CN109638223B - Silicon-based negative electrode of lithium ion battery and preparation method and application thereof - Google Patents
Silicon-based negative electrode of lithium ion battery and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of new energy, and particularly relates to a silicon-based negative electrode of a lithium ion battery, and a preparation method and application thereof.
Description
Technical Field
The invention belongs to the technical field of new energy, and particularly relates to a silicon-based negative electrode of a lithium ion battery, and a preparation method and application thereof.
Background
With the rapid development of economy, humanity and science, people and people have more frequent communication, and the urgent need is to shorten the distance between people and people. Motor vehicles, as the main means of transportation on land, are growing explosively, with this enormous convenience, there is a consequent potential risk. Most motor vehicles run by using fuel as power, and serious air pollution is caused. The protection of the environment is the current theme, in order to promote the environmental quality, the energy of the motor vehicle is developed from petroleum to clean energy, and the lithium ion battery is popular because of large specific capacity, strong endurance and reusability.
The development of high specific energy lithium ion batteries depends on the battery positive and negative electrodes, electrolyte and separatorThe respective properties and the mutual cooperation of the components such as the film. The negative electrode used in the current commercial lithium ion battery is mainly made of graphite, and lithium ions are inserted and removed from the graphite layer during charging and discharging. The common graphite negative pole in the market has the actual capacity of more than 360mAh/g, and is very close to the theoretical capacity. The theoretical capacity of the silicon-based negative electrode can reach 4212mAh/g at the highest, and lithium forms Li in silicon 4.4 The Si alloy has a large volume change during charging due to the large amount of lithium dissolved in silicon, and the negative electrode can expand up to 420%, and contract in the same volume when discharged. The silicon-based negative electrode is easy to break and fall off due to huge volume expansion and contraction, the effective electrical contact with a current collector is easy to lose in the circulation process, and along with the increase of the charging and discharging times, the stability of the lithium ion battery adopting the silicon-based negative electrode is poor due to the problems, and the service life of the battery is short. While the change of the silicon-based negative electrode reaches a certain bottleneck, a huge space exists for improvement in terms of current collectors.
Aiming at the defects of the silicon negative electrode of the conventional lithium ion battery, the publication No. 108511762A improves the tensile strength of the positive current collector, reduces the thickness of the positive current collector, improves the volume energy density of the lithium ion battery and improves the low-temperature charge and discharge performance of the lithium ion battery by improving the conductivity of the positive current collector. However, such current collector variation does not address the hazards associated with cell volume expansion.
Disclosure of Invention
Aiming at the existing problems, the invention provides a silicon-based negative electrode capable of overcoming the defects of the silicon-based negative electrode and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the silicon-based negative electrode of the lithium ion battery comprises a current collector, wherein the surface of the current collector comprises a surface coating material layer which is formed by a carbon coating layer and a conductive ink layer from inside to outside in sequence, and the surface coating material is in one or two of fibrous and granular forms.
Preferably, the base material of the current collector is copper foil.
Preferably, the thickness of the conductive ink layer is 0.2-1 μm.
Preferably, the raw material of the conductive ink comprises one or two of nano silver particles and nano silver wires.
More preferably, the particle size of the nano silver particles is 5-10nm, and the diameter of the nano silver wires is 10-20 nm.
Preferably, the raw material of the coated carbon layer comprises the following components by mass: 1-5g of carbon nano tube, 1-5g of carbon fiber, 15-35g of conductive agent, 45-60g of deionized water, 5-9g of binder and 5-8g of dispersing agent.
Further preferably, the thickness of the coated carbon layer is 1 to 5 μm. The thickness of the slurry is controlled, so that the thickness of a current collector can be reduced, the volume of the battery is compressed, the exchange rate between two poles of the battery can be promoted, and the performance of the battery is improved.
The current collector is made of copper foil, the surface of the copper foil is smooth, if the current collector is directly contacted with the silicon-based negative electrode, the adhesion force of the copper foil and the silicon-based negative electrode is insufficient, the active substances are easy to fall off, and the performance of the battery is further reduced. The coating of the carbon coating layer on the copper foil can greatly increase the roughness of the surface of the copper foil, when the silicon-based negative electrode is directly contacted with the carbon coating layer with the rough surface, the adhesion can be improved, and meanwhile, the contact area of the carbon coating layer and the current collector is increased, namely, the alternating current area of the silicon-based negative electrode and the current collector is enlarged, the interface contact resistance is reduced, and the defect of poor conductivity of the silicon-based negative electrode is overcome.
Preferably, the conductive ink is prepared by sequentially adding nano silver particles/nano silver wires, propylene glycol methyl ether, dipropylene glycol methyl ether and ethanol into deionized water, stirring at a high speed, adding acrylic resin, continuously stirring to form uniform and stable mixture slurry, and finally silk-screening (coating) on the coated carbon layer.
Although the surface of the current collector is provided with the coating carbon layer, the improvement range of the performance of the battery by the coating carbon layer is limited, the invention further silkscreens a layer of conductive ink, the conductive ink is promoted to be benefited by mainly adding a nano silver material and changing the form of the nano silver material, namely, the conductive contact between the current collector and the silicon-based negative electrode is further improved, the interface resistance is reduced, the bonding strength between the current collector and the silicon-based negative electrode is improved, the nano silver coating has good flexibility, and the reduction of the conductivity or the reduction of the bonding force caused by the falling of the coating layer possibly caused by the bending and winding of the pole piece in the actual use can be further avoided. The morphology change of the nano silver in the conductive ink promotes the morphology change of the coating material layer on the surface of the current collector.
A preparation method of a silicon-based negative electrode of a lithium ion battery comprises the following steps:
firstly, sequentially adding the carbon nano tube, the carbon fiber, the conductive agent and the dispersing agent into deionized water, fully stirring, then adding the binder, continuously stirring, and fully dispersing to form slurry;
and uniformly coating the slurry on the surface of a copper foil to form a coating carbon layer, carrying out formation and drying treatment, then, silk-screening conductive ink on the coating carbon layer to form a conductive ink layer, drying and curing to obtain a current collector, and assembling the current collector into a battery cathode.
The invention enhances the performance of the battery by improving the current collector, the preparation process of the current collector is very simple, the needed labor and time are less, the slurry mixture can obtain proper softening degree by controlling the temperature and time of formation and the binder in the slurry mixture can be promoted to form effective crosslinking effect, the slurry layer and the copper foil are tightly combined by controlling the pressure applied during formation, and the defect that the contact of active substances, the current collector and a conductive agent in the battery is poor due to volume expansion in the long-term circulation process is relieved. Meanwhile, as the carbon coating layer on the surface of the copper foil is also subjected to silk-screen printing (coating) of conductive ink, the conductive contact between the current collector and the negative electrode is improved, the interface resistance is reduced, the absorption amount of electrolyte can be further increased, and the cycling stability of the battery is improved.
Preferably, the silicon-based negative electrode of the lithium ion battery is applied to the lithium ion battery, and the lithium ion battery comprises the silicon-based negative electrode of the lithium ion battery.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, the carbon-containing mixture is coated on the copper foil, so that the adhesion force of the active substance and the current collector is improved, and the volume expansion of the silicon-based negative electrode in the charge-discharge cycle process is relieved.
(2) The method of combining the slurry coating and the conductive ink increases the contact area of the active substance and the current collector, overcomes the defect of poor conductivity of the silicon-based negative electrode, and improves the rate capability of the battery.
(3) The preparation method of the current collector is simple and effective, can greatly accelerate the commercialization process of the silicon-based negative electrode, and is beneficial to the development of the lithium ion battery with high specific energy and long service life.
Drawings
Fig. 1 is a cross-sectional view of the current collector and its surface coating material layer of the present invention.
In the figure, 1, a conductive ink layer; 2. coating a carbon layer; 3. a current collector substrate.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Example 1
Weighing the raw materials of the current collector coating material, sequentially adding 4.0g of carbon nano tube, 4.0g of carbon fiber, 30.0g of conductive carbon black Super P and 8.0g of dispersing agent into 50.0g of deionized water, stirring for 3 hours, then adding 6.0g of binder, and continuously stirring for 30 minutes to form uniform and stable slurry;
uniformly coating the slurry on a conductive copper foil with a specification thickness, drying the solvent to form a coated carbon layer after normalization, and controlling the thickness of the coated carbon layer to be 1.0 mu m;
sequentially adding 1.0g of nano silver particles with the particle size of 5nm, 1.0g of propylene glycol methyl ether, 1.0g of dipropylene glycol methyl ether and 10.0g of ethanol into 20.0g of deionized water, stirring at a high speed for 2 hours, then adding 30.0g of 37% acrylic resin, and continuously stirring for 20 minutes to form uniform and stable mixed slurry;
and uniformly coating the mixed slurry on the surface of the coated carbon layer to form a conductive ink layer, controlling the thickness of the conductive ink layer to be 0.4 mu m, and drying at 120 ℃ to obtain the current collector.
Example 2
Weighing the raw materials of the current collector coating material, sequentially adding 3.0g of carbon nano tube, 3.0g of carbon fiber, 20.0g of conductive carbon black Super P and 6.0g of dispersing agent into 50.0g of deionized water, stirring for 3 hours, then adding 6.0g of binder, and continuously stirring for 30 minutes to form uniform and stable slurry;
uniformly coating the slurry on a conductive copper foil with a specification thickness, drying a solvent to form a coated carbon layer after normalization, and controlling the thickness of the coated carbon layer to be 4.0 mu m;
sequentially adding 1.0g of nano silver particles with the particle size of 5nm, 1.0g of propylene glycol methyl ether, 1.0g of dipropylene glycol methyl ether and 10.0g of ethanol into 20.0g of deionized water, stirring at a high speed for 2 hours, then adding 30.0g of 37% acrylic resin, and continuously stirring for 20 minutes to form uniform and stable mixed slurry;
and uniformly coating the mixed slurry on the surface of the coated carbon layer to form a conductive ink layer, controlling the thickness of the conductive ink layer to be 0.2 mu m, and drying at 120 ℃ to obtain the current collector.
Example 3
Weighing the raw materials of the current collector coating material, sequentially adding 3.0g of carbon nano tube, 3.0g of carbon fiber, 20.0g of conductive carbon black Super P and 6.0g of dispersing agent into 50.0g of deionized water, stirring for 3 hours, then adding 6.0g of binder, and continuously stirring for 30 minutes to form uniform and stable slurry;
uniformly coating the slurry on a conductive copper foil with a certain thickness, drying the solvent to form a coated carbon layer after normalization, and controlling the thickness of the coated carbon layer to be 2.0 mu m;
sequentially adding 1.5g of nano silver particles with the particle size of 10nm, 1.0g of propylene glycol methyl ether, 1.0g of dipropylene glycol methyl ether and 10.0g of ethanol into 20.0g of deionized water, stirring at a high speed for 2 hours, then adding 30.0g of 37% acrylic resin, and continuously stirring for 20 minutes to form uniform and stable mixed slurry;
and uniformly coating the mixed slurry on the surface of the carbon coating layer to form a conductive ink layer, controlling the thickness of the conductive ink layer to be 1.0 mu m, and drying at 120 ℃ to obtain the current collector.
Example 4
Weighing the raw materials of the current collector coating material, sequentially adding 2.0g of carbon nano tube, 3.0g of carbon fiber, 20.0g of conductive carbon black Super P and 6.0g of dispersing agent into 50.0g of deionized water, stirring for 3 hours, then adding 8.0g of binder, and continuing stirring for 30 minutes to form uniform and stable slurry;
uniformly coating the slurry on a conductive copper foil with a certain thickness, drying the solvent to form a coated carbon layer after normalization, and controlling the thickness of the coated carbon layer to be 3.0 mu m;
sequentially adding 1.5g of nano silver wire with the diameter of 10 nanometers and the length-diameter ratio of 200, 1.2g of propylene glycol methyl ether, 1.5g of dipropylene glycol methyl ether and 13.0g of ethanol into 20.0g of deionized water, stirring at a high speed for 2 hours, adding 35.0g of 37% acrylic resin, and continuously stirring for 20 minutes to form uniform and stable mixed slurry;
and uniformly coating the mixed slurry on the surface of the carbon coating layer to form a conductive ink layer, controlling the thickness of the conductive ink layer to be 0.9 mu m, and drying at 120 ℃ to obtain the current collector.
Example 5
Weighing the raw materials of the current collector coating material, sequentially adding 2.0g of carbon nano tube, 3.0g of carbon fiber, 20.0g of conductive carbon black Super P and 6.0g of dispersing agent into 50.0g of deionized water, stirring for 3 hours, then adding 8.0g of binder, and continuing stirring for 30 minutes to form uniform and stable slurry;
uniformly coating the slurry on a conductive copper foil with a certain thickness, drying the solvent to form a coated carbon layer after normalization, and controlling the thickness of the coated carbon layer to be 1.5 mu m;
respectively and sequentially adding 1.0g of nano silver wire with the diameter of 20 nanometers and the length-diameter ratio of 100, 1.5g of propylene glycol methyl ether, 2.0g of dipropylene glycol methyl ether and 15.0g of ethanol into 25.0g of deionized water, stirring at a high speed for 2 hours, then adding 30.0g of 37% acrylic resin, and continuing stirring for 20 minutes to form uniform and stable mixed slurry;
and uniformly coating the mixed slurry on the surface of the carbon coating layer to form a conductive ink layer, controlling the thickness of the conductive ink layer to be 0.7 mu m, and drying at 120 ℃ to obtain the current collector.
Example 6
Weighing the raw materials of the current collector coating material, sequentially adding 4.0g of carbon nano tube, 4.0g of carbon fiber, 30.0g of conductive carbon black Super P and 8.0g of dispersing agent into 55.0g of deionized water, stirring for 3.0h, then adding 8.0g of binder, and continuously stirring for 30min to form uniform and stable slurry;
uniformly coating the slurry on a conductive copper foil with a certain thickness, drying the solvent to form a coated carbon layer after normalization, and controlling the thickness of the coated carbon layer to be 1.3 mu m;
sequentially adding 1.5g of nano silver wire with the diameter of 15 nanometers and the length-diameter ratio of 120, 1.2g of propylene glycol methyl ether, 1.5g of dipropylene glycol methyl ether and 13.0g of ethanol into 20.0g of deionized water, stirring at a high speed for 2 hours, adding 35.0g of 37% acrylic resin, and continuously stirring for 20 minutes to form uniform and stable mixed slurry;
and uniformly coating the mixed slurry on the surface of the coated carbon layer to form a conductive ink layer, controlling the thickness of the conductive ink layer to be 0.8 mu m, and drying at 120 ℃ to obtain the current collector.
Example 7
Weighing the raw materials of the current collector coating material, sequentially adding 2.0g of carbon nano tube, 2.0g of carbon fiber, 20.0g of conductive carbon black Super P and 6.0g of dispersing agent into 55.0g of deionized water, stirring for 3.0h, then adding 6.0g of binder, and continuously stirring for 30min to form uniform and stable slurry;
uniformly coating the slurry on a conductive copper foil with a certain thickness, drying the solvent to form a coated carbon layer after normalization, and controlling the thickness of the coated carbon layer to be 1.0 mu m;
sequentially adding 2.0g of nano silver particles with the diameter of 15 nanometers, 1.0g of propylene glycol methyl ether, 1.0g of dipropylene glycol methyl ether and 12.0g of ethanol into 20.0g of deionized water, stirring at a high speed for 2 hours, adding 35.0g of 37% acrylic resin, and continuously stirring for 20 minutes to form uniform and stable mixed slurry;
and uniformly coating the mixed slurry on the surface of the coated carbon layer to form a conductive ink layer, controlling the thickness of the conductive ink layer to be 0.8 mu m, and drying at 120 ℃ to obtain the current collector.
Comparative example 1
Weighing the raw materials of the current collector coating material, sequentially adding 4.0g of carbon nano tube, 4.0g of carbon fiber, 30.0g of conductive carbon black Super P and 8.0g of dispersing agent into 50.0g of deionized water, stirring for 3 hours, then adding 6.0g of binder, and continuously stirring for 30 minutes to form uniform and stable slurry;
and uniformly coating the slurry on a conductive copper foil with a certain thickness, drying the solvent to form a coating layer after normalization, and controlling the thickness of the coating layer to be 0.7 mu m to obtain the current collector.
Comparative example 2
Weighing the raw materials of the current collector coating material, sequentially adding 1.0g of nano silver with the particle size of 5nm, 1.0g of propylene glycol methyl ether, 1.0g of dipropylene glycol methyl ether and 10.0g of ethanol into 20.0g of deionized water, stirring at a high speed for 2 hours, then adding 30.0g of 37% acrylic resin, and continuing stirring for 20 minutes to form uniform and stable slurry;
and uniformly coating the slurry on a conductive copper foil with a certain thickness, drying the solvent to form a coating layer after normalization, controlling the thickness of the coating layer to be 0.15 mu m, and then drying at 120 ℃ to obtain the current collector.
Comparative example 3
The negative electrode current collector is directly made of a conventional commercial copper foil without any addition or special treatment on the surface without any treatment.
The current collectors obtained in examples 1 to 7 and comparative examples 1 to 3 were applied to batteries, wherein the positive and negative electrodes of the batteries were prepared as follows:
preparing a positive electrode:
mixing a positive electrode active substance, a conductive agent, a binder and a solvent NMP in an agate tank according to a ratio of 90:5:5:100, placing the mixture in a planetary ball mill, stirring and mixing for 4 hours to obtain a positive electrode slurry, coating the positive electrode slurry on a carbon-coated aluminum foil current collector by using a coating machine, performing vacuum drying and volatilization of PEG, rolling and slitting the coated electrode, and performing vacuum drying to obtain the lithium ion battery positive plate.
Preparing a negative electrode:
mixing and stirring the negative active substance, the negative conductive agent, the negative adhesive and the negative solvent uniformly to prepare negative slurry, and coating the negative slurry on a negative current collector specially made by the invention to prepare a negative plate.
Assembling the battery: and (4) placing the positive plate, the diaphragm and the negative plate into a battery shell, and sealing the battery core after injecting the electrolyte to obtain the lithium ion battery.
The assembled batteries of examples 1-7 and comparative examples 1-3 were tested for pole piece peel force, pole piece conductivity, negative electrode, specific energy, and the results are shown in table 1:
table 1: performance of the batteries of examples 1 to 7 and comparative examples 1 to 3
From the data in the table, the peel force of the negative electrode sheet is improved by the method of the present invention in examples 1 to 7, which shows that the adhesion degree of the negative electrode on the current collector is increased; comparing the resistance of the negative plate with the ohmic internal resistance of the battery, the negative resistance is obviously reduced and the ohmic internal resistance of the battery is greatly reduced after the method is adopted in the embodiments 1 to 7, which shows that the interface resistance between the silicon-based negative active material and the current collector is greatly reduced after the negative current collector is treated by the method; meanwhile, the first efficiency of the battery is improved, and the cycle life of the battery is greatly prolonged.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (2)
1. The silicon-based negative electrode of the lithium ion battery comprises a current collector and is characterized in that the surface of the current collector comprises a surface coating material layer which is formed by a carbon coating layer and a conductive ink layer from inside to outside in sequence, and the surface coating material is in one or two of fibrous and granular forms;
the thickness of the conductive ink layer is 0.4 mu m;
the raw material of the conductive ink is nano silver particles;
the raw material of the coating carbon layer comprises the following components by mass: 4.0g of carbon nano tube, 4.0g of carbon fiber, 30.0g of conductive carbon black, 50.0g of deionized water, 6.0g of binder and 8.0g of dispersant;
the particle size of the nano silver particles is 5 nm;
the thickness of the coated carbon layer is 1 μm;
the preparation method of the silicon-based negative electrode of the lithium ion battery comprises the following steps:
firstly, sequentially adding the carbon nano tube, the carbon fiber, the conductive carbon black and the dispersing agent into deionized water, fully stirring, then adding the binder, continuously stirring, and fully dispersing to form slurry;
uniformly coating the slurry on the surface of copper foil to form a coated carbon layer, performing formation and drying treatment, then silk-screening conductive ink on the coated carbon layer to form a conductive ink layer, drying and curing to obtain a current collector, and assembling the current collector into a battery cathode;
the preparation method of the conductive ink comprises the following steps: 1.0g of nano silver particles with the particle size of 5nm, 1.0g of propylene glycol methyl ether, 1.0g of dipropylene glycol methyl ether and 10.0g of ethanol are sequentially added into 20.0g of deionized water, high-speed stirring is carried out for 2 hours, then 30.0g of 37% acrylic resin is added, and stirring is continued for 20 minutes.
2. Use of the silicon-based negative electrode of a lithium ion battery according to claim 1 in a lithium ion battery, wherein the lithium ion battery comprises a silicon-based negative electrode of a lithium ion battery.
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| CN106299247A (en) * | 2016-09-26 | 2017-01-04 | 深圳市卓能新能源股份有限公司 | A kind of lithium ion battery aqueous silicon-base negative plate and preparation method thereof |
| CN106797033A (en) * | 2014-08-25 | 2017-05-31 | 日产自动车株式会社 | Electric connection structure |
| CN107528044A (en) * | 2017-07-25 | 2017-12-29 | 深圳市沃特玛电池有限公司 | A kind of lithium ion battery negative electrode and preparation method thereof |
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| CN106797033A (en) * | 2014-08-25 | 2017-05-31 | 日产自动车株式会社 | Electric connection structure |
| CN106299247A (en) * | 2016-09-26 | 2017-01-04 | 深圳市卓能新能源股份有限公司 | A kind of lithium ion battery aqueous silicon-base negative plate and preparation method thereof |
| CN107528044A (en) * | 2017-07-25 | 2017-12-29 | 深圳市沃特玛电池有限公司 | A kind of lithium ion battery negative electrode and preparation method thereof |
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