CN109830668B - Method for preparing lithium ion battery silicon-carbon negative electrode material by adopting carbon nano tube - Google Patents
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Abstract
The invention discloses a method for preparing a silicon-carbon cathode material of a lithium ion battery by adopting carbon nano tubes, which comprises the steps of dispersing and fixing the carbon nano tubes and carbonizing precursors; the carbon nano tubes are cut short and dispersed by high-speed emulsification and shearing, and the dispersing agent enables the carbon nano tubes to keep a highly dispersed state, so that the problems of difficult dispersion and easy agglomeration of the carbon nano tubes are solved; through freeze drying, the highly dispersed carbon nano tube/nano silicon is fixed by the organic carbon source, and the carbon coating is formed on the carbon nano tube/nano silicon after the organic carbon source is carbonized, so that the aim of efficiently preparing the lithium ion silicon carbon cathode material from the carbon nano tube is fulfilled.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery cathode materials, and particularly relates to a method for preparing a lithium ion battery silicon-carbon cathode material by adopting carbon nanotubes.
Background
In order to meet the increasing demands of new energy automobiles, portable equipment and the like on the capacity and energy density of the lithium ion battery, the carbon-silicon negative electrode material becomes one of the leading development directions leading to the future lithium ion battery negative electrode material. The development of carbon-silicon cathode materials is utilizing the ultrahigh theoretical capacity and low lithium intercalation potential of silicon, and the silicon is rich in resources and environment-friendly. However, the silicon material itself has significant disadvantages, such as poor conductivity, poor cyclability, and high expansion rate; the current research generally adopts a carbon-silicon compounding method to draw attention to and avoid harm, but the problems of uniformity problem, fast capacity attenuation, poor rate capability and complex preparation method of silicon-carbon compounding are not overcome.
The carbon nanotube can effectively solve the above problems; the carbon nano tube is a one-dimensional nano material, the radial dimension is nano magnitude, the axial dimension is micron magnitude, the carbon nano tube can be regarded as formed by curling a graphene sheet layer and is an excellent conductor of lithium ions and electrons, the lithium ions and the electrons reach silicon particles through the carbon tube to be inserted and separated, and the silicon can exert the advantages to the greatest extent; however, the carbon nanotubes are easy to agglomerate and entangle, so that the key problem of how to uniformly disperse and fix the carbon nanotubes in the silicon-carbon cathode material is to solve the high-efficiency application of the carbon nanotubes to play the excellent performance of the carbon nanotubes.
Disclosure of Invention
The invention provides a method for preparing a silicon-carbon cathode material of a lithium ion battery by adopting carbon nano tubes, which reduces the axial size of the carbon nano tubes through high-speed shearing, fully emulsifies a mixed solution containing nano silicon and a dispersing agent while shearing, the nano silicon and the dispersing agent are fully distributed around the sheared carbon nano tubes to effectively inhibit the reunion of the carbon nano tubes, an organic carbon source is added to form a porous structure through freeze drying, the high dispersion state of the carbon nano tubes is kept, and porous carbon formed through vacuum carbonization provides a buffer framework for the volume expansion of silicon particles in the electrochemical circulation process.
The invention discloses a method for preparing a silicon-carbon cathode material of a lithium ion battery by adopting a carbon nano tube, which comprises the following steps:
(1) uniformly mixing silicon powder, a carbon nano tube and a dispersing agent with deionized water, and shearing the mixture with a high-speed shearing machine to obtain a mixed solution, wherein the mass ratio of the silicon powder to the carbon nano tube to the dispersing agent is 1 (0.1-1) to 0.1-1, and the mass volume g: mL of a solid substance to the deionized water is 1: 50-100;
the particle size of the silicon powder is 30 nm-1 mu m;
the carbon nano tube is one or more of a single-walled carbon nano tube and a multi-walled carbon nano tube in any ratio, and the tube diameter of the carbon nano tube is 0.2-100 nm;
the dispersing agent is one or more of polyvinylpyrrolidone, maleic anhydride and styrene in any ratio;
the uniformly mixing mode is one or more of mechanical stirring, magnetic stirring and ultrasonic vibration;
the shearing speed of the high-speed shearing machine is 3000-8000 r/min, and the shearing time is 1-3 h.
(2) Dissolving an organic carbon source in deionized water, uniformly mixing with the mixed solution obtained in the step (1), and stirring the uniformly mixed solution in a water bath condition, wherein the mass ratio of the organic carbon source to the deionized water is 1: 2-10;
the organic carbon source is one or more of sucrose, citric acid, ascorbic acid and glucose; the mass ratio of the organic carbon source to the silicon powder is 1: 0.5-5; the mixing mode is one or more of mechanical stirring, magnetic stirring and ultrasonic vibration;
stirring for 2-8 h at 60-80 ℃ under the water bath condition; the stirring mode is mechanical stirring or magnetic stirring.
(3) Freezing and drying the mixed solution obtained in the step (2) to obtain a solid mixture, and carbonizing the solid mixture under a vacuum condition to obtain the carbon nano tube/silicon carbon negative electrode material;
the freeze drying condition is that the thickness of the mixed solution is 5-10 mm; the temperature of the cold trap coil is-50 to-80 ℃; the ultimate vacuum degree is 1-20 Pa; the freezing time is 24-48 h;
the carbonization treatment under the vacuum condition is carried out under the condition that the vacuum degree is 15-50 Pa, the temperature is increased to 100-150 ℃ at the temperature increase rate of 2-10 ℃/min and is kept for 1-10 h, and then the temperature is increased to 500-900 ℃ at the temperature increase rate of 0.1-5 ℃/min and is kept for 1-10 h.
Compared with the prior art, the invention has the advantages that: the invention adopts a high-speed shearing machine to shear short the carbon nano tube, adds a dispersing agent to disperse the carbon nano tube, adds an organic carbon source to freeze the carbon nano tube and then fixes the carbon nano tube in a dispersed state. The porous carbon formed after vacuum carbonization provides a stable buffer skeleton. The carbon nano tube penetrates through the composite material particles to provide a good conductive path; an amorphous porous carbon skeleton formed by an organic carbon source provides a buffer space for the expansion of silicon, and the problems of multiplying power and cyclicity of the silicon-carbon composite material are respectively solved. The main raw materials of the invention are green, environment-friendly and renewable, the operation is simple and easy, the requirements on equipment are low, the energy consumption is low, and the invention can be used for large-scale production.
Drawings
FIG. 1 is a transmission electron micrograph of an uncut carbon nanotube;
FIG. 2 is a transmission electron micrograph of sheared carbon nanotubes/silicon particles;
FIG. 3 is a transmission electron micrograph of sheared and freeze-dried carbon nanotube/silicon particles;
FIG. 4 is a transmission electron micrograph of sheared carbon nanotube/silicon particles that were not freeze dried.
FIG. 5 is a graph of electrochemical cycling for the silicon/carbon composite obtained by shear freeze drying and the silicon/carbon composite obtained by shear forced air drying in example 1;
FIG. 6 is a graph of electrochemical rate of silicon/carbon composite obtained by shear freeze drying and shear forced air drying in example 2;
fig. 7 is a graph showing electrochemical rate curves exhibited by the silicon-carbon composites obtained in examples 3, 4, 5, and 6.
Detailed Description
The invention will be further described with reference to the following figures and examples, but the scope of the invention is not limited thereto.
Example 1: the method for preparing the silicon-carbon cathode material of the lithium ion battery by adopting the carbon nano tube comprises the following steps:
(1) weighing silicon powder (the particle size of the silicon powder is 40 nm), a multi-walled carbon nanotube (the pipe diameter is 20 nm) and polyvinylpyrrolidone according to the mass ratio of silicon powder to multi-walled carbon nanotube to polyvinylpyrrolidone =1:0.1:0.1, placing the silicon powder, the multi-walled carbon nanotube (the pipe diameter is 20 nm) and the polyvinylpyrrolidone in a same beaker, magnetically stirring and dissolving the silicon powder, the multi-walled carbon nanotube and the polyvinylpyrrolidone in water according to the mass-volume ratio of g to mL of 1:50, and shearing the mixture for 1h at a shearing speed of 8000r/min by using a high-speed shearing machine to obtain a mixed solution;
(2) weighing sucrose according to the mass ratio of 1:0.5 of sucrose to silicon powder, dissolving the sucrose in water according to the mass ratio of 1:2, uniformly stirring, adding the mixture into the mixed solution obtained in the step (1), uniformly stirring by magnetic force, and placing the uniformly mixed solution in a water bath kettle at 80 ℃ for magnetic stirring for 2 hours;
(3) freezing the mixed solution (with the thickness of 5 mm) subjected to the water bath treatment in the step (2) for 24 hours under the conditions that the temperature of a cold trap coil is-50 ℃ and the ultimate vacuum degree is 20 Pa; the treated product is carbonized in vacuum, and the specific process comprises the following steps: the vacuum degree is 15Pa, the temperature is raised to 120 ℃ at the heating rate of 2 ℃/min, the temperature is preserved for 5h for pre-carbonization, then the temperature is raised to 500 ℃ at the heating rate of 1 ℃/min, the temperature is preserved for carbonization for 9h, and the carbon-silicon cathode material of the lithium ion battery is obtained.
FIG. 1 is a transmission electron microscope image of an untreated carbon nanotube, from which it can be seen that the agglomeration phenomenon of the untreated carbon nanotube is serious, and the untreated carbon nanotube hardly exerts its excellent performance; FIG. 2 is a transmission electron microscope image of sheared carbon nanotubes/silicon particles, wherein the sheared carbon nanotubes are axially shortened, and silicon nanoparticles are attached to the periphery of the sheared carbon nanotubes, so that the conductivity of the composite material can be greatly improved; FIG. 3 is a transmission electron micrograph of sheared and freeze-dried carbon nanotubes/silicon particles, where it can be observed that the outermost walls of the multiwall carbon nanotubes are ruptured, the inner walls remain tubular, and the ruptured outer walls unfold into a graphene-like structure, thereby increasing the contact between the non-conductive silicon particles and the carbon nanotubes; the carbon nanotube/silicon particle solution without freeze-drying has no such phenomenon as shown in FIG. 4; as can be seen from the electrochemical performance diagram of FIG. 5, the performance of the carbon nanotube/silicon carbon anode material subjected to the shearing and freeze-drying treatment is greatly improved.
Example 2: the method for preparing the silicon-carbon cathode material of the lithium ion battery by adopting the carbon nano tube comprises the following steps:
(1) weighing silicon powder (the particle size of the silicon powder is 60 nm), a multi-walled carbon nanotube (the pipe diameter is 25 nm) and polyvinylpyrrolidone according to the mass ratio of the silicon powder to the multi-walled carbon nanotube to the polyvinylpyrrolidone =1:0.2:0.5, placing the silicon powder, the multi-walled carbon nanotube (the pipe diameter is 25 nm) and the polyvinylpyrrolidone into a same beaker, mechanically stirring and dissolving the silicon powder, the multi-walled carbon nanotube and the polyvinylpyrrolidone into water according to the mass-volume ratio of g: mL of 1:70, and shearing the mixture for 2 hours by using a high-speed shearing machine at the shearing speed of 5000r/min to obtain a mixed solution;
(2) weighing sucrose according to the mass ratio of 1:2 of sucrose to silicon powder, dissolving the sucrose in water according to the mass ratio of 1:5, mechanically stirring and uniformly mixing, then adding the mixture in the step (1), magnetically stirring and uniformly mixing, and placing the uniformly mixed solution in a 70 ℃ water bath kettle for magnetic stirring for 5 hours;
(3) freezing the mixed solution (with the thickness of 8 mm) subjected to the water bath treatment in the step (2) for 35 hours under the conditions that the temperature of a cold trap coil is-65 ℃ and the ultimate vacuum degree is 10 Pa; the treated product is carbonized in vacuum, and the specific process comprises the following steps: the vacuum degree is 30Pa, the temperature is raised to 100 ℃ at the heating rate of 5 ℃/min and is preserved for 10h for pre-carbonization, then the temperature is raised to 650 ℃ at the heating rate of 3 ℃/min, and the temperature is preserved for carbonization for 5h, so as to obtain the carbon-silicon cathode material of the lithium ion battery.
FIG. 6 is an electrochemical rate curve of the composite obtained in example 2; the graph shows that the capacity and the rate of the composite material after freeze drying are improved, so that the graphene structure is formed by cracking of a plurality of layers of pipe walls at the periphery of the multi-wall carbon nano tube in the freeze drying process, the contact between the carbon nano tube and the nano silicon particles is increased, and the rate of the silicon-carbon composite material is improved.
Example 3: the method for preparing the silicon-carbon cathode material of the lithium ion battery by adopting the carbon nano tube comprises the following steps:
(1) weighing silicon powder, multi-walled carbon nanotubes, polyvinylpyrrolidone (the particle size of the silicon powder is 80 nm), multi-walled carbon nanotubes (the pipe diameter of the silicon powder is 30 nm) and polyvinylpyrrolidone (the pipe diameter of the silicon powder is 30 nm) according to the mass ratio of the silicon powder to the multi-walled carbon nanotubes to the polyvinylpyrrolidone is =1:1:1, placing the silicon powder to the multi-walled carbon nanotubes to the polyvinylpyrrolidone in the same beaker, dissolving the silicon powder to the multiwalled carbon nanotubes to the polyvinylpyrrolidone in water according to the mass-volume ratio of g to mL of 1:95, and shearing the mixture for 3 hours at the shearing speed of 3000r/min by using a high-speed shearing machine to obtain a mixed solution;
(2) weighing sucrose according to the mass ratio of 1:5 of sucrose to silicon powder, dissolving the sucrose in water according to the mass ratio of 1:10, uniformly mixing by magnetic stirring, adding the mixture into the mixed solution obtained in the step (1), mechanically stirring and uniformly mixing, and placing the uniformly mixed solution in a 60 ℃ water bath kettle for magnetic stirring for 8 hours;
(3) freezing the mixed solution (with the thickness of 10 mm) subjected to the water bath treatment in the step (2) for 45 hours under the conditions that the temperature of a cold trap coil is-80 ℃ and the ultimate vacuum degree is 2 Pa; the treated product is carbonized in vacuum, and the specific process comprises the following steps: the vacuum degree is 45Pa, the temperature is raised to 150 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1.5h for pre-carbonization, then the temperature is raised to 900 ℃ at the heating rate of 5 ℃/min, the temperature is kept for carbonization for 1h, the carbon-silicon cathode material of the lithium ion battery is obtained, and the electrochemical multiplying power performance of the obtained composite material is shown in figure 7.
Example 4 the method for preparing the silicon-carbon cathode material of the lithium ion battery by adopting the carbon nano tube comprises the following steps
(1) Weighing silicon powder (the particle size of the silicon powder is 100 nm), a single-walled carbon nanotube (the pipe diameter is 40 nm) and maleic anhydride according to the mass ratio of the silicon powder to the single-walled carbon nanotube to maleic anhydride =1:0.5:0.4, placing the silicon powder, the single-walled carbon nanotube (the pipe diameter is 40 nm) and the maleic anhydride in the same beaker, dissolving the mixture in water according to the mass-volume ratio g: mL of 1:80 by ultrasonic oscillation, and shearing the mixture for 2.5 hours at the shearing speed of 4000r/min by using a high-speed shearing machine to obtain a mixed solution;
(2) weighing glucose according to the mass ratio of the glucose to the silicon powder of 1:1, dissolving the glucose in water according to the mass ratio of 1:7, uniformly mixing by ultrasonic oscillation, adding the obtained solution into the mixed solution obtained in the step (1), uniformly stirring by magnetic force, and placing the uniformly mixed solution in a 65 ℃ water bath kettle for magnetic stirring for 6 hours;
(3) freezing the mixed solution (with the thickness of 6 mm) subjected to the water bath treatment in the step (2) for 40h under the conditions that the temperature of a cold trap coil is-60 ℃ and the ultimate vacuum degree is 5 Pa; the treated product is carbonized in vacuum, and the specific process comprises the following steps: the vacuum degree is 40Pa, the temperature is raised to 110 ℃ at the heating rate of 7 ℃/min and is preserved for 8h for pre-carbonization, then the temperature is raised to 850 ℃ at the heating rate of 0.5 ℃/min, and the temperature is preserved for carbonization for 3h, so as to obtain the carbon-silicon cathode material of the lithium ion battery; the electrochemical rate results of the carbon-silicon negative electrode material of the lithium ion battery are shown in fig. 7.
Example 5: the method for preparing the silicon-carbon cathode material of the lithium ion battery by adopting the carbon nano tube comprises the following steps
(1) Weighing silicon powder (the particle size of the silicon powder is 100 nm), a single-walled carbon nanotube (the pipe diameter is 50 nm) and maleic anhydride according to the mass ratio of the silicon powder to the single-walled carbon nanotube to styrene =1:0.7:0.2, placing the silicon powder, the single-walled carbon nanotube (the pipe diameter is 50 nm) and the maleic anhydride into the same beaker, dissolving the mixture in water according to the mass-volume ratio g: mL of 1:75 by ultrasonic oscillation, and shearing the mixture for 1.5h at the shearing speed of 6500r/min by using a high-speed shearing machine to obtain a mixed solution;
(2) weighing citric acid according to the mass ratio of 1:2 of citric acid to silicon powder, dissolving the citric acid in water according to the mass ratio of 1:9, uniformly mixing by ultrasonic oscillation, adding the mixture into the mixed solution obtained in the step (1), uniformly stirring by magnetic force, and placing the uniformly mixed solution in a 75 ℃ water bath kettle for magnetic stirring for 4 hours;
(3) freezing the mixed solution (with the thickness of 7 mm) subjected to the water bath treatment in the step (2) for 35 hours under the conditions that the temperature of a cold trap coil is-70 ℃ and the ultimate vacuum degree is 8 Pa; the treated product is carbonized in vacuum, and the specific process comprises the following steps: the vacuum degree is 25Pa, the temperature is raised to 140 ℃ at the heating rate of 3 ℃/min and is preserved for 3h for pre-carbonization, then the temperature is raised to 750 ℃ at the heating rate of 2 ℃/min, and the temperature is preserved for carbonization for 5h, so as to obtain the carbon-silicon cathode material of the lithium ion battery; the electrochemical rate results of the carbon-silicon negative electrode material of the lithium ion battery are shown in fig. 7.
Example 6: the method for preparing the silicon-carbon cathode material of the lithium ion battery by adopting the carbon nano tube comprises the following steps
(1) Weighing silicon powder (the particle size of the silicon powder is 1 mu m), a single-walled carbon nanotube (the pipe diameter is 100 nm) and polyvinylpyrrolidone according to the mass ratio of silicon powder to single-walled carbon nanotube to polyvinylpyrrolidone =1:0.7:0.2, placing the silicon powder, the single-walled carbon nanotube and the polyvinylpyrrolidone into the same beaker, ultrasonically vibrating and dissolving the silicon powder, the single-walled carbon nanotube and the polyvinylpyrrolidone into water according to the mass-volume ratio of g: mL of 1:85, and shearing the mixture for 1h at the shearing speed of 7500r/min by using a high-speed shearing machine to obtain a mixed solution;
(2) weighing ascorbic acid according to the mass ratio of 1:4 of ascorbic acid to silicon powder, dissolving the ascorbic acid in water according to the mass ratio of 1:7, uniformly mixing by ultrasonic oscillation, adding the ascorbic acid into the mixed solution obtained in the step (1), uniformly stirring by magnetic force, and placing the uniformly mixed solution in a 60 ℃ water bath kettle for magnetic stirring for 7 hours;
(3) freezing the mixed solution (with the thickness of 9 mm) subjected to the water bath treatment in the step (2) for 45 hours under the conditions that the temperature of a cold trap coil is-75 ℃ and the ultimate vacuum degree is 2 Pa; the treated product is carbonized in vacuum, and the specific process comprises the following steps: the vacuum degree is 35Pa, the temperature is raised to 130 ℃ at the heating rate of 7 ℃/min and is preserved for 5h for pre-carbonization, then the temperature is raised to 550 ℃ at the heating rate of 3 ℃/min, and the temperature is preserved for carbonization for 9h, so as to obtain the carbon-silicon cathode material of the lithium ion battery; the electrochemical rate results of the carbon-silicon negative electrode material of the lithium ion battery are shown in fig. 7.
Claims (4)
1. A method for preparing a silicon-carbon cathode material of a lithium ion battery by adopting a carbon nano tube is characterized by comprising the following steps:
(1) uniformly mixing silicon powder, a carbon nano tube and a dispersing agent with deionized water, and shearing the mixture with a high-speed shearing machine to obtain a mixed solution, wherein the mass ratio of the silicon powder to the carbon nano tube to the dispersing agent is 1 (0.1-1) to 0.1-1, and the mass volume ratio g to mL of a solid substance to the deionized water is 1: 50-100;
(2) dissolving an organic carbon source in deionized water, uniformly mixing with the mixed solution obtained in the step (1), and stirring the uniformly mixed solution in a water bath condition, wherein the mass ratio of the organic carbon source to the deionized water is 1: 2-10;
(3) freezing and drying the mixed solution obtained in the step (2) to obtain a solid mixture, and carbonizing the solid mixture under a vacuum condition to obtain the carbon nano tube/silicon carbon negative electrode material;
the particle size of the silicon powder is 30 nm-1 mu m;
the dispersing agent is one or more of polyvinylpyrrolidone, maleic anhydride and styrene in any ratio;
the carbon nano tube is a multi-wall carbon nano tube, and the diameter of the carbon nano tube is 0.2-100 nm;
the shearing speed of the high-speed shearing machine is 3000-8000 r/min, and the shearing time is 1-3 h;
the freeze drying condition is that the thickness of the mixed solution is 5-10 mm; the temperature of the cold trap coil is-50 to-80 ℃; the ultimate vacuum degree is 1-20 Pa; the freezing time is 24-48 h.
2. The method for preparing the silicon-carbon anode material of the lithium ion battery by adopting the carbon nano tube as claimed in claim 1, is characterized in that: the organic carbon source is one or more of sucrose, citric acid, ascorbic acid and glucose; the mass ratio of the organic carbon source to the silicon powder is 1: 0.5-5.
3. The method for preparing the silicon-carbon anode material of the lithium ion battery by adopting the carbon nano tube as claimed in claim 1, is characterized in that: stirring for 2-8 h at 60-80 ℃ under the water bath condition; the stirring mode is mechanical stirring or magnetic stirring.
4. The method for preparing the silicon-carbon anode material of the lithium ion battery by adopting the carbon nano tube as claimed in claim 1, is characterized in that: the carbonization treatment under the vacuum condition is carried out under the condition that the vacuum degree is 15-50 Pa, the temperature is increased to 100-150 ℃ at the temperature increase rate of 2-10 ℃/min and is kept for 1-10 h, and then the temperature is increased to 500-900 ℃ at the temperature increase rate of 0.1-5 ℃/min and is kept for 1-10 h.
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| TWI830935B (en) * | 2020-07-24 | 2024-02-01 | 芯量科技股份有限公司 | Manufacturing method of multi-layered long-cycle silicon carbon anode material |
| CN112117457B (en) * | 2020-09-18 | 2021-07-30 | 昆明理工大学 | Preparation method of carbon nano tube doped tubular tin oxalate negative electrode material |
| CN112952059A (en) * | 2021-02-09 | 2021-06-11 | 昆山宝创新能源科技有限公司 | Silicon-based negative electrode material and preparation method and application thereof |
| CN113036146B (en) * | 2021-03-10 | 2022-06-28 | 哈尔滨万鑫石墨谷科技有限公司 | Carbon nano tube conductive slurry and preparation method and application thereof |
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