CN116314791A - Preparation method of silicon-carbon anode material - Google Patents

Preparation method of silicon-carbon anode material Download PDF

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Publication number
CN116314791A
CN116314791A CN202310054027.8A CN202310054027A CN116314791A CN 116314791 A CN116314791 A CN 116314791A CN 202310054027 A CN202310054027 A CN 202310054027A CN 116314791 A CN116314791 A CN 116314791A
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silicon
carbon
pore
anode material
forming agent
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薛孟尧
李云祥
张长安
曹新龙
屈涛
贾彦龙
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Jinghe Xincheng Shaanxi Coal Technology Research Institute New Energy Materials Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method of a silicon-carbon anode material, which specifically comprises the following steps: step 1, adding a pore-forming agent and a dispersing agent into a solvent, uniformly mixing, adding asphalt, mixing to obtain a uniform liquid phase mixture, drying, sequentially granulating, carbonizing, crushing, treating carbide with an etching solution, and removing the pore-forming agent to obtain porous carbon; step 2, placing the porous carbon prepared in the step 1 into a gas phase rotary kiln for gas phase deposition, heating, introducing silane and carrier gas, preserving heat, and then realizing nano-silicon in-situ compounding on a porous carbon matrix; continuously heating, introducing pyrolytic carbon source and carrier gas, and preserving heat to realize pyrolytic carbon cladding; cooling to room temperature, and discharging to obtain the silicon-carbon anode material. The invention solves the problems of nano silicon deposition on the surface of a carbon matrix and poor electrochemical performance in the existing preparation method of the silicon-carbon negative electrode material.

Description

Preparation method of silicon-carbon anode material
Technical Field
The invention belongs to the technical field of lithium ion battery anode active material, and relates to a preparation method of a silicon-carbon anode material.
Background
The traditional commercial silicon-carbon cathode material is usually compounded with graphite and the like after micron polysilicon is crushed to the nanometer level by using a sand milling method or a ball milling method and the like, but the nanometer polysilicon can only be crushed to about 100nm by using a crushing method. The size and crystallinity of the nano silicon have a decisive effect on the performance of the final silicon-carbon anode material, the smaller the nano silicon size is, the smaller the volume expansion effect is, and the literature reports that when the nano silicon size is smaller than 30nm, the volume expansion is greatly inhibited; meanwhile, amorphous silicon has better isotropy than polysilicon, and stress release is more uniform in the lithium ion intercalation process, so that pulverization of nano silicon is greatly inhibited.
Currently, nano-silicon is generally prepared by ball milling, vapor deposition, vacuum thermal evaporation and the like, wherein the vapor deposition can prepare nano-silicon with the particle size distribution of 1-1000nm and is widely focused. At present, a great deal of literature reports that a carbon material is used as a matrix and high-purity silane is used as a silicon source, but the existing preparation method of the silicon-carbon anode material generally has the following problems: 1. depositing a large amount of nano silicon on the surface of the carbon material; 2. the final material has poor electrochemical properties.
Disclosure of Invention
The invention aims to provide a preparation method of a silicon-carbon negative electrode material, which solves the problems of nano silicon deposition on the surface of a carbon matrix and poor electrochemical performance in the existing preparation method of the silicon-carbon negative electrode material.
The technical scheme adopted by the invention is that the preparation method of the silicon-carbon anode material comprises the following steps:
step 1, adding a pore-forming agent and a dispersing agent into a solvent, uniformly mixing, adding a carbon source, mixing to obtain a uniform liquid phase mixture, drying, sequentially granulating, carbonizing, crushing, treating carbide with an etching solution, and removing the pore-forming agent to obtain porous carbon;
step 2, placing the porous carbon prepared in the step 1 into a gas phase rotary kiln for gas phase deposition, heating, introducing silane and carrier gas, preserving heat, and then realizing nano-silicon in-situ compounding on a porous carbon matrix; continuously heating, introducing pyrolytic carbon source and carrier gas, and preserving heat to realize pyrolytic carbon cladding; cooling to room temperature, and discharging to obtain the silicon-carbon anode material.
The invention is also characterized in that:
in the step 1, the mixing time of the pore-forming agent and the dispersing agent is 1h-10h, the mixture is continuously mixed for 1h-5h after asphalt is added, and the solid content of the liquid phase mixed solution is 1% -40%.
In the step 1, the mass ratio of the carbon source to the pore-forming agent is 1:0.2-10, and the mass ratio of the dispersing agent to the pore-forming agent is 1:50-100.
In the step 1, the etching liquid is one of hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, potassium hydroxide and sodium hydroxide, the concentration used for removing the pore-forming agent is 1-10mol/L, the etching time is more than 12 hours, and the etching temperature is 40-80 ℃.
The pore-forming agent is at least one of calcium carbonate, magnesium oxide, ferric oxide, zinc oxide, potassium hydroxide, zinc chloride, silicon dioxide, calcium citrate, sodium citrate and barium citrate.
In the step 2, the carrier gas is hydrogen, and the flow ratio of silane to hydrogen is 1:1-15, wherein the vapor deposition temperature is 500-600 ℃; the deposition time is 60-180min.
The invention has the beneficial effects that the porous carbon is prepared by a template method, the internal pores are uniformly distributed, and the pore volume, the pore diameter and the specific surface of the porous carbon are controlled by the addition proportion of the template and the asphalt; and (3) in-situ generating small-particle-size amorphous silicon in the pores through silane deposition, and then further coating pyrolytic carbon, filling the pores and coating nano silicon. Compared with the traditional silicon-carbon anode material, the small-particle-size nano silicon greatly inhibits the volume expansion effect of nano silicon, and the amorphous silicon has better isotropy than the crystalline silicon, so that the stress distribution in the expansion process is uniform. The material has better electrochemical performance and lower expansion.
Drawings
FIG. 1 is a preparation flow chart of a preparation method of the silicon-carbon anode material;
FIG. 2 is a graph showing the pore size distribution of mesoporous carbon prepared in example 1 of the preparation method of the silicon-carbon negative electrode material of the present invention;
FIG. 3 is a graph showing the first charge and discharge curves of the finished Si-C product prepared in example 1 of the preparation method of the Si-C anode material of the present invention;
FIG. 4 is a graph showing XRD test results of example 1 and comparative example 1 of the preparation method of the silicon carbon negative electrode material of the present invention;
FIG. 5 is a chart of mesoporous carbon Scanning Electron Microscope (SEM) test prepared in example 1 of the preparation method of the silicon-carbon negative electrode material of the invention;
fig. 6 (a) to (e) are test charts of the silicon-carbon negative electrode material prepared in example 1 of the preparation method of the silicon-carbon negative electrode material of the present invention, fig. 6 (a) and 6 (b) are two partial sectional views of the silicon-carbon negative electrode material after being cut from the middle, and fig. 6 (C) to (e) are distribution diagrams of Si, C and O elements of the silicon-carbon negative electrode material in the mapping test, respectively.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The preparation method of the silicon-carbon anode material disclosed by the invention, as shown in fig. 1, comprises the following steps:
step 1, adding a pore-forming agent and a dispersing agent into a solvent, uniformly mixing, adding a carbon source, mixing to obtain a uniform liquid phase mixture, drying, granulating, carbonizing, crushing, and treating carbide with an etching solution to remove the pore-forming agent to obtain the porous carbon. The carbon source is pitch.
In the step 1, firstly, a pore-forming agent and a dispersing agent are added into a solvent for mixing for a period of time, and then asphalt is added for continuous mixing to obtain a uniform liquid phase mixture, so that the pore-forming agent is uniformly combined with a carbon source, and after subsequent etching, internal pores are uniformly distributed, and deposited nano silicon is uniformly distributed; wherein, the mixing time of the pore-forming agent and the dispersing agent is 1-10h, the mixture is continuously mixed for 1-5h after asphalt is added, and the solid content of the liquid phase mixed solution is 1% -40%. The carbon source is pitch.
The pore-forming agent is at least one of templates of calcium carbonate, magnesium oxide, ferric oxide, zinc oxide, potassium hydroxide, zinc chloride, silicon dioxide, calcium citrate, sodium citrate, barium citrate and the like with the size of 1-50nm, the dispersing agent is at least one of stearic acid, PVP, oleic acid, ricinoleic acid and n-caprylic acid, the mass ratio of the carbon source to the pore-forming agent is 1 (0.2-10), and the adding amount of the dispersing agent and the mass of the pore-forming agent are 1: (50-100).
The liquid phase mixture adopts at least one of evaporation drying, spray drying and freeze drying, and the drying modes have certain granulating effect, and the materials can be more compact by isostatic pressing, tabletting and other treatments after drying; in carbonization treatment, in order to ensure complete volatilization of asphalt, a low heating rate of 0.5-3 ℃/min is adopted below 500 ℃, the carbonization temperature is between 850-1500 ℃, the heat preservation time is between 60-360min, and complete carbonization of asphalt is ensured; after carbonization, the porous carbon is crushed, the median particle diameter D50 of the porous carbon is between 5 and 15 mu m, the larger particle diameter is unfavorable for the uniform deposition of silane in the porous carbon, and the yield of the porous carbon is seriously reduced by the smaller particle diameter.
The etching liquid is hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, potassium hydroxide, sodium hydroxide and other substances, the concentration used for removing the pore-forming agent is 1-10mol/L, the etching time is more than 12 hours, and the template can be etched more completely at the high temperature, preferably at 40-80 ℃.
The porous carbon prepared in the step 1 has a specific surface area of 100-1500m 2 Per gram, pore volume of 0.5-1.1cm 3 The average pore diameter is 5-50nm, wherein the micropore ratio is 0-50%, the medium Kong Zhanbi is 0-100%, the silane is difficult to deposit into the porous carbon due to the excessively low ratio and pore volume, and the material is difficult to completely fill due to the excessively high ratio and pore volume, so that the pressure resistance of the material is affected; the pore diameter which is too high has no certain inhibition effect on the growth of the nano silicon, so that the particle size of the nano silicon is too large.
Step 2, placing the porous carbon in a gas phase rotary kiln, heating, introducing silane and carrier gas, and preserving heat for a period of time to realize nano-silicon in-situ compounding on a porous carbon matrix; continuously heating, introducing pyrolytic carbon source and carrier gas, and preserving heat for a period of time to realize pyrolytic carbon cladding; cooling to room temperature, discharging and obtaining the silicon-carbon anode material.
In the step 2, in vapor deposition, the silicon source used is silane, and the carrier gas is hydrogen; the deposition temperature is 500-600 ℃, the excessive temperature can lead the silane to be directly deposited to generate amorphous silicon with the particle size, and the excessive low temperature can lead the silane to be incompletely deposited; the silane/hydrogen flow ratio is 1: (1-15), hydrogen can inhibit silane deposition to reduce nano silicon particle size and amorphous state, and meanwhile, in the subsequent heating and pyrolytic carbon deposition process, hydrogen is always introduced, so that amorphous silicon is inhibited from being converted into crystalline silicon by heating and dehydrogenation; the deposition temperature of pyrolytic carbon is 700-900 ℃, the pyrolytic carbon source is acetylene, acetone, cyclohexane and the like, and the deposition time is 60-180min.
Example 1
Adding 2kg of 20nm calcium carbonate and 0.1kg of stearic acid into 30kg of ethanol solution, sanding for 1h, adding 1kg of asphalt, continuously sanding for 30min, carbonizing powder obtained by spray drying liquid phase materials, heating to 480 ℃ at 1 ℃/min in the carbonization process, preserving heat for 120min, heating to 900 ℃ at 5 ℃/min, preserving heat for 120min, reacting the collected black powder at 2MHCl and 50 ℃ for 24h, flushing with deionized water to neutrality, leaching and drying after no obvious bubbles are generated to obtain mesoporous carbon, and carrying out jet milling on the mesoporous carbon with D50=5.8 mu m and pore volume of 0.7cm 3 And/g, average pore diameter 11.8nm.
Placing mesoporous carbon in a vapor deposition furnace, heating to 500 ℃ under inert atmosphere, introducing according to silane/hydrogen=0.5/3L/min flow, keeping the temperature for 60min, stopping introducing silane, and introducing hydrogen according to 3L/min; heating to 800 ℃, maintaining the temperature of acetylene/hydrogen=0.5/3L/min for 120min, keeping the hydrogen at 3L/min in the cooling process, and cooling to room temperature to obtain the final silicon-carbon anode material.
FIG. 2 is a pore size distribution curve of porous carbon of example 1, which has a uniform and narrow pore size distribution and an average pore size of 11nm. FIG. 3 shows the charge-discharge curves of the sample prepared in example 1, in which the specific discharge capacity was concentrated at 0.2V or less and the specific charge capacity was concentrated at 0.6V, which are characteristic curves of silicon. Fig. 4 is XRD test results of example 1 and comparative example 1, and nano-silicon assumes an amorphous form after hydrogen gas is introduced. Fig. 5 is a graph showing the result of the porous carbon scanning electron microscope test prepared in example 1, and abundant pores can be observed. FIG. 6 (a) is a cross-sectional electron microscope test chart of the sample prepared in example 1, FIG. 6 (b) is a cross-sectional mapping test of selected regions, and FIG. 6 (C) (d) (e) is an elemental distribution of Si, C, O, and it can be observed that Si, C, O are uniformly distributed.
Example 2
Compared with example 1, the mesoporous carbon d50=10.8 μm and the pore volume of 1.1cm were the same except that 1kg of 20nm calcium carbonate and 0.05kg of stearic acid were added to 15kg of ethanol solution 3 And/g, average pore size 9.4nm.
Example 3
In comparison with example 1, instead of 50nm zinc oxide, the remainder of the procedure was the same, the mesoporous carbon d50=14.8 μm, the pore volume 0.85cm3/g, and the average pore diameter 30nm.
Example 4
1kg of bitumen is added to 2kg of 5nm oily SiO 2 Stirring the dispersion for 2 hours to uniformly disperse asphalt, drying and then carrying out carbonization, wherein in the carbonization process, the temperature is raised to 500 ℃ at 1 ℃/min, the temperature is kept for 240min, then the temperature is raised to 1300 ℃ at 5 ℃/min, the temperature is kept for 120min, the collected black powder reacts for 24 hours at 2M HF and 50 ℃ and is washed to be neutral by deionized water, after no obvious bubbles are generated, the mesoporous carbon is obtained by suction filtration and drying, and is subjected to jet milling, the mesoporous carbon D50=12.2 mu M, the pore volume is 0.85cm < 3 >/g, and the average pore diameter is 3.8nm.
Placing mesoporous carbon in a vapor deposition furnace, heating to 500 ℃ under inert atmosphere, introducing according to silane/hydrogen=1/15L/min flow, keeping the temperature for 60min, stopping introducing silane, and introducing hydrogen according to 5L/min; heating to 700 ℃, maintaining the temperature of acetylene/hydrogen=1/5L/min for 120min, keeping the hydrogen at 5L/min in the cooling process, and cooling to room temperature to obtain the final silicon-carbon anode material.
Example 5
Adding 2kg of calcium citrate and 0.2kg of PVP into 20kg of ethanol, ball milling for 3 hours, adding 1.5kg of asphalt, continuing ball milling for 1 hour to uniformly mix the asphalt and the calcium citrate, discharging, drying, performing carbonization, heating to 500 ℃ at 1 ℃/min in the carbonization process, preserving heat for 240min, heating to 950 ℃ at 5 ℃/min, preserving heat for 120min, etching at 60 ℃ by using 2mol/L dilute nitric acid, filtering, washing to be neutral, and obtaining mesoporous carbon D50=8.8 mu m, pore volume of 1.37cm < 3 >/g and average pore diameter of 15nm.
Placing mesoporous carbon in a vapor deposition furnace, heating to 500 ℃ under inert atmosphere, introducing according to silane/hydrogen=1/10L/min flow, preserving heat for 180min, and stopping introducing silane; and (3) introducing hydrogen at the speed of 10L/min, heating to 700 ℃, keeping the temperature for 180min while keeping the hydrogen at the speed of 10L/min, and cooling to room temperature to obtain the final silicon-carbon anode material.
Comparative example 1
In contrast to example 1, no hydrogen was introduced.
The mesoporous carbon materials and the silicon carbon materials provided in examples 1 to 5 and comparative example 1 were respectively subjected to performance tests, and the test items are: specific surface area, pore volume, pore diameter, electrochemical properties, and X-ray diffraction.
The mesoporous carbon materials provided in examples 1-5 and comparative example 1 were used to prepare lithium ion battery negative electrode materials, then button-type lithium ion batteries were assembled, all the materials used to assemble the lithium ion batteries were the same, wherein the positive electrode was a lithium sheet, the current collector was a copper foil, and the first charge specific capacity and the first coulombic efficiency of each group of lithium ion batteries were tested after the assembly was completed.
TABLE 1 comparison of porous carbon Properties
Figure BDA0004059668640000081
Figure BDA0004059668640000091
Table 2 electrochemical performance and physical Property index tests for examples 1-5 and comparative example 1
Figure BDA0004059668640000092

Claims (6)

1. The preparation method of the silicon-carbon anode material is characterized by comprising the following steps of: the method specifically comprises the following steps:
step 1, adding a pore-forming agent and a dispersing agent into a solvent, uniformly mixing, adding a carbon source, mixing to obtain a uniform liquid phase mixture, drying, sequentially granulating, carbonizing, crushing, treating carbide with an etching solution, and removing the pore-forming agent to obtain porous carbon;
step 2, placing the porous carbon prepared in the step 1 into a gas phase rotary kiln for gas phase deposition, heating, introducing silane and carrier gas, preserving heat, and then realizing nano-silicon in-situ compounding on a porous carbon matrix; continuously heating, introducing pyrolytic carbon source and carrier gas, and preserving heat to realize pyrolytic carbon cladding; cooling to room temperature, and discharging to obtain the silicon-carbon anode material.
2. The method for preparing the silicon-carbon anode material according to claim 1, wherein: in the step 1, the mixing time of the pore-forming agent and the dispersing agent is 1-10h, the mixture is continuously mixed for 1-5h after asphalt is added, and the solid content of the liquid phase mixed solution is 1-40%.
3. The method for preparing the silicon-carbon anode material according to claim 2, characterized in that: in the step 1, the mass ratio of the carbon source to the pore-forming agent is 1:0.2-10, and the mass ratio of the dispersing agent to the pore-forming agent is 1:50-100.
4. The method for preparing a silicon-carbon anode material according to claim 3, wherein: in the step 1, the etching liquid is one of hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, potassium hydroxide and sodium hydroxide, the concentration used for removing the pore-forming agent is 1-10mol/L, the etching time is more than 12 hours, and the etching temperature is 40-80 ℃.
5. The method for preparing the silicon-carbon anode material according to claim 4, wherein: the pore-forming agent is at least one of calcium carbonate, magnesium oxide, ferric oxide, zinc oxide, potassium hydroxide, zinc chloride, silicon dioxide, calcium citrate, sodium citrate and barium citrate.
6. The method for preparing the silicon-carbon anode material according to claim 1, wherein: in the step 2, the carrier gas is hydrogen, and the flow ratio of silane to hydrogen is 1:1-15, wherein the vapor deposition temperature is 500-600 ℃; the deposition time is 60-180min.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116613299A (en) * 2023-07-17 2023-08-18 浙江锂宸新材料科技有限公司 Preparation method of novel silicon-carbon anode material and product thereof
CN116885158A (en) * 2023-09-08 2023-10-13 琥崧智能装备(太仓)有限公司 Carbon-silicon composite anode active material and preparation method and application thereof
CN116936780A (en) * 2023-09-18 2023-10-24 北京壹金新能源科技有限公司 Silicon-carbon composite material, preparation method and application thereof, and battery

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116613299A (en) * 2023-07-17 2023-08-18 浙江锂宸新材料科技有限公司 Preparation method of novel silicon-carbon anode material and product thereof
CN116613299B (en) * 2023-07-17 2023-11-24 浙江锂宸新材料科技有限公司 Preparation method of silicon-carbon anode material and product thereof
CN116885158A (en) * 2023-09-08 2023-10-13 琥崧智能装备(太仓)有限公司 Carbon-silicon composite anode active material and preparation method and application thereof
CN116885158B (en) * 2023-09-08 2023-12-01 琥崧智能装备(太仓)有限公司 Carbon-silicon composite anode active material and preparation method and application thereof
CN116936780A (en) * 2023-09-18 2023-10-24 北京壹金新能源科技有限公司 Silicon-carbon composite material, preparation method and application thereof, and battery

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