CN113764622B - Preparation method of low-expansion lithium battery silicon-carbon negative plate - Google Patents
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Abstract
The invention discloses a preparation method of a low-expansion lithium battery silicon-carbon negative plate, which comprises the steps of compounding porous nano-silicon and a long-tube carbon nano-tube in a citric acid solution to obtain a Si-CNT precursor, grinding, mixing and sintering the Si-CNT precursor with artificial graphite and cane sugar to obtain silicon-carbon powder, dispersing the obtained silicon-carbon powder, a water-based composite binder, graphene, a dispersing agent and pure water in proportion to prepare slurry, coating the slurry on two sides of a metal foil material, and drying to obtain the low-expansion lithium battery silicon-carbon negative plate. According to the invention, porous nano-silicon and one-dimensional material carbon nano-tubes are selected for compounding, and a linear network structure is formed outside and inside the porous nano-silicon with larger aperture, so that the volume expansion of silicon-carbon powder in the charge-discharge cycle process is effectively inhibited.
Description
Technical Field
The invention relates to the technical field of ternary lithium ion power batteries, in particular to a preparation method of a low-expansion lithium battery silicon-carbon negative plate.
Background
In recent years, china pays more attention to new energy, and with the coming of a series of policies, the research of lithium ion batteries is gradually developed towards indexes of high energy density, long cycle performance and high safety. To meet this demand, research into high capacity density negative electrode materials has been conducted. And the silicon material has higher theoretical capacity, so that the silicon material is one of the most ideal high-performance lithium battery negative electrode materials.
The theoretical capacity of silicon is up to 4200mAh/g, which is more than ten times of the theoretical capacity of 372mAh/g of graphite which is the cathode material of the current mainstream lithium ion battery, and the silicon has lower de-intercalation lithium voltage (less than 0.5V), high safety, rich sources and low price. However, during the charging and discharging process of the battery, the lithium-intercalation reaction of silicon is accompanied with huge volume change (> 300%), which causes the destruction and mechanical pulverization of the material structure, leads to the separation between electrode materials and between the electrode materials and a current collector, and further loses the electrical contact, thus causing rapid capacity attenuation and deterioration of cycle performance. The severe volume effect causes the SEI film on the silicon surface to be in a dynamic process of destruction-reconstruction, which causes continuous lithium ion consumption and further influences the cycle performance. The severe volume effect of silicon during charging and discharging limits its current commercial application.
Disclosure of Invention
The invention aims to provide a preparation method of a low-expansion lithium battery silicon-carbon negative plate, which greatly inhibits the volume expansion of a silicon-carbon negative material and prolongs the cycle life of the battery.
The technical scheme of the invention is as follows:
a preparation method of a low-expansion lithium battery silicon-carbon negative plate specifically comprises the following steps:
(1) Preparation of Si-CNT precursor: adding porous nano-silicon, a carbon nano-tube and a dispersing agent into deionized water according to a certain proportion, uniformly stirring, adding a citric acid solution, introducing the mixture solution into a sand mill for mixing and dispersing, introducing the mixed dispersion solution into a spray dryer, and preparing a Si-CNT precursor after spray drying; wherein, the ratio of porous nano silicon: carbon nanotube: the mass ratio of the dispersing agent is 85-95:3-15:0.2 to 1.3;
(2) Ball-milling and mixing the Si-CNT precursor prepared in the step (1), artificial graphite and cane sugar in proportion, and vibrating and sieving to prepare uniform and compact Si-CNT/graphite/cane sugar mixed powder; wherein, si-CNT precursor: artificial graphite: the mass ratio of the sucrose is 1-15:70-90:5-20 parts of;
(3) And preparing silicon-carbon powder: sintering the Si-CNT/graphite/sucrose mixed powder prepared in the step (2) under the protective atmosphere of inert gas, cooling, taking out, crushing and sieving to obtain silicon-carbon powder;
(4) And preparing the low-expansion lithium battery silicon-carbon negative plate: and (3) mixing and dispersing the silicon-carbon powder prepared in the step (3), the water-based composite binder, the graphene, the dispersing agent and pure water into slurry, coating the slurry on two sides of the metal foil, and then sequentially drying, rolling, slitting and laser cutting to obtain the low-expansion lithium battery silicon-carbon negative plate.
The specific surface area of the porous nano silicon is 200-350m 2 Per g, pore volume of 0.3-0.5cm 3 Per g, wall thickness of 5-100nm, pore diameter of 50-300nm.
The length of the carbon nano tube is 20-100 mu m, and the tube diameter is 1-15nm.
The dispersing agent is polyvinylpyrrolidone and carboxymethyl cellulose, and the mass ratio of the polyvinylpyrrolidone to the carboxymethyl cellulose is (0.1-0.3): 0.1-1.0.
The spray drying process parameters in the step (1) are as follows: the liquid inlet amount is 50-100ml/min, the air inlet temperature is 200-300 ℃, the air outlet temperature is 150-200 ℃, and the blowing frequency is 20-30Hz.
The sintering process parameters in the step (3) under the inert gas protective atmosphere are as follows: in the first stage, the heating rate is 0.5-2 ℃/min, the temperature is raised to 150-250 ℃, and the heat preservation time is 0.5-1h; the temperature rise rate of the second stage is 5-10 ℃/min, the temperature is raised to 1000-1200 ℃, and the heat preservation time is 1-10h.
The aqueous composite binder in the step (4) comprises polyacrylic acid and polyvinyl alcohol, and the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 8.5.
The mass ratio of the silicon-carbon powder, the aqueous composite binder, the graphene and the dispersing agent in the step (4) is 93-96:2.0-4.0:0.5-1.5:1.0-1.5.
The invention has the advantages that:
(1) According to the invention, the silicon-carbon material is inhibited from expanding from the material end, the porous nano-silicon is selected to be compounded with the one-dimensional material carbon nano-tube, and a linear network structure is formed outside and inside the porous nano-silicon with larger aperture through the carbon nano-tube with longer tube length, so that the volume expansion of the silicon-carbon cathode material in the charge-discharge cycle process is effectively inhibited.
(2) The invention distributes the Si-CNT precursor in the artificial graphite uniformly through the high-temperature pyrolysis of the cane sugar, and the network structure formed by the one-dimensional material carbon nano-tube provides more channels for the electron transfer,
the internal resistance of the battery is reduced, and the electrical performance of the battery is improved.
(3) The binder in the cathode plate coating slurry is high-bonding water-based composite binder, and the water-based composite binder can be better contacted with the silicon-carbon powder through a network formed by ester bonds, so that the binding force between the silicon-carbon powder and other powder in the slurry and between the powder in the slurry and a metal foil is improved, the expansion of the silicon-carbon cathode plate is further reduced, and the cycle life of the battery is prolonged.
Drawings
FIG. 1 is a charge/discharge curve diagram of the discharge lamp obtained in example 2 of the present invention.
FIG. 2 is a graph comparing the cycle performance of the charging prepared in each example of the present invention and the comparative example.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
A preparation method of a low-expansion lithium battery silicon-carbon negative plate specifically comprises the following steps:
(1) Preparation of Si-CNT precursor: mixing porous nano silicon, a carbon nano tube and a dispersing agent according to a mass ratio of 94:5:1 (the dispersing agent is polyvinylpyrrolidone (PVP) and carboxymethylcellulose (CMC), the mass ratio of the PVP to the CMC is 0.2; wherein, the technological parameters of the spray drying are as follows: the liquid inlet amount is 50-60ml/min, the temperature of the air inlet is 260 ℃, the temperature of the air outlet is 180 ℃, and the blowing frequency is 25Hz;
(2) And (2) mixing the Si-CNT precursor prepared in the step (1), artificial graphite and sucrose according to a mass ratio of 5:90:5, putting the mixture into a ball mill for ball milling and mixing, vibrating and sieving to prepare uniform and compact Si-CNT/graphite/sucrose mixed powder; wherein the ball milling mixing speed is 1000r/min, the frequency of the vibrating screen is 15Hz, and the aperture of the screen mesh is 300 meshes;
(3) And preparing silicon-carbon powder: putting the Si-CNT/graphite/sucrose mixed powder into a tube furnace, introducing argon, starting to heat after 1 hour, wherein the argon flow is 100ml/min, the first-stage heating rate is 1 ℃/min, heating to 200 ℃, and keeping the temperature for 1 hour; in the second stage, the heating rate is 8 ℃/min, the temperature is raised to 1100 ℃, the temperature is kept for 5h, and finally, the silicon-carbon powder is obtained by cooling in the argon atmosphere, crushing and sieving;
(4) And preparing the low-expansion lithium battery silicon-carbon negative plate: and (3) mixing the silicon-carbon powder prepared in the step (3), the water-based composite binder, the graphene and the dispersing agent according to a mass ratio of 95:1:3:1, mixing and adding the mixture into a dispersion kettle containing pure water, and stirring at a high speed (revolution: 35rpm, dispersion: 4000 rpm) for 6 hours to obtain slurry; the viscosity of the slurry is 5000 +/-1000mPa.s, the solid content is 53 +/-1%, then the prepared slurry is coated on a copper foil according to the requirement of the practical surface density by spraying, double-sided coating is carried out after single-sided coating is finished, and then drying, rolling, slitting and laser cutting are sequentially carried out to prepare a silicon-carbon negative plate;
(5) And preparing a square battery: assembling the silicon-carbon negative plate prepared in the step (4) with a ternary 5-series positive plate to form a square battery of 50 Ah; wherein the electrolyte adopts standard test electrolyte 1molLiPF6+ EC + EMC + DEC, and the diaphragm is a gluing diaphragm.
And (3) detecting the thickness rebound rate of the silicon-carbon negative plate at different stages, and testing the thickness expansion rate of the battery by adopting a 1C/1C charge-discharge normal-temperature cycle performance test, wherein the charge-discharge voltage range is 2.8-4.2V.
Example 2
A preparation method of a low-expansion lithium battery silicon-carbon negative plate specifically comprises the following steps:
(1) Preparation of Si-CNT precursor: mixing porous nano silicon, a carbon nano tube and a dispersing agent according to a mass ratio of 90:9:1 (the dispersing agent is polyvinylpyrrolidone (PVP) and carboxymethylcellulose (CMC), the mass ratio of the PVP to the CMC is 0.2; wherein, the technological parameters of the spray drying are as follows: the liquid inlet amount is 50-60ml/min, the air inlet temperature is 260 ℃, the air outlet temperature is 180 ℃, and the blowing frequency is 25Hz.
And (3) preparing a square battery in the same steps (2) to (5) of the example 1, detecting the thickness rebound rate of the silicon-carbon negative plate at different stages, and testing the thickness expansion rate of the battery by adopting a 1C/1C charge-discharge normal-temperature cycle performance test, wherein the charge-discharge voltage range is 2.8-4.2V.
Example 3
A preparation method of a low-expansion lithium battery silicon-carbon negative plate comprises the following steps:
(1) Preparation of Si-CNT precursor: mixing porous nano silicon, a carbon nano tube and a dispersing agent according to a mass ratio of 94:5:1 (the dispersing agent is polyvinylpyrrolidone (PVP) and carboxymethylcellulose (CMC), the mass ratio of the PVP to the CMC is 0.2; wherein, the technological parameters of the spray drying are as follows: the liquid inlet amount is 50-60ml/min, the temperature of the air inlet is 260 ℃, the temperature of the air outlet is 180 ℃, and the blowing frequency is 25Hz;
(2) And (2) mixing the Si-CNT precursor prepared in the step (1), artificial graphite and sucrose according to a mass ratio of 10:85:5, putting the mixture into a ball mill for ball milling and mixing, and performing vibration sieving to prepare uniform and compact Si-CNT/graphite/sucrose mixed powder; wherein, the ball milling mixing speed is 1000r/min, the frequency of the vibrating screen is 15Hz, and the aperture of the screen mesh is 300 meshes;
and (5) preparing a square battery in the same steps as the steps (3) to (5) of the example 1, detecting the thickness rebound rate of the silicon-carbon negative plate at different stages, and testing the thickness expansion rate of the battery by adopting a 1C/1C charge-discharge normal-temperature cycle performance test, wherein the charge-discharge voltage range is 2.8-4.2V.
Comparative example 1
A preparation method of a silicon-carbon negative plate of a lithium battery specifically comprises the following steps:
(1) Firstly, mixing porous nano silicon, artificial graphite and cane sugar according to the mass ratio of 5:90:5, proportioning, putting into a ball mill for ball milling mixing, vibrating and sieving to obtain mixed powder; wherein the ball milling mixing speed is 1000r/min, the frequency of the vibrating screen is 15Hz, and the aperture of the screen mesh is 300 meshes;
(2) Placing the mixed powder into a tubular furnace, introducing argon, wherein the flow of the argon is 100ml/min, starting to heat up after 1 hour, heating up to 200 ℃ at the first-stage heating rate of 1 ℃/min, and keeping the temperature for 1 hour; and in the second stage, the heating rate is 8 ℃/min, the temperature is increased to 1100 ℃, the temperature is kept for 5h, and finally, the silicon-carbon powder is obtained by cooling in an argon atmosphere, crushing and sieving.
Then, according to the steps (4) and (5) of the embodiment 1, a square battery is prepared, the thickness rebound rate of the silicon-carbon negative plate at different stages is detected, a 1C/1C charge-discharge normal temperature cycle performance test is adopted, the charge-discharge voltage range is 2.8-4.2V, and the battery thickness expansion rate is tested.
Comparative example 2
A preparation method of a silicon-carbon negative plate of a lithium battery specifically comprises the following steps:
(1) Firstly, preparing silicon-carbon powder according to the steps (1) to (3) of the embodiment 1;
(2) And mixing silicon-carbon powder, graphene, styrene Butadiene Rubber (SBR) and a dispersing agent according to a mass ratio of 95:1:3:1, mixing and adding the mixture into a dispersion kettle containing pure water, and stirring at a high speed (revolution: 35rpm, dispersion: 4000 rpm) for 6 hours to obtain slurry; the viscosity of the slurry is 5000 +/-1000mPa.s, the solid content is 53 +/-1%, then the prepared slurry is coated on a copper foil according to the requirement of the practical surface density by spraying, double-sided coating is carried out after single-sided coating is finished, and then drying, rolling, slitting and laser cutting are sequentially carried out to prepare a silicon-carbon negative plate;
(3) And (3) preparing the square battery according to the step (5) of the embodiment 1, detecting the thickness rebound rate of the silicon-carbon negative plate at different stages, and testing the thickness expansion rate of the battery by adopting a 1C/1C charge-discharge normal-temperature cycle performance test, wherein the charge-discharge voltage range is 2.8-4.2V.
See table 1 below, comparative tables of basic properties of the silicon carbon powders prepared in examples 1 to 3 and comparative example 1.
TABLE 1 comparison table of basic performances of silicon-carbon negative electrode materials
As can be seen from the comparison in Table 1, the physical properties of the silicon carbon powder obtained in examples 1 to 3 are similar to those of the silicon carbon powder obtained in comparative example 1, and the addition of carbon nanotubes to the silicon carbon powder according to the present invention has a small influence on the physical properties of the silicon carbon powder.
See fig. 1, the charging and discharging curve chart of example 2. As can be seen from FIG. 2, the gram capacity of the silicon-carbon anode material prepared according to the embodiment 2 of the present invention is more than 450mAh/g.
See table 2 below, comparative table of cell cycle swelling for example 1-and comparative examples 1 and 2.
TABLE 2 comparison table of battery cycle thickness expansion
| Test example | Number of cycles | Swelling rate/%) |
| Example 1 | 500 | 3.6 |
| Example 2 | 500 | 2.3 |
| Example 3 | 500 | 2.9 |
| Comparative example 1 | 500 | 6.9 |
| Comparative example 2 | 500 | 8.5 |
As can be seen from comparison in Table 2, the batteries prepared in examples 1 to 3 according to the present invention exhibited a significantly lower rate of thickness expansion than those of comparative examples 1 to 2, when cycled for 500 weeks.
Referring to FIG. 2, a graph comparing the cycle performance of the charging prepared in examples 1 to 3 and comparative examples 1 and 2 is shown.
As can be seen from a comparison of fig. 2, the batteries manufactured in examples 1 to 3 according to the present invention have superior cycle performance to those of comparative examples 1 to 2. The low-expansion silicon-carbon negative plate can reduce the cycle thickness of the battery and reduce the internal cycle stress of the battery, thereby prolonging the cycle life of the battery.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A preparation method of a low-expansion lithium battery silicon-carbon negative plate is characterized by comprising the following steps: the method specifically comprises the following steps:
(1) Preparation of Si-CNT precursor: adding porous nano-silicon, a carbon nano-tube and a dispersing agent into deionized water according to a certain proportion, uniformly stirring, adding a citric acid solution, introducing the mixture solution into a sand mill for mixing and dispersing, introducing the mixed dispersion solution into a spray dryer, and preparing a Si-CNT precursor after spray drying; wherein, the ratio of porous nano silicon: carbon nanotube: the mass ratio of the dispersing agent is 85-95:3-15:0.2 to 1.3; the specific surface area of the porous nano silicon is 200-350m 2 Per g, pore volume of 0.3-0.5cm 3 Per g, the wall thickness is 5-100nm, and the pore diameter is 50-300nm; the length of the carbon nano tube is 20-100 mu m, and the tube diameter is 1-15nm; the dispersing agent is polyvinylpyrrolidone and carboxymethyl cellulose, and the mass ratio of the polyvinylpyrrolidone to the carboxymethyl cellulose is (0.1-0.3): 0.1-1.0;
(2) Ball-milling and mixing the Si-CNT precursor prepared in the step (1), artificial graphite and cane sugar in proportion, and vibrating and sieving to prepare uniform and compact Si-CNT/graphite/cane sugar mixed powder; wherein, si-CNT precursor: artificial graphite: the mass ratio of the sucrose is 1-15:70-90:5-20 parts of;
(3) And preparing silicon-carbon powder: sintering the Si-CNT/graphite/sucrose mixed powder prepared in the step (2) under the protective atmosphere of inert gas, cooling, taking out, crushing and sieving to obtain silicon-carbon powder; wherein, the technological parameters of sintering under the inert gas protective atmosphere are as follows: in the first stage, the heating rate is 0.5-2 ℃/min, the temperature is raised to 150-250 ℃, and the heat preservation time is 0.5-1h; in the second stage, the heating rate is 5-10 ℃/min, the temperature is increased to 1000-1200 ℃, and the heat preservation time is 1-10h;
(4) And preparing the low-expansion lithium battery silicon-carbon negative plate: and (3) mixing and dispersing the silicon-carbon powder prepared in the step (3), a water-based composite binder, graphene, a dispersing agent and pure water into slurry, wherein the water-based composite binder comprises polyacrylic acid and polyvinyl alcohol, the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 8.5.
2. The preparation method of the low-expansion lithium battery silicon-carbon negative electrode sheet according to claim 1, characterized in that: the spray drying process parameters in the step (1) are as follows: the liquid inlet amount is 50-100ml/min, the air inlet temperature is 200-300 ℃, the air outlet temperature is 150-200 ℃, and the blowing frequency is 20-30Hz.
3. The preparation method of the low-expansion lithium battery silicon-carbon negative electrode sheet according to claim 1, characterized in that: the mass ratio of the silicon-carbon powder, the aqueous composite binder, the graphene and the dispersing agent in the step (4) is 93-96:2.0-4.0:0.5-1.5:1.0-1.5.
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