CN111211314A - Carbon-coated porous silicon-carbon composite material and preparation method thereof - Google Patents
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Abstract
The invention discloses a preparation method of a carbon-coated porous silicon-carbon composite material, which comprises the following steps of: acid cleaning and etching are carried out on the silicon alloy powder, and the carbon nano tube is added before or after the acid cleaning to obtain the porous silicon mixed material; preparing the porous silicon mixed material, the dispersing agent and the slurry solvent into slurry, performing ball milling dispersion or sanding dispersion, drying the uniformly dispersed slurry, putting the slurry into a high-temperature furnace, performing heat preservation carbonization in an inert gas atmosphere, and finally performing jet milling to obtain a finished product. The invention also discloses a carbon-coated porous silicon-carbon composite material, which is a composite material in which porous silicon is uniformly coated with carbon nano tubes. The carbon-coated porous silicon-carbon composite material has strong conductivity, limits the expansion and contraction in the process of silicon lithium intercalation and deintercalation, has simple preparation process and low cost, is easy to prepare on a large scale, and is suitable for the cathodes of all lithium ion batteries.
Description
Technical Field
The invention belongs to the field of battery materials, relates to a lithium ion battery cathode material and a preparation method thereof, and particularly relates to a carbon-coated porous silicon-carbon composite material and a preparation method thereof.
Background
The lithium ion battery has the advantages of high energy density, small self-discharge, wide working voltage range, no memory effect, long service life, no environmental pollution and the like, and is widely applied to the fields of electronic products, electric automobiles and energy storage. At present, the application of the negative electrode material is mainly based on the traditional graphite material, but the specific capacity of the graphite is close to the theoretical value of 372mAh/g, so that the space for improving the specific capacity is difficult to be provided, and the energy density of the lithium ion battery is limited. The silicon-carbon composite material has a high specific capacity, and thus becomes a development trend of the lithium ion battery cathode material.
However, silicon as a negative electrode material of a lithium ion battery also has obvious disadvantages: firstly, silicon is used as a semiconductor material, and the self conductivity of the silicon is lower; secondly, in the charging and discharging process, along with the insertion and the separation of lithium ions, the volume change of the silicon material is large, so that the material is pulverized and falls off, and finally, the material is separated from a current collector, and the circulation stability is poor; finally, although doping, nanocrystallization and other methods can be adopted to improve the electrochemical performance of the silicon-based material, these preparation methods are relatively complex and costly, and are not easy to prepare on a large scale, and the electrochemical performance of the prepared material needs to be further improved.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a carbon-coated porous silicon-carbon composite material and a preparation method thereof, so as to achieve the purposes of enhancing the electrical conductivity of an electrode, limiting the expansion and contraction in the process of silicon lithium intercalation and deintercalation, simplifying the preparation process and facilitating large-scale preparation.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a carbon-coated porous silicon-carbon composite material comprises the following steps of:
s1: acid cleaning and etching are carried out on the silicon alloy powder, and the carbon nano tube is added before or after the acid cleaning to obtain the porous silicon mixed material;
s2: preparing a porous silicon mixed material, a dispersing agent and a slurry solvent into slurry, performing ball milling dispersion or sand milling dispersion for 2-50h, and performing forced air drying on the uniformly dispersed slurry at 50-90 ℃ for 6-48h to obtain a Si/SiOx-dispersing agent-carbon nanotube composite;
s3: putting the Si/SiOx-dispersant-carbon nanotube composite into a high-temperature furnace, and carbonizing the Si/SiOx-dispersant-carbon nanotube composite for 2 to 24 hours at the temperature of 500-;
s4: and (3) carrying out jet milling on the Si/SiOx-C-carbon nanotube composite to obtain a final finished product.
As a limitation of the present invention: the S1 includes the following steps performed in sequence:
the method comprises the following steps: adding silicon alloy powder into hydrochloric acid, reacting at 60-90 ℃ for 15-30h to remove metal elements, cleaning to neutrality, and performing forced air drying at 50-90 ℃ for 6-48h to obtain silicon powder;
step two: adding silicon oxide into hydrofluoric acid solution, reacting for 5-20h at normal temperature, and cleaning to be neutral to obtain porous silicon material;
step three: and uniformly mixing the porous silicon material and the carbon nano tube to obtain the porous silicon mixed material.
As a limitation of the present invention: the step S1 includes the following steps performed in sequence:
the method comprises the following steps: uniformly mixing the silicon alloy powder and the carbon nano tubes to obtain a silicon alloy carbon nano tube mixture;
step two: adding the silicon alloy carbon nanotube mixture into hydrochloric acid, reacting at 60-90 ℃ for 15-30h to remove metal elements, cleaning to neutrality, and performing forced air drying at 50-90 ℃ for 6-48h to obtain a mixture of silicon powder and carbon nanotubes;
step three: and adding the mixture of the silicon powder and the carbon nano tube into a hydrofluoric acid solution, reacting for 5-20h at normal temperature, and cleaning to be neutral to obtain the porous silicon mixed material.
As a further limitation of the invention: in the cleaning process, deionized water is used for cleaning.
The invention also discloses a carbon-coated porous silicon-carbon composite material, which is a composite material in which porous silicon is uniformly coated with carbon nano tubes.
As a limitation of the present invention: the composite material is prepared from the following raw materials in parts by weight: 10-20 parts of silicon alloy powder, 50-100 parts of hydrochloric acid, 50-100 parts of hydrofluoric acid solution, 0.1-2 parts of dispersant, 70-90 parts of slurry solvent and 0.05-2 parts of carbon nano tube.
As a further limitation of the invention: the silicon alloy powder is at least one of ferrosilicon alloy powder, silicon-aluminum alloy powder, silicon-magnesium alloy powder and silicon-manganese alloy powder.
As a further limitation of the invention: the molar concentration of the hydrochloric acid is 1-12mol/L, and the molar concentration of the hydrofluoric acid solution is 0.5-2 mol/L.
As a further limitation of the invention: the slurry solvent is any one of water, ethanol, isopropanol and NMP.
As still further limiting the invention: the dispersing agent is any one of PVP (polyvinylpyrrolidone), PVA (polyvinyl alcohol), PAA (polyacrylic acid) and PEO (polyethylene oxide).
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) the silicon alloy in the invention removes metal element impurities by acid cleaning, and then is etched by hydrofluoric acid with certain concentration, thus effectively manufacturing the porous structure of Si/SiOx;
(2) the raw materials for preparing the material comprise the carbon nano tube, the carbon nano tube has excellent conductivity, the defect of poor silicon conductivity can be effectively overcome, and meanwhile, the carbon nano tube has the advantage of great length-diameter ratio and can more effectively limit the expansion and contraction in the process of silicon lithium intercalation and deintercalation;
(3) the slurry is subjected to ball milling dispersion or sanding dispersion, so that the operation is simple, the preparation cost is reduced, and the carbon nano tubes and the silicon are dispersed more efficiently and uniformly; and then the obtained Si/SiOx-dispersant-carbon nanotube composite is carbonized at high temperature, so that the carbon nanotube is uniformly and effectively coated on the Si/SiOx.
In conclusion, the carbon-coated porous silicon-carbon composite material disclosed by the invention is high in conductivity, can be used for limiting expansion and contraction in the process of silicon lithium intercalation and deintercalation, is simple in preparation process, low in cost and easy to prepare on a large scale, and is suitable for cathodes of all lithium ion batteries.
Drawings
The invention is described in further detail below with reference to the figures and the embodiments.
FIG. 1 is an SEM (scanning electron microscope) image of a silicon alloy material after acid cleaning and etching in example 9 of the present invention;
fig. 2 is an SEM image of the carbon-coated porous silicon-carbon composite material finally prepared in example 9 of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the carbon-coated porous silicon carbon composite material and the method of making the same described herein are preferred embodiments, are only for illustrating and explaining the present invention, and do not constitute a limitation on the present invention.
Example 1 preparation method of carbon-coated porous silicon-carbon composite Material
The embodiment is a preparation method of a carbon-coated porous silicon-carbon composite material, which is performed according to the following steps in sequence:
1) adding silicon alloy powder into hydrochloric acid, reacting at 90 ℃ for 24 hours to remove metal elements, washing to be neutral by using deionized water, and carrying out vacuum drying at 80 ℃ for 24 hours to obtain silicon powder;
2) adding silicon oxide into hydrofluoric acid solution for etching, reacting for 6h at normal temperature, and cleaning with deionized water to be neutral to obtain porous silicon material;
3) uniformly mixing a porous silicon material and a carbon nano tube to obtain a porous silicon mixed material;
4) preparing a porous silicon mixed material, a dispersing agent and a slurry solvent into slurry, sanding and dispersing for 8 hours, and carrying out forced air drying on the uniformly dispersed slurry for 20 hours at 80 ℃ to obtain a Si/SiOx-dispersing agent-carbon nanotube composite;
5) placing the Si/SiOx-dispersant-carbon nanotube composite into a tube furnace, evacuating with argon, heating to 1100 ℃ at a speed of 5 ℃/min, preserving heat, carbonizing for 10h, and finally performing jet milling on the obtained product to obtain the Si/SiOx-C-carbon nanotube composite;
6) and (3) carrying out jet milling on the Si/SiOx-C-carbon nanotube composite to obtain a final finished product.
Example 2-4 preparation of carbon-coated porous silicon-carbon composite Material
Examples 2 to 4 are a method for preparing a carbon-coated porous silicon carbon composite material, wherein the preparation process is the same as that of example 1 except for the parameters in the preparation process, which are specifically shown in table 1:
TABLE 1 parameters of the preparation
Example 5 preparation of carbon-coated porous silicon-carbon composite Material
The embodiment is a preparation method of a carbon-coated porous silicon-carbon composite material, which is performed according to the following steps in sequence:
1) uniformly mixing the silicon alloy powder and the carbon nano tubes to obtain a silicon alloy carbon nano tube mixture;
2) adding the silicon alloy carbon nanotube mixture into hydrochloric acid, reacting at 90 ℃ for 24h to remove metal elements, washing to be neutral by using deionized water, and then carrying out vacuum drying at 80 ℃ for 24h to obtain a mixture of silicon powder and carbon nanotubes;
3) adding the mixture of silicon oxide and carbon nano tubes into a hydrofluoric acid solution, reacting for 6h at normal temperature, and cleaning with deionized water to be neutral to obtain a porous silicon mixed material;
4) preparing a porous silicon mixed material, a dispersing agent and a slurry solvent into slurry, sanding and dispersing for 8 hours, and carrying out forced air drying on the uniformly dispersed slurry for 24 hours at 80 ℃ to obtain a Si/SiOx-dispersing agent-carbon nanotube compound;
5) placing the Si/SiOx-dispersant-carbon nanotube composite into a tube furnace, evacuating with argon, heating to 1100 ℃ at a speed of 5 ℃/min, preserving heat and carbonizing for 10h to obtain the Si/SiOx-C-carbon nanotube composite;
6) and (3) carrying out jet milling on the Si/SiOx-C-carbon nanotube composite to obtain a final finished product.
Examples 6-8 preparation of carbon-coated porous silicon-carbon composites
Examples 6 to 8 are a method of preparing a carbon-coated porous silicon carbon composite material, in which the preparation process is the same as that of example 5 except for the parameters in the preparation process, as shown in table 2:
TABLE 2 parameters of the preparation
Example 9 carbon-coated porous silicon carbon composite
This example is a carbon-coated porous silicon-carbon composite material prepared by the method of any one of examples 1 to 8, in which porous silicon is uniformly coated with carbon nanotubes. The raw materials for preparing the composite material comprise 1kg of silicon alloy powder, 7.5kg of 6mol/L hydrochloric acid, 7.5kg of 1mol/L hydrofluoric acid solution, 0.01kg of dispersing agent, 7kg of slurry solvent and 0.05kg of carbon nano tube.
The silicon alloy powder is ferrosilicon alloy powder with 75% of silicon content, the dispersant is PVP (polyvinylpyrrolidone), and the slurry solvent is water.
Examples 10-13 carbon-coated porous silicon-carbon composites
Examples 10 to 13 are carbon-coated porous silicon-carbon composites prepared by the method of any of examples 1 to 8, which are composites in which carbon nanotubes are uniformly coated on porous silicon. The raw material components for preparing the composite material are the same as those in example 9, except for the types and contents of the components, which are specifically shown in Table 3:
TABLE 3 kinds and contents of the respective components in the raw materials
Example 14 microstructure of carbon-coated porous silicon carbon composite
In order to observe the structure of the carbon-coated porous silicon-carbon composite material, in example 9, the silicon alloy material after being washed with acid to remove the metal element impurities and etched with hydrofluoric acid was imaged under a scanning electron microscope, as shown in fig. 1, which is an SEM (scanning electron microscope) image of the material, it can be seen from the figure that the porous structure of Si/SiOx can be effectively manufactured by removing the metal element impurities through acid washing and then etching with hydrofluoric acid.
The carbon-coated porous silicon-carbon composite material finally prepared in example 9 is imaged under a scanning electron microscope, as shown in fig. 2, which is an SEM (scanning electron microscope) image of the material, and it can be seen from the image that carbon nanotubes are uniformly distributed among silicon particles, so that the carbon nanotubes can be uniformly and effectively coated on the silicon particles by using the method of the present invention, a long-range conductive network is provided for the silicon particles after the carbon nanotubes are cyclically expanded in a battery, and electron conduction of an electrode material is ensured not to be lost.
Example 15 preparation and testing of lithium ion batteries
The carbon-coated porous silicon-carbon composite material prepared in example 9 and the carbon-silicon composite material prepared by the conventional method (in the conventional method, silicon powder, a dispersing agent and isopropanol are placed in a sand mill for sanding and then dried to obtain nano silicon particles, and the nano silicon particles are mixed with asphalt to coat and carbonize to obtain a finished product) are mixed according to the following steps: conductive agent (conductive carbon black, super-p): mixing the binder (0.2% CMC +0.8% SBR) in a mass ratio of 8:1:1 to prepare a negative plate, taking a lithium plate as a positive plate, taking a diaphragm as a polypropylene film, and taking lithium hexafluorophosphate (LiPF) containing 1mol/L lithium salt as electrolyte6) The solvent is a solvent with the volume ratio of 1: 1: ethylene Carbonate (EC) of 1: dimethyl carbonate (DMC): and methyl ethyl carbonate (EMC) to prepare the button cell. The button cell made of the carbon-silicon composite material obtained in example 9 was sample 1, and the button cell made of the carbon-silicon composite material obtained by the conventional method was sample 2. The lithium ion battery is subjected to charge and discharge tests by using the constant current of the blue test system, the voltage test range is 0.01-1.5V, and the test results are shown in a table 4:
table 4 sample 1 charge and discharge test results
Table 5 sample 2 charge and discharge test results
From the data in tables 4 and 5, it can be seen that: after 100 cycles, sample 1 has better cycle stability than sample 2, and the specific charge capacity retention rate of sample 1 is also kept at a higher level than that of sample 2. Therefore, the carbon-coated porous silicon-carbon composite material prepared by the invention has strong conductivity, and limits the expansion and contraction in the process of lithium intercalation and deintercalation from silicon.
Claims (10)
1. The preparation method of the carbon-coated porous silicon-carbon composite material is characterized by comprising the following steps of:
s1: acid cleaning and etching are carried out on the silicon alloy powder, and the carbon nano tube is added before or after the acid cleaning to obtain the porous silicon mixed material;
s2: preparing a porous silicon mixed material, a dispersing agent and a slurry solvent into slurry, performing ball milling dispersion or sand milling dispersion for 2-50h, and performing forced air drying on the uniformly dispersed slurry for 6-48h at 50-90 ℃ to obtain a Si/SiOx-dispersing agent-carbon nanotube composite;
s3: putting the Si/SiOx-dispersant-carbon nanotube composite into a high-temperature furnace, and carbonizing the Si/SiOx-dispersant-carbon nanotube composite for 2 to 24 hours at the temperature of 500-;
s4: and (3) carrying out jet milling on the Si/SiOx-C-carbon nanotube composite to obtain a final finished product.
2. The method of claim 1, wherein the step S1 comprises the following steps performed in sequence:
the method comprises the following steps: adding silicon alloy powder into hydrochloric acid, reacting at 60-90 ℃ for 15-30h to remove metal elements, cleaning to neutrality, and vacuum drying at 50-90 ℃ for 6-48h to obtain silicon powder;
step two: adding silicon oxide into hydrofluoric acid solution, reacting for 5-20h at normal temperature, and cleaning to be neutral to obtain porous silicon material;
step three: and uniformly mixing the porous silicon material and the carbon nano tube to obtain the porous silicon mixed material.
3. The method of claim 1, wherein the step S1 comprises the following steps performed in sequence:
the method comprises the following steps: uniformly mixing the silicon alloy powder and the carbon nano tubes to obtain a silicon alloy carbon nano tube mixture;
step two: adding the silicon alloy carbon nanotube mixture into hydrochloric acid, reacting at 60-90 ℃ for 15-30h to remove metal elements, cleaning to neutrality, and performing forced air drying at 50-90 ℃ for 6-48h to obtain a mixture of silicon powder and carbon nanotubes;
step three: and adding the mixture of the silicon powder and the carbon nano tube into a hydrofluoric acid solution, reacting for 5-20h at normal temperature, and cleaning to be neutral to obtain the porous silicon mixed material.
4. The method of claim 2 or 3, wherein the cleaning is performed with deionized water during the cleaning.
5. The carbon-coated porous silicon-carbon composite material prepared by the method of any one of claims 1 to 4, wherein the porous silicon-carbon composite material is a composite material in which carbon nanotubes are uniformly coated on porous silicon.
6. The carbon-coated porous silicon-carbon composite material according to claim 5, wherein the composite material is prepared from the following raw materials in parts by weight: 10-20 parts of silicon alloy powder, 50-100 parts of hydrochloric acid, 50-100 parts of hydrofluoric acid solution, 0.1-2 parts of dispersant, 70-90 parts of slurry solvent and 0.05-2 parts of carbon nano tube.
7. The carbon-coated porous silicon-carbon composite material according to claim 6, wherein the silicon alloy powder is at least one of a silicon-iron alloy powder, a silicon-aluminum alloy powder, a silicon-magnesium alloy powder, and a silicon-manganese alloy powder.
8. The carbon-coated porous silicon-carbon composite material according to claim 6 or 7, wherein the hydrochloric acid has a molar concentration of 1 to 12mol/L and the hydrofluoric acid solution has a molar concentration of 0.5 to 2 mol/L.
9. The carbon-coated porous silicon-carbon composite material according to claim 8, wherein the dispersant is any one of PVP, PVA, PAA, PEO.
10. The carbon-coated porous silicon-carbon composite material according to any one of claims 6, 7 and 9, wherein the slurry solvent is any one of water, ethanol, isopropanol and NMP.
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| CN113764622A (en) * | 2021-09-13 | 2021-12-07 | 合肥国轩高科动力能源有限公司 | Preparation method of low-expansion lithium battery silicon-carbon negative plate |
| CN115010135A (en) * | 2022-07-08 | 2022-09-06 | 上海旦元新材料科技有限公司 | Two-dimensional silicon nanosheet for lithium ion battery cathode and preparation method thereof |
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