-7 wt%, and the product doped in the step 1) is the balance of 100 wt%;
3) crushing the artificial graphite, adding the crushed artificial graphite into an ethanol solution of the conductive carbon black, uniformly stirring, heating, evaporating, drying, crushing, performing high-temperature heat treatment at 1500-; wherein the weight ratio of the artificial stone toner to the conductive carbon black is 100: 0.2-3.0, preferably 100: 0.5-2.0.
Needle coke with small particle size is selected as a raw material of artificial graphite, nano metal particles are doped in carbon powder, the particle size of the metal particles is about 2-50nm, and specifically, the metal particles with D50-10 mm can be selected. Because the metal particles have small particle size, after the metal particles are doped, the metal particles enter pores inside the artificial graphite secondary particles (the conductive agent has large particle size and cannot enter the pores), so that primary particles inside the pores can directly conduct electrons through the metal particles, the conductive capacity of the graphite secondary particles is improved, and the rate capability of the negative electrode coating/negative electrode plate/battery is further improved. The surface of the artificial graphite particle is coated with a layer of amorphous carbon pyrolyzed by phenolic resin to form a shell-core structure composite material, so that the structural damage of the graphite particle due to the embedding of electrolyte solvent molecules is effectively avoided, and the cycle performance and the large-current discharge capacity of the negative electrode active material are improved; the surface of the artificial graphite forms a porous surface structure through heat treatment, so that the surface area of artificial graphite particles is increased, the migration path of lithium ions is expanded, and the large-current discharge capacity of the negative electrode active material is improved.
4) Mixing the negative electrode active material obtained in the step 3), a binder, a conductive agent and a suspending agent, wherein the negative electrode active material accounts for 95.5 wt% of the negative electrode slurry, the binder accounts for 1.5 wt% of the negative electrode slurry, the conductive agent accounts for 1.8 wt% of the negative electrode slurry, and the suspending agent accounts for 1.2 wt% of the negative electrode slurry;
5) adding a solvent into the mixture obtained in the step 4), and stirring to prepare negative electrode slurry with the solid content of 40-52%.
Further, in step 4), the binder is an acrylic binder, and the conductive agent includes carbon nanotubes and/or SP. A conventional binder is polyvinylidene fluoride (PVDF), which has no electrical conductivity. The acrylic adhesive plays a role in adhesion and electric conduction. Acrylic binders have a high molecular weight and provide excellent bonding capability. The acrylic binder is a polymer, the monomer of which is acrylic acid. Acrylic acid itself has carbon-carbon double bonds, carboxyl (-COOH) and hydroxyl (-OH) functional groups, which undergo lithiation reactions to produce lithium carboxylate and lithium hydroxylate. Through the improvement, the acrylic binder contains a large number of carboxylic acid lithium functional groups in the structure, so that the lithium ion conduction is accelerated, the resistance of the negative pole piece is reduced, and the large-current discharge capacity of the negative pole piece is remarkably improved. The 'line contact' of the carbon nano tube is matched with the 'point contact' of the SP, a good three-dimensional conductive network is formed by point-line combination, the conductive capability of the cathode slurry is obviously improved, and the high-rate discharge capability of the lithium ion battery is further improved.
Further, in the step 5), the solvent is deionized water.
A negative pole piece comprises a negative pole current collector and negative pole slurry coated on the surface of the negative pole current collector, the drying temperature of the coated negative pole piece is 100-130 ℃, and the negative pole slurry is prepared by the preparation method of the negative pole slurry for the lithium ion battery.
The pole piece takes copper foil as a current collector, and the thickness of the copper foil is 6-20 mu m. The negative pole piece is a cuboid, and the length (1000 +/-50) mm, the width (57.5-58.5) mm and the thickness (0.11 +/-0.02) mm; the head and the tail of the pole piece in the length direction are respectively welded with a 1pcs negative pole lug which plays a role in drainage and reduces the structural internal resistance of the battery.
Further, the lithium ion battery also comprises a negative electrode lug, and the negative electrode lug is welded on the negative electrode current collector.
A lithium ion battery adopts the negative pole piece mentioned above as a negative pole.
Furthermore, the lithium ion battery also comprises electrolyte, a diaphragm and a positive pole piece arranged on the positive pole of the battery core of the lithium ion battery, and a positive lug is welded on the positive pole piece.
Still further, the electrolyte of the lithium ion battery comprises lithium salt, additive and solvent, wherein the lithium salt accounts for 12-18 wt% of the electrolyte, the solvent accounts for 70-80 wt% of the electrolyte, and the additive accounts for 4-16 wt% of the electrolyte.
Further, the lithium salt in the electrolyte of the lithium ion battery is LiPF6，LiPF6The concentration of (a) is 1.2-1.6mol/L, the solvent comprises Ethylene Carbonate (EC), dimethyl carbonate (EMC) and methyl ethyl carbonate (DMC), the molar ratio is EC: EMC: DMC ═ 2:1:7, the additive comprises one or more of fluoroethylene carbonate (FEC), vinyl sulfite (VES), 3-fluoropropane sulfonate lactone (FPS), 1-propylene-1, 3-sulfonate lactone (PST) and lithium bis-fluorosulfonyl imide (LiFSI).
LiPF in electrolyte6The lithium ion battery has the advantages that the concentration is high, the content of active lithium ions is more, the transfer number of the lithium ions in unit time is more in the high-rate discharge process, the rate performance is favorably improved, and meanwhile, the cycle life of the lithium ion battery is prolonged. Fluoroethylene carbonate (FEC) and 1-propylene-1, 3-sultone (PST) are used as additives, and can participate in forming a compact and thin SEI film with low impedance and good flexibility on a negative pole piece; the film forming impedance is low, which is beneficial to the rapid conduction of lithium ions; the flexibility of the formed film is good, and the damage to the SEI film structure caused by the volume rapid change of graphite particles in the charging and discharging process is effectively avoided; the film forming structure is compact, and the damage of the graphite structure caused by the solvent molecules being embedded into the graphite is prevented; the thickness of the formed film is thinner, which is beneficial to the rapid conduction of lithium ions. The internal temperature of the lithium ion battery can be rapidly increased during high-rate discharge to cause the thermal decomposition of the SEI film, and the VES and the FPS are added to participate in the formation of the SEI film, so that the structure of the SEI film is more stable at high temperature, and the performance reduction of the lithium ion battery caused by the decomposition of the SEI film at high temperature is avoided; LiFSI is added to improve the conductivity of the electrolyte, and the electrolyte and LiPF are added6And the high-rate discharge capacity of the lithium ion battery is improved under the synergistic effect.
The above-mentioned method for mounting a lithium ion battery comprises the following steps:
winding the positive pole piece, the negative pole piece and the diaphragm according to the overlapping mode of the diaphragm/the negative pole piece/the diaphragm/the positive pole piece to prepare a cylindrical winding core;
and II, welding the negative electrode lug of the negative electrode plate at the bottom of the shell, welding the positive electrode lug of the positive electrode plate at the position of the cap afflux sheet, baking the cylindrical winding core, injecting 5.6-6.0g of electrolyte, and sealing to obtain the lithium ion battery.
Compared with the prior art, the invention has the beneficial effects that:
(1) the modified artificial graphite is selected as a negative active material, and the metal doped with the artificial graphite comprises one or more of Cu, Ni and Ag, so that the conductivity of the negative active material can be improved, and the high-current discharge capacity is further improved; the surface of the artificial graphite particle is coated with a layer of amorphous carbon pyrolyzed by phenolic resin to form a shell-core structure composite material, so that the structural damage of the graphite particle due to the embedding of electrolyte solvent molecules is effectively avoided, and the cycle performance and the large-current discharge capacity of the negative electrode active material are improved; the surface of the artificial graphite forms a porous surface structure through heat treatment, so that the surface area of artificial graphite particles is increased, the migration path of lithium ions is expanded, and the large-current discharge capacity of a negative electrode active material, a negative electrode plate coated with the negative electrode active material and a lithium ion battery taking the negative electrode plate as a negative electrode are improved.
(2) In the formula of the electrolyte used by the lithium ion battery, the concentration of lithium salt is high, the content of active lithium ions is more, the transfer number of lithium ions in unit time is more in the high-rate discharge process, the rate performance is favorably improved, the cycle life of the lithium ion battery is prolonged, VES and FPS are added, the structure of an SEI film is more stable at high temperature, and the problem that the performance of the battery is reduced due to the fact that the SEI film is decomposed at high temperature is avoided; LiFSI is added to improve the conductivity of the electrolyte, and the electrolyte and LiPF are added6And the high-rate discharge capacity of the lithium ion battery is improved under the synergistic effect.
Drawings
Fig. 1 is an internal structural view of a lithium ion battery.
Reference numerals:
1. a positive electrode plate; 2. a negative pole piece; 3. a safety valve; 4. a diaphragm; 5. an insulating sheet; 6. capping; 11. a positive tab; 21. and a negative tab.
Detailed Description
The present invention will be further described with reference to the drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
Example 1
A preparation method of negative electrode slurry for a lithium ion battery comprises the following steps:
1) fully mixing and grinding carbon powder and copper powder according to the weight ratio of 99.99:0.01, graphitizing at 2900 ℃, and cooling to finish doping; wherein the D50 of the metal copper powder is 10 mm;
2) mixing the product doped in the step 1) with phenolic resin according to a ratio of 95: 5, mixing and crushing the materials in a weight ratio, performing high temperature treatment at 2700 ℃, and cooling to finish carbon coating to obtain artificial graphite;
3) crushing the artificial graphite, adding the crushed artificial graphite into an ethanol solution of conductive carbon black, uniformly stirring, heating, evaporating, drying, crushing, carrying out high-temperature heat treatment at 1500 ℃, and cooling to obtain a negative active substance; wherein the weight ratio of the artificial stone toner to the conductive carbon black is 100: 0.5.
4) mixing the negative electrode active material obtained in the step 3), a binder, a conductive agent and a suspending agent, wherein the negative electrode active material accounts for 95.5 wt% of the negative electrode slurry, the binder accounts for 1.5 wt% of the negative electrode slurry, the conductive agent accounts for 1.8 wt% of the negative electrode slurry, and the suspending agent accounts for 1.2 wt% of the negative electrode slurry;
5) adding a solvent into the mixture obtained in the step 4), and stirring to prepare negative electrode slurry with the solid content of 40%.
Further, in step 4), the binder is an acrylic binder, and the conductive agent includes carbon nanotubes and/or SP.
Further, in the step 5), the solvent is deionized water.
A negative pole piece 2 is shown in figure 1 and comprises a negative pole current collector and negative pole slurry coated on the surface of the negative pole current collector, wherein the drying temperature of the coated negative pole piece 2 is 100-130 ℃, and the negative pole slurry is prepared by adopting the preparation method of the negative pole slurry for the lithium ion battery. Coating the negative electrode slurry with the solid content of 40% on a metal copper foil with the thickness of 10 microns, drying at the temperature of 100 ℃, rolling the negative electrode plate 2 with the thickness of about 110 microns, and cutting into long strips. Finally, the negative pole piece 2 is a cuboid with the length (1000 +/-50) mm and the width (57.5-58.5) mm and the thickness (0.11 +/-0.02) mm.
Further, the lithium ion battery also comprises a negative electrode tab 21, and the negative electrode tab 21 is welded on a negative electrode current collector. And welding the negative electrode lug 21 on the copper foil which is not coated with the negative electrode slurry at the two ends of the negative electrode pole piece 2, and sticking the insulating sheet 5.
A lithium ion battery adopts the above-mentioned negative pole piece 2 as a negative pole.
Further, the lithium ion battery further comprises electrolyte, a diaphragm 4 and a positive pole piece 1 arranged on the positive pole of the battery core of the lithium ion battery, wherein a positive current collector 11 is arranged on the positive pole piece 1, and a positive lug 11 is welded on the positive current collector 11.
Still further, the electrolyte of the lithium ion battery comprises lithium salt, an additive and a solvent, wherein the lithium salt accounts for 18 wt% of the electrolyte, the solvent accounts for 70 wt% of the electrolyte, and the additive accounts for 12 wt% of the electrolyte.
Further, the lithium salt in the electrolyte of the lithium ion battery is LiPF6，LiPF6The concentration of (a) is 1.2-1.6mol/L, the solvent comprises Ethylene Carbonate (EC), dimethyl carbonate (EMC) and methyl ethyl carbonate (DMC), the molar ratio is EC: EMC: DMC ═ 2:1:7, the additive comprises one or more of fluoroethylene carbonate (FEC), vinyl sulfite (VES), 3-fluoropropane sulfonate lactone (FPS), 1-propylene-1, 3-sulfonate lactone (PST) and lithium bis-fluorosulfonyl imide (LiFSI).
The above-mentioned method for mounting a lithium ion battery comprises the following steps:
i, winding a positive pole piece 1, a negative pole piece 2 and a diaphragm 4 in an overlapping mode of the diaphragm 4/the negative pole piece 2/the diaphragm 4/the positive pole piece 1 to prepare a cylindrical winding core;
and II, welding the negative electrode tab 21 of the negative electrode plate 2 at the bottom of the shell, laser welding the positive electrode tab 11 of the positive electrode plate 1 at the position of the cap afflux sheet, baking the cylindrical winding core, injecting 5.6-6.0g of electrolyte, combining the cap 6 and the shell, and sealing to obtain the lithium ion battery.
The diaphragm 4 is a PP/PE/PP composite diaphragm 4 with high porosity (45-52%) and low air permeability (110-; the diaphragm 4 has high compressive strength and tensile strength, and is beneficial to improving the safety performance of the lithium ion battery; the diaphragm 4 has strong liquid absorption, which is beneficial to enhancing the infiltration effect of the anode pole piece 1 and the cathode pole piece 2 and improving the cycle performance of the lithium ion battery.
Wherein, the cap 6 is a combined part and is formed by combining a confluence piece, a safety valve 3, a steel cap and a sealing ring.
Example 2
1) Fully mixing and grinding carbon powder and metallic nickel powder according to a weight ratio of 99.80:0.20, graphitizing at a high temperature of 3000 ℃, and cooling to finish doping; wherein the D50 of the metal copper powder is 10 mm;
2) mixing and crushing the doped product in the step 1) and phenolic resin according to a weight ratio of 93:7, performing high temperature 2800 ℃, and cooling to complete carbon coating to obtain artificial graphite;
3) crushing the artificial graphite, adding the crushed artificial graphite into an ethanol solution of conductive carbon black, uniformly stirring, heating, evaporating, drying, crushing, carrying out high-temperature heat treatment at 1800 ℃, and cooling to obtain a negative active substance; wherein the weight ratio of the artificial stone toner to the conductive carbon black is 100: 0.2.
4) mixing the negative electrode active material obtained in the step 3), a binder, a conductive agent and a suspending agent, wherein the negative electrode active material accounts for 95.3 wt% of the negative electrode slurry, the binder accounts for 2.0 wt% of the negative electrode slurry, the conductive agent accounts for 1.2 wt% of the negative electrode slurry, and the suspending agent accounts for 1.5 wt% of the negative electrode slurry;
5) adding a solvent into the mixture obtained in the step 4), and stirring to prepare negative electrode slurry with solid content of 48%.
Further, in step 4), the binder is an acrylic binder, and the conductive agent includes carbon nanotubes and/or SP.
Further, in the step 5), the solvent is deionized water.
A negative pole piece 2 is shown in figure 1 and comprises a negative pole current collector and negative pole slurry coated on the surface of the negative pole current collector, wherein the drying temperature of the coated negative pole piece 2 is 100-130 ℃, and the negative pole slurry is prepared by adopting the preparation method of the negative pole slurry for the lithium ion battery. Coating the negative electrode slurry with the solid content of 40% on a metal copper foil with the thickness of 10 microns, drying at the temperature of 100 ℃, rolling the negative electrode plate 2 with the thickness of about 110 microns, and cutting into long strips. Finally, the negative pole piece 2 is a cuboid with the length (1000 +/-50) mm and the width (57.5-58.5) mm and the thickness (0.11 +/-0.02) mm.
Further, the lithium ion battery also comprises a negative electrode tab 21, and the negative electrode tab 21 is welded on a negative electrode current collector. And welding the negative electrode lug 21 on the copper foil which is not coated with the negative electrode slurry at the two ends of the negative electrode pole piece 2, and sticking the insulating sheet 5.
A lithium ion battery adopts the above-mentioned negative pole piece 2 as a negative pole.
Further, the lithium ion battery further comprises electrolyte, a diaphragm 4 and a positive pole piece 1 arranged on the positive pole of the battery core of the lithium ion battery, wherein a positive current collector 11 is arranged on the positive pole piece 1, and a positive lug 11 is welded on the positive current collector 11.
Still further, the electrolyte of the lithium ion battery comprises lithium salt, an additive and a solvent, wherein the lithium salt accounts for 12 wt% of the electrolyte, the solvent accounts for 80 wt% of the electrolyte, and the additive accounts for 8 wt% of the electrolyte.
Further, the lithium salt in the electrolyte of the lithium ion battery is LiPF6，LiPF6The concentration of (a) is 1.2-1.6mol/L, the solvent comprises Ethylene Carbonate (EC), dimethyl carbonate (EMC) and methyl ethyl carbonate (DMC), the molar ratio is EC: EMC: DMC ═ 2:1:7, the additive comprises one or more of fluoroethylene carbonate (FEC), vinyl sulfite (VES), 3-fluoropropane sulfonate lactone (FPS), 1-propylene-1, 3-sulfonate lactone (PST) and lithium bis-fluorosulfonyl imide (LiFSI).
The above-mentioned method for mounting a lithium ion battery comprises the following steps:
i, winding a positive pole piece 1, a negative pole piece 2 and a diaphragm 4 in an overlapping mode of the diaphragm 4/the negative pole piece 2/the diaphragm 4/the positive pole piece 1 to prepare a cylindrical winding core;
and II, welding the negative electrode tab 21 of the negative electrode plate 2 at the bottom of the shell, laser welding the positive electrode tab 11 of the positive electrode plate 1 at the position of the cap afflux sheet, baking the cylindrical winding core, injecting 5.8g of electrolyte, combining the cap 6 and the shell, and sealing to obtain the lithium ion battery.
The diaphragm 4 is a PP/PE/PP composite diaphragm 4 with high porosity (45-52%) and low air permeability (110-; the diaphragm 4 has high compressive strength and tensile strength, and is beneficial to improving the safety performance of the lithium ion battery; the diaphragm 4 has strong liquid absorption, which is beneficial to enhancing the infiltration effect of the anode pole piece 1 and the cathode pole piece 2 and improving the cycle performance of the lithium ion battery.
Wherein, the cap 6 is a combined part and is formed by combining a confluence piece, a safety valve 3, a steel cap and a sealing ring.
Example 3
1) Mixing carbon powder and silver powder according to a weight ratio of 99.70: 0.30, fully mixing and grinding, graphitizing at the high temperature of 3100 ℃, and cooling to finish doping; wherein the D50 of the metal copper powder is 10 mm;
2) mixing the product doped in the step 1) with phenolic resin according to a ratio of 96: 4, mixing and crushing the raw materials in a weight ratio, cooling the mixture at a high temperature of 3000 ℃ to finish carbon coating to obtain artificial graphite;
3) crushing the artificial graphite, adding the crushed artificial graphite into an ethanol solution of conductive carbon black, uniformly stirring, heating, evaporating, drying, crushing, carrying out high-temperature heat treatment at 2000 ℃, and cooling to obtain a negative active substance; wherein the weight ratio of the artificial stone toner to the conductive carbon black is 100: 3.
4) mixing the negative electrode active material obtained in the step 3), a binder, a conductive agent and a suspending agent, wherein the negative electrode active material accounts for 95.8 wt% of the negative electrode slurry, the binder accounts for 1.7 wt% of the negative electrode slurry, the conductive agent accounts for 1.0 wt% of the negative electrode slurry, and the suspending agent accounts for 1.5 wt% of the negative electrode slurry;
5) adding a solvent into the mixture obtained in the step 4), and stirring to prepare negative electrode slurry with the solid content of 52%.
Further, in step 4), the binder is an acrylic binder, and the conductive agent includes carbon nanotubes and/or SP.
Further, in the step 5), the solvent is deionized water.
A negative pole piece 2 is shown in figure 1 and comprises a negative pole current collector and negative pole slurry coated on the surface of the negative pole current collector, wherein the drying temperature of the coated negative pole piece 2 is 100-130 ℃, and the negative pole slurry is prepared by adopting the preparation method of the negative pole slurry for the lithium ion battery. Coating the negative electrode slurry with the solid content of 52% on a metal copper foil with the thickness of 10 microns, drying at the temperature of 100 ℃, rolling the negative electrode plate 2 with the thickness of about 110 microns, and cutting into long strips. Finally, the negative pole piece 2 is a cuboid with the length (1000 +/-50) mm and the width (57.5-58.5) mm and the thickness (0.11 +/-0.02) mm.
Further, the lithium ion battery also comprises a negative electrode tab 21, and the negative electrode tab 21 is welded on a negative electrode current collector. And welding the negative electrode lug 21 on the copper foil which is not coated with the negative electrode slurry at the two ends of the negative electrode pole piece 2, and sticking the insulating sheet 5.
A lithium ion battery adopts the above-mentioned negative pole piece 2 as a negative pole.
Further, the lithium ion battery further comprises electrolyte, a diaphragm 4 and a positive pole piece 1 arranged on the positive pole of the battery core of the lithium ion battery, wherein a positive current collector 11 is arranged on the positive pole piece 1, and a positive lug 11 is welded on the positive current collector 11.
Still further, the electrolyte of the lithium ion battery comprises lithium salt, an additive and a solvent, wherein the lithium salt accounts for 14 wt% of the electrolyte, the solvent accounts for 70 wt% of the electrolyte, and the additive accounts for 16 wt% of the electrolyte.
Further, the lithium salt in the electrolyte of the lithium ion battery is LiPF6，LiPF6The concentration of (a) is 1.2-1.6mol/L, the solvent comprises Ethylene Carbonate (EC), dimethyl carbonate (EMC) and methyl ethyl carbonate (DMC), the molar ratio is EC: EMC: DMC ═ 2:1:7, the additive comprises one or more of fluoroethylene carbonate (FEC), vinyl sulfite (VES), 3-fluoropropane sulfonate lactone (FPS), 1-propylene-1, 3-sulfonate lactone (PST) and lithium bis-fluorosulfonyl imide (LiFSI).
The above-mentioned method for mounting a lithium ion battery comprises the following steps:
i, winding a positive pole piece 1, a negative pole piece 2 and a diaphragm 4 in an overlapping mode of the diaphragm 4/the negative pole piece 2/the diaphragm 4/the positive pole piece 1 to prepare a cylindrical winding core;
and II, welding the negative electrode tab 21 of the negative electrode plate 2 at the bottom of the shell, laser welding the positive electrode tab 11 of the positive electrode plate 1 at the position of the cap afflux sheet, baking the cylindrical winding core, injecting 6.0g of electrolyte, combining the cap 6 and the shell, and sealing to obtain the lithium ion battery.
The diaphragm 4 is a PP/PE/PP composite diaphragm 4 with high porosity (45-52%) and low air permeability (110-; the diaphragm 4 has high compressive strength and tensile strength, and is beneficial to improving the safety performance of the lithium ion battery; the diaphragm 4 has strong liquid absorption, which is beneficial to enhancing the infiltration effect of the anode pole piece 1 and the cathode pole piece 2 and improving the cycle performance of the lithium ion battery.
Wherein, the cap 6 is a combined part and is formed by combining a confluence piece, a safety valve 3, a steel cap and a sealing ring.
1) Fully grinding carbon powder with the same dosage as that of the embodiment 1, graphitizing at 2900 ℃, and cooling to complete graphitization;
2) mixing the graphitized product in the step 1) with phenolic resin according to a ratio of 95: 5, mixing and crushing the materials in a weight ratio, performing high temperature treatment at 2700 ℃, and cooling to finish carbon coating to obtain artificial graphite;
3) then crushing the artificial graphite, adding the crushed artificial graphite into ethanol solution of conductive carbon black, uniformly stirring, heating, evaporating, drying, crushing, carrying out high-temperature heat treatment at 1500 ℃, and cooling to obtain the negative active substance not doped with copper metal
4) Mixing the negative electrode active material which is not doped with copper metal and is obtained in the step 3), a binder, a conductive agent and a suspending agent, wherein the negative electrode active material accounts for 95.3 wt% of the negative electrode slurry, the binder accounts for 2.0 wt% of the negative electrode slurry, the conductive agent accounts for 1.2 wt% of the negative electrode slurry, and the suspending agent accounts for 1.5 wt% of the negative electrode slurry;
5) adding a solvent into the mixture obtained in the step 4), and stirring to prepare negative electrode slurry with solid content of 48%.
The negative electrode coating, negative electrode sheet and battery were manufactured in the same manner as in example 1.
1) Fully mixing and grinding carbon powder and copper powder according to a weight ratio of 99.99:0.01, graphitizing at 2900 ℃, and cooling to complete doping to obtain artificial graphite; wherein the D50 of the metal copper powder is 10 mm;
2) crushing the doped product in the step 1), adding the crushed product into an ethanol solution of conductive carbon black, uniformly stirring, heating, evaporating, drying, crushing, performing high-temperature heat treatment at 1500 ℃, and cooling to obtain a negative active substance of which the surface of the artificial graphite is not coated with amorphous carbon pyrolyzed by phenolic resin;
3) mixing the artificial graphite obtained in the step 2), wherein the surface of the artificial graphite is not coated with the negative active material, the binder, the conductive agent and the suspending agent, wherein the amorphous carbon is pyrolyzed by phenolic resin, the negative active material accounts for 95.3 wt% of the negative slurry, the binder accounts for 2.0 wt% of the negative slurry, the conductive agent accounts for 1.2 wt% of the negative slurry, and the suspending agent accounts for 1.5 wt% of the negative slurry;
4) adding a solvent into the mixture obtained in the step 3), and stirring to prepare negative electrode slurry with the solid content of 48%.
The negative electrode coating, negative electrode sheet and battery were manufactured in the same manner as in example 1.
1) Fully mixing and grinding carbon powder and copper powder according to the weight ratio of 99.99:0.01, graphitizing at 2900 ℃, and cooling to finish doping; wherein the D50 of the metal copper powder is 10 mm;
2) mixing the product doped in the step 1) with phenolic resin according to a ratio of 95: 5, mixing and crushing the raw materials in a weight ratio, cooling the mixture at a high temperature of 2700 ℃, and finishing carbon coating to obtain a negative active material of which the surface of the artificial graphite is not subjected to heat treatment;
3) mixing the artificial graphite obtained in the step 2), wherein the surface of the artificial graphite is not subjected to heat treatment, and the negative active material, the binder, the conductive agent and the suspending agent are mixed, wherein the negative active material accounts for 95.3 wt% of the negative slurry, the binder accounts for 2.0 wt% of the negative slurry, the conductive agent accounts for 1.2 wt% of the negative slurry, and the suspending agent accounts for 1.5 wt% of the negative slurry;
4) adding a solvent into the mixture obtained in the step 3), and stirring to prepare negative electrode slurry with the solid content of 48%.
The negative electrode coating, negative electrode sheet and battery were manufactured in the same manner as in example 1.
1) Taking carbon powder with the same amount as that in the embodiment 1, graphitizing the carbon powder at the high temperature of 2900 ℃, cooling the carbon powder and crushing the carbon powder to obtain a negative electrode active substance which is not doped with copper metal, does not have amorphous carbon coated on the surface of the artificial graphite after pyrolysis of phenolic resin and has not been subjected to heat treatment on the surface of the artificial graphite;
2) mixing the negative electrode active material obtained in the step 1), a binder, a conductive agent and a suspending agent, wherein the negative electrode active material accounts for 95.3 wt% of the negative electrode slurry, the binder accounts for 2.0 wt% of the negative electrode slurry, the conductive agent accounts for 1.2 wt% of the negative electrode slurry, and the suspending agent accounts for 1.5 wt% of the negative electrode slurry;
3) adding a solvent into the mixture obtained in the step 2), and stirring to prepare negative electrode slurry with the solid content of 48%.
The negative electrode coating, negative electrode sheet and battery were manufactured in the same manner as in example 1.
Results of battery performance testing
The performance of the lithium ion batteries manufactured in the above examples 1 to 3 and the control groups 1 to 4 was tested, and the following test results were obtained:
and (3) capacity testing: the battery was fully charged with a CC-CV (cutoff current 0.01CA) using a current of 0.2CA, left to stand for 5min, and then discharged to 2.75V using a constant current of 0.2CA, and the battery discharge capacity was recorded.
And (3) rate discharge test: charging to 4.2V with constant current and constant voltage at 1.25A (0.5CA), stopping current at 25mA, standing for 5min, discharging to 2.75V with 1.25A (0.5CA), and standing for five min; the cells were charged according to the above-mentioned charge system, and then discharged at 5A/10A/15A/20A/25A/30A/35A/40A, respectively, and the discharge capacities thereof were recorded.
And (3) testing the cycle performance: charging to 4.2V at constant current and constant voltage with 2A (0.8CA) current and cutoff current of 25mA, standing for five minutes, discharging to 2.75V with 20A (8CA) current, and standing for five minutes; the cycle life test was carried out according to this protocol.
Table 1 discharge capacity comparison of lithium ion batteries
| Example 1 | Example 2 | Example 3 | |
|
|
|
|
| Capacity mAh | 2550 | 2556 | 2560 | 2540 | 2543 | 2550 | 2530 |
TABLE 2 comparison of discharge capacity retention rates of lithium ion batteries at different discharge rates
| Discharge rate | Discharge current | Example 1 | Example 2 | Example 3 | |
|
|
|
| 0.5C | 1.25A | 100.00％ | 100.00％ | 100.00％ | 100.00％ | 100.00％ | 100.00％ | 100.00％ |
| 2C | 5A | 99.52％ | 99.62％ | 99.54％ | 99.10％ | 99.01％ | 98.90％ | 98.20％ |
| 4C | 10A | 98.12％ | 98.28％ | 98.32％ | 97.83％ | 97.91％ | 97.88％ | 96.51％ |
| 6C | 15A | 97.65％ | 97.69％ | 97.70％ | 97.10％ | 97.02％ | 96.92％ | 93.22％ |
| 8C | 20A | 96.35％ | 96.12％ | 96.21％ | 95.71％ | 95.99％ | 95.37％ | 88.81％ |
| 10C | 25A | 95.51％ | 95.58％ | 95.62％ | 94.85％ | 94.73％ | 94.66％ | 79.68％ |
| 12C | 30A | 94.12％ | 94.09％ | 94.37％ | 93.62％ | 93.27％ | 92.58％ | 62.24％ |
| 14C | 35A | 93.37％ | 93.48％ | 93.56％ | 92.85％ | 92.92％ | 91.28％ | 31.38％ |
| 16C | 40A | 92.47％ | 92.64％ | 92.73％ | 90.87％ | 90.16％ | 89.75％ | 9.59％ |
TABLE 3 comparison of capacity retention after 1000 weeks cycling of lithium ion batteries
As can be seen from Table 1, the discharge capacities of the lithium ion batteries of examples 1 to 3 and comparative examples 1 to 3 were higher than that of comparative example 4, and the discharge capacities of examples 1 to 3 were higher than that of comparative examples 1 to 4.
As can be seen from Table 2, the capacity retention rates of the discharge at 16C rate (40A current) in examples 1 to 3 and comparative examples 1 to 3 were higher than that of comparative example 4; wherein the examples 1 to 3 had higher retention of discharge capacity at 16C rate than the comparative examples 1 to 4. When the control group is discharged at the rate of 8C/10C/12C/14C/16C, the discharge capacity retention rate is sharply reduced, and the high-rate discharge performance of the control group battery is poor. Compared with the control group 1, the multiplying power discharge performance of the doped metal powder is better; compared with the control group 2, the multiplying power discharge performance of the coating of the amorphous carbon is better in the example 1; the comparative example 1 and the comparative example 3 have better rate discharge performance after surface heat treatment.
As can be seen from Table 3, the capacity retention rates of the examples 1-3 and the controls 1-3 are higher than that of the control 4 after 1000 cycles, and the capacity retention rates of the examples 1-3 are higher than those of the controls 1-4. The capacity retention rate of the control group 4 after 300 weeks of circulation is only 75.8%, and the circulation performance is poor. Compared with the control group 1, the cycle performance is better after the copper metal powder is doped in the embodiment 1; compared with the control group 2, the cycle performance of the coated amorphous carbon is better in the example 1; the cycle performance after the surface heat treatment was better in comparative example 1 and comparative example 3.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. A preparation method of negative electrode slurry for a lithium ion battery is characterized by comprising the following steps:
1) fully mixing and grinding carbon powder and metal powder, graphitizing at the high temperature of 2900-; wherein, the metal powder is 0.01 to 0.3 weight percent, the carbon powder is complemented to 100 weight percent, and the metal powder comprises one or more of Cu, Ni and Ag;
2) mixing and crushing the product doped in the step 1) with phenolic resin, heating to 2700-; wherein the phenolic resin accounts for 4-7 wt%, and the product doped in the step 1) is the balance of 100 wt%;
3) crushing the artificial graphite, adding the crushed artificial graphite into an ethanol solution of the conductive carbon black, uniformly stirring, heating, evaporating, drying, crushing, performing high-temperature heat treatment at 1500-; wherein the weight ratio of the artificial stone toner to the conductive carbon black is 100: 0.2-3.0;
4) mixing the negative electrode active material obtained in the step 3), a binder, a conductive agent and a suspending agent, wherein the negative electrode active material accounts for 95.5 wt% of the negative electrode slurry, the binder accounts for 1.5 wt% of the negative electrode slurry, the conductive agent accounts for 1.8 wt% of the negative electrode slurry, and the suspending agent accounts for 1.2 wt% of the negative electrode slurry;
5) adding a solvent into the mixture obtained in the step 4), and stirring to prepare negative electrode slurry with the solid content of 40-52%.
2. The method for preparing the negative electrode slurry for the lithium ion battery according to claim 1, wherein in the step 4), the binder is an acrylic binder, and the conductive agent comprises carbon nanotubes and/or SP.
3. The method for preparing the negative electrode slurry for the lithium ion battery according to claim 1, wherein in the step 5), the solvent is deionized water.
4. A negative pole piece is characterized in that: the method comprises a negative current collector and negative slurry coated on the surface of the negative current collector, wherein the drying temperature of the coated negative pole piece is 100-130 ℃, and the negative slurry is prepared by the preparation method of the negative slurry for the lithium ion battery as claimed in any one of claims 1-3.
5. The negative electrode tab of claim 4, wherein: the negative electrode tab is welded on the negative electrode current collector.
6. A lithium ion battery, characterized in that the negative pole piece of any one of claims 4 to 5 is used as a negative pole.
7. The lithium ion battery of claim 6, wherein: the lithium ion battery also comprises electrolyte, a diaphragm and a positive pole piece arranged on the positive pole of the battery core of the lithium ion battery, wherein a positive lug is welded on the positive pole piece.
8. The lithium ion battery of claim 7, wherein: the electrolyte of the lithium ion battery comprises lithium salt, an additive and a solvent, wherein the lithium salt accounts for 12-18 wt% of the electrolyte, the solvent accounts for 70-80 wt% of the electrolyte, and the additive accounts for 4-16 wt% of the electrolyte.
9. The lithium ion battery of claim 8, wherein: the lithium salt in the electrolyte of the lithium ion battery is LiPF6，LiPF6In a concentration of 1.2 to 1.6mol/L, a solvent comprising ethylene carbonate, dimethyl carbonate and methyl ethyl carbonate in a molar ratio of ethylene carbonate to dimethyl carbonate to methyl ethyl carbonate of 2:1:7, and an additive comprising fluoroethylene carbonate, vinyl ethylene sulfite, 3-fluoropropane sultone, 1-propene-1, 3-sultone and bis-ethyl carbonateOne or more of lithium fluorosulfonylimide.
10. A method of mounting a lithium ion battery according to any of claims 7 to 9, comprising the steps of:
winding the positive pole piece, the negative pole piece and the diaphragm according to the overlapping mode of the diaphragm/the negative pole piece/the diaphragm/the positive pole piece to prepare a cylindrical winding core;
and II, welding the negative electrode lug of the negative electrode plate at the bottom of the shell, welding the positive electrode lug of the positive electrode plate at the position of the cap afflux sheet, baking the cylindrical winding core, injecting 5.6-6.0g of electrolyte, and sealing to obtain the lithium ion battery.
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| CN113972372A (en) * | 2021-09-26 | 2022-01-25 | 西安交通大学 | Metal graphite medium-temperature energy storage battery and preparation method thereof |
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