CN110957481A - Porous silicon-carbon composite material and preparation method thereof - Google Patents
Porous silicon-carbon composite material and preparation method thereof Download PDFInfo
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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Abstract
The embodiment of the invention discloses a porous silicon-carbon composite material and a preparation method thereof, wherein the preparation method comprises the following steps: dissolving an organic carbon source and a water-soluble pore-forming agent by using water to obtain a solution; dispersing silicon powder in the solution to obtain a mixed solution; drying the mixed solution to obtain a first solid; heating the first solid to carbonize the organic carbon source to obtain a second solid; and washing the second solid by using water, and removing the water-soluble pore-forming agent to obtain the porous silicon-carbon composite material. The pore-forming agent can be repeatedly used, so that the production cost is greatly saved, strong corrosive and dangerous chemicals are not used in the whole process, no waste liquid is generated, the operation is simple, the production cost is low, the safety is high, the product performance is excellent, and the application prospect is wide.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to a porous silicon-carbon composite material and a preparation method thereof.
Background
Lithium ion batteries have been widely used in consumer electronics fields such as smart phones, smart bracelets, digital cameras, and notebook computers, and have the greatest consumer demand. Meanwhile, the electric vehicle is gradually popularized in the fields of pure electric vehicles, hybrid electric vehicles and extended-range electric vehicles, and the market share is the largest in increasing trend. In addition, the lithium ion battery has a good development trend in the large-scale energy storage fields of power grid peak shaving, household power distribution, communication base stations and the like.
Currently, graphite is a commonly used negative electrode material for lithium batteries. In order to accelerate the development of the next generation of lithium ion power batteries, the industry provides the aim that the energy density of a power battery monomer reaches 300 W.h/kg in the middle period and reaches 400 W.h/kg in the long period. In response to this requirement, the actual capacity of graphite for the negative electrode material has been close to its theoretical limit, and it is necessary to develop a new material having a higher energy density and taking other criteria into consideration. Among them, the silicon carbon negative electrode is considered as a negative electrode material for a next-generation lithium ion battery, since it can combine the conductivity of a carbon material and the high capacity of a silicon material. At present, manufacturers capable of producing silicon-carbon cathode materials are few, and due to the high process cost, the price of downstream products is too high to be accepted by the market.
One of the preparation methods of the silicon carbon material is to use pore-forming agent to increase the porous structure of the loaded carbon layer. In the existing preparation method, the pore-forming agent is usually a substance which can generate a chemical reaction with the lotion or a substance which generates gas through a chemical reaction, the porous agent is removed from the loaded carbon layer after the reaction, and pores are formed by the overflow of the gas, so that the loaded carbon layer forms a porous structure.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a porous silicon-carbon composite material and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the preparation method of the porous silicon-carbon composite material is characterized by comprising the following steps of:
dissolving an organic carbon source and a water-soluble pore-forming agent by using water to obtain a solution;
dispersing silicon powder in the solution to obtain a mixed solution;
drying the mixed solution to obtain a first solid;
heating the first solid to carbonize the organic carbon source to obtain a second solid;
and washing the second solid by using water, and removing the water-soluble pore-forming agent to obtain the porous silicon-carbon composite material.
Preferably, the water-soluble pore-forming agent is at least one of sodium carbonate, potassium carbonate, sodium sulfate, potassium sulfate and magnesium sulfate.
Preferably, the organic carbon source is at least one of glucose, sucrose, polyvinylpyrrolidone and carboxymethylcellulose.
Preferably, the mass ratio of the silicon powder, the organic carbon source and the pore-forming agent is 1: 0.1-10: 0.05-5.
Preferably, the mass ratio of the silicon powder, the organic carbon source and the pore-forming agent is 1:2.5: 0.25.
Preferably, the concentration of the organic carbon source in the solution is 0.01 g/mL-0.80 g/mL; the concentration of the water-soluble pore-forming agent in the solution is 0.001 g/mL-0.20 g/mL.
Preferably, the silicon powder is dispersed in the solution by using an ultrasonic dispersion technology.
Preferably, the specific process of heating the first solid is: heating for 0.5-10 h at 700-1000 ℃ in protective atmosphere.
Preferably, the protective atmosphere is selected from at least one of nitrogen, argon, a mixture of nitrogen and hydrogen, and a mixture of argon and hydrogen.
A porous silicon-carbon composite material is characterized by comprising a silicon core and a carbon layer positioned outside the silicon core, wherein the carbon layer is provided with pores, and the pore diameter of the pores ranges from 1nm to 22 nm.
The embodiment of the invention has the following beneficial effects:
the method comprises the steps of dissolving a water-soluble organic carbon source and a pore-forming agent by using water as a solvent, and uniformly mixing the organic solvent and the pore-forming agent; the pore-forming agent is removed by taking water as a lotion, so that the pore-forming agent does not generate chemical reaction, only exists in the form of aqueous solution, is not polluted by other solvents, can be repeatedly used, and greatly saves the cost of the pore-forming agent. From the whole process, the whole process has no extreme reaction conditions, does not use strong corrosive and dangerous chemicals, does not generate waste liquid, is simple to operate, has low production cost and high safety, has excellent product performance and has a wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Wherein:
FIG. 1 is an SEM image of the porous silicon carbon composite obtained in example 1;
FIG. 2 is a plot of the pore size distribution of the porous silicon carbon composite shown in FIG. 1;
FIG. 3 is a graph showing the relationship between the charge/discharge voltage and the specific capacity in the case where the porous Si-C composite material obtained in example 1 is used as a negative electrode for charge/discharge;
FIG. 4 shows the porous Si-C composite obtained in example 1 as a negative electrode at 200mA g-1A relation graph of cycle performance test under current density;
FIG. 5 is a graph showing the relationship between the cycle performance test using the porous Si-C composite obtained in example 1 as a negative electrode;
FIG. 6 shows that the porous Si-C composite obtained in example 2 was used as a negative electrode at 200mA g-1A relation graph of cycle performance test under current density;
FIG. 7 shows that the porous Si-C composite obtained in example 3 was used as a negative electrode at 200mA g-1And (3) a relation graph of a cycle performance test under current density.
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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to solve the problem that the pore-forming agent in the prior art cannot be recycled, the invention provides an improved preparation method of a porous silicon-carbon composite material. In addition, the dissolution process has no violent chemical reaction, and strong corrosive and dangerous chemicals are not used, so that the whole process is simpler and safer. The whole process does not produce waste liquid, and reduces the environmental protection hazard.
Specifically, the method comprises the following steps:
dissolving an organic carbon source and a water-soluble pore-forming agent by using water to obtain a solution. The organic carbon source is also water-soluble, which is beneficial to the uniform dispersion of the pore-forming agent in the organic carbon source, so that the finally formed porous silicon-carbon composite material has uniform pore distribution. Preferably, the organic carbon source is at least one of glucose, sucrose, polyvinylpyrrolidone and carboxymethylcellulose. The water-soluble pore-forming agent is a substance that can be dissolved in water, and the water-soluble pore-forming agent has sufficient stability in the subsequent heating process of carbonizing the organic carbon source, does not melt, does not decompose itself, and does not react with other substances to generate new substances, and preferably, the water-soluble pore-forming agent is at least one of sodium carbonate, potassium carbonate, sodium sulfate, potassium sulfate and magnesium sulfate. The water-soluble pore-forming agent does not generate gas in the removing process, so that very uniform and tiny pores can be obtained, the loaded carbon layer has higher specific surface area and higher hardness, and the stability of the porous silicon-carbon composite material in the repeated charging and discharging process is improved.
Next, silicon powder is dispersed in the above solution to obtain a mixed solution. In the process, preferably, the silicon powder is uniformly dispersed in the solution by using an ultrasonic dispersion technology.
Then, the mixed solution is dried to obtain a first solid. At this time, the first solid includes a silicon core inside and an organic carbon source layer coated on the silicon core and internally mixed with a water-soluble pore-forming agent.
Continuously heating the first solid to carbonize the organic carbon source to obtain a second solid; the second solid includes an inner silicon core and an amorphous carbon layer coated on the silicon core and mixed with a water-soluble pore-forming agent. Preferably, in the process, the organic carbon source is completely carbonized by heating for 0.5 to 10 hours at a temperature of 700 to 1000 ℃ in a protective atmosphere. Preferably, the protective atmosphere is selected from at least one of nitrogen, argon, a mixture of nitrogen and hydrogen, and a mixture of argon and hydrogen.
And washing the second solid by using water, and removing the water-soluble pore-forming agent to obtain the porous silicon-carbon composite material. The aqueous solution containing the water-soluble pore-forming agent can be reused.
According to the invention, through multiple experiments, reaction parameters are adjusted, the material ratio is optimized, and the porous silicon-carbon composite material with uniform pores and excellent electrical property is prepared. Preferably, the mass ratio of the silicon powder, the organic carbon source and the pore-forming agent is 1: 0.1-10: 0.05-5. In the dissolving process of the first step, the concentration of the organic carbon source in the solution is preferably 0.01 g/mL-0.80 g/mL; the concentration of the water-soluble pore-forming agent in the solution is 0.001 g/mL-0.20 g/mL.
The specific embodiment is as follows:
example 1
Weighing 10ml of aqueous solution, and respectively weighing 2.5g of glucose, 0.25g of sodium carbonate and 1g of silicon powder;
dissolving the glucose and the sodium carbonate in a water solvent, and ultrasonically dispersing silicon powder in the obtained solution for 1 h;
fully mixing, and drying at 80 ℃ to obtain a first solid;
placing the first solid in a protective atmosphere of argon, heating to 800 ℃, and heating at a constant temperature for 2h to obtain a second solid;
and (3) repeatedly washing and filtering the second solid for 5 times by using water, and drying at 80 ℃ to obtain the final porous silicon-carbon composite material P-Si @ C-1.
The porous silicon-carbon composite material obtained in the above way is subjected to material characterization, so as to obtain an SEM image as shown in fig. 1, and it can be seen from the figure that: the surface of the nano silicon particles is loaded with uniform amorphous carbon; the pore size distribution curve in fig. 2 shows that the material has a porous structure distribution of both micropores and mesopores.
The prepared porous silicon-carbon composite material, super P (small-particle conductive carbon black which can be used in both a positive electrode and a negative electrode and has no lithium storage function are dispersed around an active substance to form a branched conductive network, the branched conductive network has the functions of reducing the battery resistance and improving the ion conductivity), CMC (thickening agent for lithium batteries, sodium carboxymethylcellulose) and SBR (binder for lithium batteries, styrene butadiene rubber) are mixed according to the mass ratio of 91:3:2:4, a proper amount of deionized water is added, the mixture is stirred into uniform slurry, the uniform slurry is coated on a copper foil, and the copper foil is dried and punched into an electrode plate with the diameter of 12 mm. Taking a metal lithium sheet as a counter electrode, and matching a diaphragm and 1mol/L LiPF in a glove box6(EC: DEC: DMC 1:1:1) electrolyte solution assembly 2032 type button half cell electrochemical performance tests were performed to obtain the results of fig. 3 to 5. The porous silicon carbon composite material exhibits a low and smooth charge and discharge plateau (fig. 3); at 200mAg-1Charging and discharging circulation is nearly 200 circles under current density, reversible specific capacity is kept to be 604mAhg-1Showing higher energy storage and cycle stability (fig. 4); meanwhile, the composite material has excellent rate performance, the reversible specific capacity attenuation is reduced under the heavy current density, and the high energy storage level and the capacity recovery are maintainedSex at 2000mAg-1The current density is kept to be not less than 550mAhg-1Reversible specific capacity (fig. 5).
Example 2
Weighing 10ml of aqueous solution, and respectively weighing 0.1g of polyvinylpyrrolidone, 0.1g of sodium sulfate and 1g of silicon powder;
dissolving the polyvinylpyrrolidone and the sodium sulfate in a water solvent, and ultrasonically dispersing silicon powder in the obtained solution for 1 h;
fully mixing, and drying at 80 ℃ to obtain a first solid;
heating the first solid in a nitrogen protective atmosphere to 800 ℃, and heating at a constant temperature for 6h to obtain a second solid;
and (3) repeatedly washing and filtering the second solid for 5 times by using water, and drying at 80 ℃ to obtain the final porous silicon-carbon composite material P-Si @ C-2, wherein the material has higher silicon-carbon ratio and less porous structure.
Electrochemical performance tests carried out on half-cells assembled in the same way as in example 1 gave the results of fig. 6, from which it can be seen that: at 200mAg-1The charge-discharge cycle of 100 circles under the current density shows that the whole reversible specific capacity is higher than that of P-Si @ C-1, and the initial stage reaches 1158mAhg-1The specific capacity is slowly attenuated along with the progress of charge and discharge circulation, and 815mAhg is still maintained after 100 circles-1But the cycling stability is relatively deficient.
Example 3
Weighing 30ml of aqueous solution, and respectively weighing 10g of glucose, 5g of magnesium sulfate and 1g of silicon powder;
dissolving the glucose and the magnesium sulfate in a water solvent, and ultrasonically dispersing silicon powder in the obtained solution for 1.5 h;
fully mixing, and drying at 80 ℃ to obtain a first solid;
placing the first solid in a protective atmosphere of nitrogen-hydrogen mixed gas, heating to 1000 ℃, and heating at a constant temperature for 4 hours to obtain a second solid;
repeatedly washing with water, vacuum filtering the second solid for 5 times, and freeze drying to obtain final porous silicon-carbon composite material P-Si @ C-3The material has a low silicon-carbon ratio and a large amount of porous structures. Electrochemical performance tests carried out on the assembled button half-cells gave the results of fig. 7, from which it can be seen that: at 200mAg-1The charge-discharge cycle of 200 cycles under the current density shows extremely strong cycle stability, but the reversible specific capacity is lower than P-Si @ C-1 and P-Si @ C-2 due to high carbon content, and the reversible specific capacity is stably kept at 453mAhg-1Left and right.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (10)
1. The preparation method of the porous silicon-carbon composite material is characterized by comprising the following steps of:
dissolving an organic carbon source and a water-soluble pore-forming agent by using water to obtain a solution;
dispersing silicon powder in the solution to obtain a mixed solution;
drying the mixed solution to obtain a first solid;
heating the first solid to carbonize the organic carbon source to obtain a second solid;
and washing the second solid by using water, and removing the water-soluble pore-forming agent to obtain the porous silicon-carbon composite material.
2. The method according to claim 1, wherein the water-soluble pore-forming agent is at least one of sodium carbonate, potassium carbonate, sodium sulfate, potassium sulfate, and magnesium sulfate.
3. The production method according to claim 1, wherein the organic carbon source is at least one of glucose, sucrose, polyvinylpyrrolidone and carboxymethylcellulose.
4. The preparation method according to claim 1, wherein the mass ratio of the silicon powder, the organic carbon source and the pore-forming agent is 1: 0.1-10: 0.05-5.
5. The preparation method according to claim 1, wherein the mass ratio of the silicon powder, the organic carbon source and the pore-forming agent is 1:2.5: 0.25.
6. The method according to claim 1, wherein the concentration of the organic carbon source in the solution is 0.01 to 0.80 g/mL; the concentration of the water-soluble pore-forming agent in the solution is 0.001 g/mL-0.20 g/mL.
7. The preparation method according to claim 1, wherein the silicon powder is dispersed in the solution by an ultrasonic dispersion technique.
8. The preparation method according to claim 1, wherein the specific process of heating the first solid is: heating for 0.5-10 h at 700-1000 ℃ in protective atmosphere.
9. The method according to claim 8, wherein the protective atmosphere is at least one selected from the group consisting of nitrogen, argon, a mixed gas of nitrogen and hydrogen, and a mixed gas of argon and hydrogen.
10. A porous silicon-carbon composite material is characterized by comprising a silicon core and a carbon layer positioned outside the silicon core, wherein the carbon layer is provided with pores, and the pore diameter of the pores ranges from 1nm to 22 nm.
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| CN114335473A (en) * | 2021-12-30 | 2022-04-12 | 宁波亿纬创能锂电池有限公司 | Negative electrode material and preparation method and application thereof |
| CN114649523A (en) * | 2020-12-18 | 2022-06-21 | 恒大新能源技术(深圳)有限公司 | Silicon-carbon negative electrode material and preparation method thereof |
| US11611115B2 (en) | 2017-12-29 | 2023-03-21 | Form Energy, Inc. | Long life sealed alkaline secondary batteries |
| CN115849381A (en) * | 2022-11-18 | 2023-03-28 | 浙江新安化工集团股份有限公司 | Three-dimensional porous silicon-carbon composite material and preparation method and application thereof |
| CN116237017A (en) * | 2023-03-08 | 2023-06-09 | 松山湖材料实验室 | Preparation method of porous carbon, porous carbon material and application of porous carbon material |
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