CN113417069A - Method for preparing silicon cathode material based on electrostatic spinning technology and application thereof - Google Patents
Method for preparing silicon cathode material based on electrostatic spinning technology and application thereof Download PDFInfo
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- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention discloses a method for preparing a silicon cathode material based on an electrostatic spinning technology and application thereof, wherein the preparation method comprises the following steps: (1) mixing deionized water and absolute ethyl alcohol as solvents, an organic silicon source and an organic carbon source as solutes, and adjusting the pH value of the solution to form transparent sol; (2) uniformly mixing the spinning solution and the prepared transparent sol, and preparing a fiber membrane by using an electrostatic spinning machine; (3) putting the fiber membrane into a drying box for drying; (4) and placing the dried fiber membrane in an argon protection environment for heat treatment to obtain the silicon negative electrode material. The method can improve the dispersity and the cladding property of the silicon-based particles in the carbon-based conductive network, thereby improving the electrochemical performance of the silicon-based material.
Description
Technical Field
The invention relates to the technical field of new energy materials, in particular to a method for preparing a silicon cathode material based on an electrostatic spinning technology and application thereof.
Background
The theoretical specific mass capacity of the silicon material is 4200 mAh/g, which is more than 10 times of that of the traditional graphite material, so that the silicon material is concerned, is considered to possibly replace the traditional graphite electrode and becomes the next generation of high-energy density lithium ion battery cathode material. However, there are many difficulties to be solved in the commercial application of silicon anode materials. The silicon negative electrode material has a serious volume expansion effect in the processes of lithium intercalation and lithium deintercalation, the generated stress can lead active substances to be pulverized and fall off from a current collector, and the service life of the lithium ion battery is seriously influenced by the problems. The SEI film is repeatedly broken and regenerated due to the constant change in the volume of the negative electrode material, consuming the electrolyte, and attenuating the capacity. These problems have all been obstacles to practical application of silicon-based materials.
Among the existing solutions, carbon coating technology is the most common method for optimizing the electrical conductivity and relieving the volume expansion of silicon-based materials. However, in the coating process, since the nano-sized silicon particles have a small particle size, the nano-sized silicon particles are difficult to be uniformly dispersed in the carbon substrate and are easily agglomerated, resulting in a decrease in the overall electrochemical performance.
Disclosure of Invention
The invention aims to provide a method for preparing a silicon cathode material by using an organic silicon source and an electrostatic spinning technology, aiming at the defects of the prior art, the method can enable the sub-silicon particles to grow out in situ in carbon nanofibers, has a uniform dispersion effect and a good coating effect, and can obviously improve the electrochemical performance of a lithium ion battery when being used as a lithium ion battery cathode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a silicon cathode material based on an electrostatic spinning technology comprises the following steps:
(1) deionized water and absolute ethyl alcohol are mixed according to a mass ratio of 1: 1-1: 2 is prepared into a solvent, and the mass ratio of the organic silicon source to the organic carbon source is 1: 0.5-1: 2 is mixed into a solute, and the pH value of the solution is adjusted within the range of 2-6 to form transparent sol;
(2) uniformly mixing the spinning solution and the prepared transparent sol, and preparing a fiber membrane by using an electrostatic spinning machine;
(3) putting the fiber membrane into a drying box for drying;
(4) and placing the dried fiber membrane in an argon protection environment for heat treatment to obtain the silicon negative electrode material.
The organic silicon source in the step (1) is preferably ethyl orthosilicate.
The organic carbon source in the step (1) is preferably glucose or sucrose or citric acid or phenolic resin.
And (2) adjusting the pH value of the solution in the step (1), wherein the acidic solution for adjusting the pH value is HCL or H2O2 or glacial acetic acid, and the alkaline solution is ammonia water.
The preparation method of the spinning solution in the step (2) comprises the following steps: the composite material is prepared by mixing polyvinylpyrrolidone or polyacrylonitrile as a solute and deionized water and absolute ethyl alcohol as solvents according to the mass ratio of 1:2: 4.
In the step (2), the fiber membrane is obtained by using an electrostatic spinning machine, and various parameters of the electrostatic spinning machine are set as follows: the electrostatic spinning machine has positive voltage of 10-15KV, negative voltage of 0-5KV, injection speed of 0.2-0.5mm/min, and spinning temperature of 30-40 deg.C.
And (4) drying the fiber membrane in the drying oven in the step (3), wherein the drying temperature is 90 ℃, and the drying time is 24 hours.
The heat treatment process in the step (4) comprises the following steps: the fiber membrane is placed in a tube furnace filled with argon, the temperature is raised to 700-1200 ℃, and the temperature is kept for 60-120 min.
The silicon negative electrode material, conductive carbon black and sodium alginate are mixed to prepare slurry, and the slurry is subjected to coating, drying, tabletting, slicing and weighing to prepare a silicon negative electrode sheet, wherein the prepared silicon negative electrode sheet is used for manufacturing a button cell.
The silicon negative electrode material, the conductive carbon black and the sodium alginate are prepared from the following components in parts by weight: 75 parts of silicon negative electrode material, 15 parts of conductive carbon black and 15 parts of sodium alginate.
The invention has the beneficial effects that:
(1) the heat treatment process of the method can lead the nano-sized silicon particles to grow out in situ in the carbon substrate and be uniformly distributed in the carbon substrate;
(2) according to the silicon cathode material prepared by the method, the conductive network is composed of the carbon nanofibers, so that the overall conductivity of the electrode material is improved;
(3) the preparation method of the silicon cathode material has less powder generated in the preparation process and is environment-friendly.
Detailed Description
The present invention will be further described in detail with reference to several specific examples, but the following examples are only illustrative and not intended to limit the scope of the present invention, which is defined by the claims.
A method for preparing a silicon cathode material based on an electrostatic spinning technology comprises the following steps:
(1) deionized water and absolute ethyl alcohol are mixed according to a mass ratio of 1: 1-1: 2 is prepared into a solvent, and the mass ratio of the organic silicon source to the organic carbon source is 1: 0.5-1: 2 is mixed into a solute, and the pH value of the solution is adjusted within the range of 2-6 to form transparent sol;
(2) uniformly mixing the spinning solution and the prepared transparent sol, and preparing a fiber membrane by using an electrostatic spinning machine;
(3) putting the fiber membrane into a drying box for drying;
(4) and placing the dried fiber membrane in an argon protection environment for heat treatment to obtain the silicon negative electrode material.
The organic silicon source in the step (1) is preferably ethyl orthosilicate.
The organic carbon source in the step (1) is preferably glucose or sucrose or citric acid or phenolic resin.
And (2) adjusting the pH value of the solution in the step (1), wherein the acidic solution for adjusting the pH value is HCL or H2O2 or glacial acetic acid, and the alkaline solution is ammonia water.
The preparation method of the spinning solution in the step (2) comprises the following steps: the composite material is prepared by mixing polyvinylpyrrolidone or polyacrylonitrile as a solute and deionized water and absolute ethyl alcohol as solvents according to the mass ratio of 1:2: 4.
In the step (2), the fiber membrane is obtained by using an electrostatic spinning machine, and various parameters of the electrostatic spinning machine are set as follows: the electrostatic spinning machine has positive voltage of 10-15KV, negative voltage of 0-5KV, injection speed of 0.2-0.5mm/min, and spinning temperature of 30-40 deg.C.
And (4) drying the fiber membrane in the drying oven in the step (3), wherein the drying temperature is 90 ℃, and the drying time is 24 hours.
The heat treatment process in the step (4) comprises the following steps: the fiber membrane is placed in a tube furnace filled with argon, the temperature is raised to 700-1200 ℃, and the temperature is kept for 60-120 min.
The silicon negative electrode material, conductive carbon black and sodium alginate are mixed to prepare slurry, and the slurry is subjected to coating, drying, tabletting, slicing and weighing to prepare a silicon negative electrode sheet, wherein the prepared silicon negative electrode sheet is used for manufacturing a button cell.
The silicon negative electrode material, the conductive carbon black and the sodium alginate are prepared from the following components in parts by weight: 75 parts of silicon negative electrode material, 15 parts of conductive carbon black and 15 parts of sodium alginate.
Example 1
A method for preparing a silicon cathode material based on an electrostatic spinning technology comprises the following steps:
(1) preparing sucrose, deionized water and glacial acetic acid into a mixed solution according to the mass ratio of 1:8:1, and uniformly stirring;
(2) sequentially adding absolute ethyl alcohol and tetraethoxysilane into the solution according to the mass ratio of 3:1, and stirring for 3 hours to form a transparent solution;
(3) adding 2g of polyvinylpyrrolidone into the transparent solution, and stirring for 1h to form colloidal liquid;
(4) putting the colloidal liquid into an electrostatic spinning machine, setting the positive voltage of the spinning machine to be 15KV, the negative voltage to be 1.5KV, the injection speed to be 0.25 mm/min and the spinning temperature to be 30 ℃ to prepare a fiber membrane;
(5) putting the fiber membrane into a drying oven for drying, wherein the drying temperature is 50 ℃, and the drying time is 24 hours;
(6) and (3) placing the dried fiber membrane in a tubular furnace under the protection of argon, heating to 1000 ℃, and carrying out heat treatment for 120 min.
Mixing the silicon negative electrode material prepared by the method, conductive carbon black and sodium alginate according to the weight ratio of 75: 15: 15 to prepare slurry, coating, drying, tabletting, slicing, weighing and the like to prepare the silicon negative plate, and using the prepared silicon negative plate to prepare the button cell.
And (3) performing a power-on test on the button cell: the button cell battery has the specific capacity still stabilized at 600mAh/g after 0.5C circulation for 200 weeks.
Example 2
A method for preparing a silicon cathode material based on an electrostatic spinning technology comprises the following steps:
(1) preparing phenolic resin, deionized water and glacial acetic acid into a mixed solution according to the mass ratio of 1:8:1, and uniformly stirring;
(2) sequentially adding absolute ethyl alcohol and tetraethoxysilane into the solution according to the mass ratio of 3:1, stirring for 3 hours to form a transparent solution, and stirring for 3 hours to form a transparent solution;
(3) adding 2g of polyvinylpyrrolidone into the transparent solution, and stirring for 1h to form colloidal liquid;
(4) putting the colloidal liquid into an electrostatic spinning machine, setting the positive voltage of the spinning machine to be 15KV, the negative voltage to be 1.5KV, the injection speed to be 0.25 mm/min and the spinning temperature to be 30 ℃ to prepare a fiber membrane;
(5) putting the fiber membrane into a drying oven for drying, wherein the drying temperature is 50 ℃, and the drying time is 24 hours;
(6) and (3) placing the dried fiber membrane in a tubular furnace under the protection of argon, heating to 1000 ℃, and carrying out heat treatment for 120 min.
Mixing the silicon negative electrode material prepared by the method, conductive carbon black and sodium alginate according to the weight ratio of 75: 15: 15 to prepare slurry, coating, drying, tabletting, slicing, weighing and the like to prepare the silicon negative plate, and using the prepared silicon negative plate to prepare the button cell.
And (3) performing a power-on test on the button cell: the button cell battery has the specific capacity still stabilized at 650mAh/g after 0.5C circulation for 200 weeks.
Example 3
A method for preparing a silicon cathode material based on an electrostatic spinning technology comprises the following steps:
(1) mixing ethyl orthosilicate and absolute ethyl alcohol according to a mass ratio of 1: 3, uniformly mixing to prepare a solution A;
(2) dissolving glucose in a mixed solution prepared from deionized water and hydrogen peroxide (the mass ratio of the glucose to the deionized water to the hydrogen peroxide is 0.5:4: 0.5), and adjusting the pH of the solution to be =2 by using HCl to obtain a solution B;
(3) adding the solution B into the solution A to form a transparent solution;
(4) adding 2g of polyvinylpyrrolidone into the transparent solution, and stirring for 1h in a water bath kettle at 40 ℃ to form transparent sol;
(5) putting the colloidal liquid into an electrostatic spinning machine, setting the positive voltage of the spinning machine to be 12KV, the negative voltage to be 1KV, the injection speed to be 0.25 mm/min and the spinning temperature to be 40 ℃ to prepare a fiber membrane;
(6) putting the fiber membrane into a drying oven for drying, wherein the drying temperature is 50 ℃, and the drying time is 24 hours;
(7) placing the dried fiber membrane in a tubular furnace under the protection of argon, heating to 1200 ℃, and carrying out heat treatment for 120 min;
mixing the silicon negative electrode material prepared by the method, conductive carbon black and sodium alginate according to the weight ratio of 75: 15: 15 to prepare slurry, coating, drying, tabletting, slicing, weighing and the like to prepare the silicon negative plate, and using the prepared silicon negative plate to prepare the button cell.
And (3) performing a power-on test on the button cell: the button cell battery has the specific capacity still stabilized at 800 mAh/g after 0.5C circulation for 200 weeks.
In conclusion, the heat treatment process of the fiber membrane in the method can enable nano-sized silicon particles to grow out in situ in the carbon substrate and be uniformly distributed in the carbon substrate, the conductive network of the prepared silicon negative electrode material consists of carbon nano-fibers, the overall conductivity of the electrode material is improved, and meanwhile, compared with the button cell using a graphite material to prepare a negative electrode plate, the button cell prepared from the silicon negative electrode material in the method has the advantage that the capacity can be obviously improved.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for preparing a silicon cathode material based on an electrostatic spinning technology is characterized by comprising the following steps:
(1) deionized water and absolute ethyl alcohol are mixed according to a mass ratio of 1: 1-1: 2 is prepared into a solvent, and the mass ratio of the organic silicon source to the organic carbon source is 1: 0.5-1: 2 is mixed into a solute, and the pH value of the solution is adjusted within the range of 2-6 to form transparent sol;
(2) uniformly mixing the spinning solution and the prepared transparent sol, and preparing a fiber membrane by using an electrostatic spinning machine;
(3) putting the fiber membrane into a drying box for drying;
(4) and placing the dried fiber membrane in an argon protection environment for heat treatment to obtain the silicon negative electrode material.
2. The method for preparing the silicon cathode material based on the electrospinning technology according to claim 1, wherein the organic silicon source in step (1) is preferably ethyl orthosilicate.
3. The method for preparing the silicon anode material based on the electrospinning technology according to claim 1, wherein the organic carbon source in step (1) is preferably glucose or sucrose or citric acid or phenolic resin.
4. The method for preparing the silicon anode material based on the electrospinning technology as claimed in claim 1, wherein the pH value of the solution is adjusted in step (1), and the acidic solution used for adjusting the pH value is HCL or H2O2Or glacial acetic acid, and the alkaline solution is ammonia water.
5. The method for preparing the silicon anode material based on the electrostatic spinning technology according to claim 1, wherein the preparation method of the spinning solution in the step (2) comprises the following steps: the composite material is prepared by mixing polyvinylpyrrolidone or polyacrylonitrile as a solute and deionized water and absolute ethyl alcohol as solvents according to the mass ratio of 1:2: 4.
6. The method for preparing the silicon anode material based on the electrospinning technology according to claim 1, wherein the fiber membrane is obtained by using the electrospinning machine in the step (2), and the parameters of the electrospinning machine are set as follows: the electrostatic spinning machine has positive voltage of 10-15KV, negative voltage of 0-5KV, injection speed of 0.2-0.5mm/min, and spinning temperature of 30-40 deg.C.
7. The method for preparing the silicon anode material based on the electrospinning technology as claimed in claim 1, wherein the fiber membrane is dried in a drying oven in step (3), the drying temperature is 90 ℃ and the drying time is 24 h.
8. The method for preparing the silicon anode material based on the electrospinning technology according to claim 1, wherein the heat treatment process in the step (4) is as follows: the fiber membrane is placed in a tube furnace filled with argon, the temperature is raised to 700-1200 ℃, and the temperature is kept for 60-120 min.
9. The application of the silicon negative electrode material prepared based on the electrostatic spinning technology is characterized in that the prepared silicon negative electrode material, conductive carbon black and sodium alginate are mixed to prepare slurry, and the slurry is coated, dried, pressed into sheets, sliced and weighed to prepare the silicon negative electrode sheet, wherein the prepared silicon negative electrode sheet is used for manufacturing a button cell.
10. The application of the silicon negative electrode material prepared based on the electrostatic spinning technology as claimed in claim 9, wherein the proportion of the silicon negative electrode material, the conductive carbon black and the sodium alginate is as follows according to the parts by weight: 75 parts of silicon negative electrode material, 15 parts of conductive carbon black and 15 parts of sodium alginate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114242987A (en) * | 2021-12-22 | 2022-03-25 | 格龙新材料科技(常州)有限公司 | Preparation method of three-dimensional porous silicon-carbon composite material |
| CN114284479A (en) * | 2021-12-22 | 2022-04-05 | 博路天成新能源科技有限公司 | Preparation method of novel carbon-silicon negative electrode material |
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