CN115332496B - Preparation method of silica composite material for lithium ion battery - Google Patents
Preparation method of silica composite material for lithium ion battery Download PDFInfo
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- CN115332496B CN115332496B CN202210833370.8A CN202210833370A CN115332496B CN 115332496 B CN115332496 B CN 115332496B CN 202210833370 A CN202210833370 A CN 202210833370A CN 115332496 B CN115332496 B CN 115332496B
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/36—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
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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- 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-oxygen composite material for a lithium ion battery. The technical scheme is that the preparation process is as follows: preparing ferrocene formaldehyde solution, adding a silicon oxide material, dispersing uniformly, then dripping a phenol solution, performing hydrothermal reaction at 100-200 ℃ for 6-24 hours, washing and drying, and then performing reaction at 700-1100 ℃ for 1-6 hours by a vapor deposition method to obtain the carbon nano tube-amorphous carbon coated silicon oxide composite material. The beneficial effects of the invention are as follows: the silicon-oxygen composite material of the invention utilizes phenolic reaction to generate phenolic resin, and the carbonized amorphous carbon has the characteristics of good isotropy, stable structure and the like, thereby improving the performances of multiplying power, circulation and the like; the phenolic resin contains ferrocene catalyst, so that carbon nanotubes are generated in the carbonization process of the phenolic resin, a network structure is formed, and the expansion is reduced.
Description
Technical Field
The invention relates to the field of preparation of lithium ion battery materials, in particular to a preparation method of a silicon-oxygen composite material for a lithium ion battery.
Background
The silicon-oxygen material is composed of a silicon-oxygen core and an amorphous carbon shell, wherein the amorphous carbon on one hand improves the electronic conductivity of the core silicon, and on the other hand, the amorphous carbon isolates the electrolyte between the core and the shell to improve the circulation and the storage performance of the electrolyte, so that the quality of a shell coating layer has a great influence on the performance of the silicon-carbon material, and particularly plays a main role in multiplying power, storage and cycle performance of the material. The amorphous carbon deposited on the surface of the silicon-based material at present mainly comprises amorphous carbon formed by cracking a gaseous carbon source and carbonizing a polymer, and the amorphous carbon has low densification degree and poor isotropy of a coating material, so that the material has larger impedance and the cycle performance is influenced.
The Chinese patent number is CN201910260235.7, the patent name is lithium ion battery silicon-oxygen composite anode material and a preparation method thereof, the lithium ion battery silicon-oxygen composite anode material is composite particles, the composite particles comprise silicon-oxygen powder, carbon nano tubes and conductive carbon layers, wherein the chemical formula of the silicon-oxygen powder is SiOx, and the value range of x meets the following conditions: x is more than or equal to 0.6 and less than or equal to 1.4, and nano silicon is distributed in the particles of the silicon oxide powder; the conductive carbon layer is coated on the surface of the silicon oxide powder; the carbon nano tube is perpendicular to the particle surface of the silicon oxide powder and penetrates through the conductive carbon layer. In addition, the Chinese patent application number is CN202210337601.6, and the patent name is 'a lithium ion battery silicon-oxygen composite anode material and a preparation method thereof', and the silicon-oxygen composite anode material provided by the invention comprises three parts, namely a silicon-oxygen powder inner core, a fast ion conductor layer and a conductive carbon layer, wherein the chemical formula of the silicon-oxygen powder inner core is SiOx (x is more than or equal to 0.6 and less than or equal to 1.1). The surface of the silica particles in the silica composite anode material is provided with two layers of shells, the first layer of shells is a fast ion conductor, the fast ion conductor is a continuous phase, the expansion of the particles can be restrained, and the shells can inhibit the expansion and the contraction of the materials, so that the SEI film on the surface of the silica composite anode material particles is stabilized; the second shell is a conductive carbon layer, and the second shell can ensure that the silicon-oxygen composite anode material particles have good electric contact activity. The problems with the above patents are: the densification degree of the coating material is low, the isotropy is poor, the impedance of the material is larger, and the cycle performance of the material is influenced.
Disclosure of Invention
The invention aims at overcoming the defects in the prior art, and provides a preparation method of a silicon-oxygen composite material for a lithium ion battery, which mainly deposits amorphous carbon and carbon nano tubes on the surface of silicon oxygen through phenolic aldehyde reaction, improves the interface impedance and reduces the expansion.
The invention relates to a preparation method of a silicon-oxygen composite material for a lithium ion battery, which adopts the following technical scheme: the method comprises the following steps:
(1) Adding ferrocenyl formaldehyde into an organic solution to prepare a solution with the weight percent of 0.5-5%, and then adding a silicon oxide material and a dispersing agent to uniformly disperse to obtain a solution A;
mass ratio, ferrocenyl formaldehyde: silica: dispersant=1-10:100:0.5-2;
(2) Dripping a phenolic solution and an organic catalyst into the solution A, uniformly dispersing by ultrasonic, transferring into a high-pressure reaction kettle, carrying out hydrothermal reaction for 6-24 hours at the temperature of 100-200 ℃, washing by adopting 0.1mol/L dilute hydrochloric acid, carrying out vacuum drying for 24 hours at the temperature of 80 ℃, and crushing to obtain a composite material B;
mass ratio, solution a: phenolic solution: organic catalyst=100:1-10:0.5-2;
(3) Transferring the composite material B into a tube furnace, introducing inert gas to remove air in the tube, introducing carbon source gas, and carbonizing at 700-1100 ℃ for 1-6h to obtain the silicon-oxygen composite material.
Preferably, the dispersing agent in the step (1) is one of aminotrimethylene phosphoric acid, polyacrylamide and sodium polyacrylate.
Preferably, the organic catalyst in the step (2) is one of ethylene oxide, propylene oxide and cyclohexyl oxide.
Preferably, the phenol in the step (2) is one of phenol, aminophenol and naphthol.
Preferably, the carbon source gas in the step (3) is one of methane, acetylene and ethane.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, ferrocenyl formaldehyde is coated on the surface of nano silicon through chemical reaction, and amorphous carbon is deposited by phenolic reaction by taking the ferrocenyl formaldehyde as a matrix, so that the method has the advantages of controllable process, high density, high isotropy, low impedance and the like; meanwhile, ferrocene in ferrocene formaldehyde has a catalytic effect, provides a foundation for the subsequent vapor deposition of carbon nanotubes, and the obtained carbon nanotubes form a network structure to restrict the expansion of silicon in the charge and discharge processes.
Drawings
FIG. 1 is an SEM image of a silica composite prepared according to example 1.
Detailed Description
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present invention only, and are not intended to limit the present invention.
Example 1 the preparation method of the silicon oxide composite material for the lithium ion battery provided by the invention comprises the following steps:
(1) 5g of ferrocene formaldehyde is added into 250g of cyclohexane organic solution to prepare 2wt% solution, and then 100g of silica material and 1g of amino-trimethoprim acid are added to be uniformly dispersed to obtain solution A;
(2) Dripping 5g of phenol and 1g of ethylene oxide into 100ml of solution A, uniformly dispersing by ultrasonic, transferring into a high-pressure reaction kettle, carrying out hydrothermal reaction for 12 hours at the temperature of 150 ℃, washing by adopting 0.1mol/L of dilute hydrochloric acid, drying in vacuum at 80 ℃ for 24 hours, and crushing to obtain a composite material B;
(3) Transferring the composite material B into a tube furnace, introducing argon inert gas to remove air in the tube, introducing methane carbon source gas, and carbonizing at 950 ℃ for 3 hours to obtain the silicon-oxygen composite material.
Example 2 the preparation method of the silicon oxide composite material for the lithium ion battery provided by the invention comprises the following steps:
(1) 1g of ferrocene formaldehyde is added into 200ml of N-methyl pyrrolidone organic solution to prepare 0.5wt% solution, and then 100g of silicon oxygen material and 0.5g of polyacrylamide are added to obtain solution A after uniform dispersion;
(2) Dripping 1g of aminophenol and 0.5g of propylene oxide into 100ml of solution A, uniformly dispersing by ultrasonic, transferring into a high-pressure reaction kettle, carrying out hydrothermal reaction at 100 ℃ for 24 hours, washing by adopting 0.1mol/L of dilute hydrochloric acid, drying at 80 ℃ in vacuum for 24 hours, and crushing to obtain a composite material B;
(3) Transferring the composite material B into a tube furnace, introducing argon inert gas to remove air in the tube, introducing acetylene carbon source gas, and carbonizing at 700 ℃ for 6 hours to obtain the silicon-oxygen composite material.
Example 3 the preparation method of the silicon oxide composite material for the lithium ion battery provided by the invention comprises the following steps:
(1) Adding 10g of ferrocene formaldehyde into 200ml of carbon tetrachloride organic solution to prepare 5wt% solution, and then adding 100g of silica material and 2g of sodium polyacrylate to uniformly disperse to obtain solution A;
(2) Dropwise adding 10g of naphthol and 2g of epoxy cyclohexyl into 100ml of solution A, uniformly dispersing by ultrasonic, transferring into a high-pressure reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 6 hours, washing by adopting 0.1mol/L of dilute hydrochloric acid, carrying out vacuum drying at 80 ℃ for 24 hours, and crushing to obtain a composite material B;
(3) Transferring the composite material B into a tube furnace, introducing argon inert gas to remove air in the tube, introducing ethane carbon source gas, and carbonizing for 1h at 1100 ℃ to obtain the silicon-oxygen composite material.
Comparative example:
100g of silicon-oxygen material and 1g of nano nickel are uniformly mixed, then the mixture is transferred into a tube furnace, argon inert gas is introduced to remove air in the tube, then methane carbon source gas is introduced, and carbonization is carried out for 3 hours at the temperature of 950 ℃ to obtain the silicon-oxygen composite material.
Performance measurement:
(1) Topography testing
SEM testing was performed on the silicone composite of example 1, and the test results are shown in fig. 1. As can be seen from FIG. 1, the material has a granular structure, and the size distribution of the material particles is uniform, reasonable and smooth, and the particle size is between 3 and 7 mu m.
(2) Button cell testing
The silicon-oxygen composite materials in examples 1 to 3 and comparative examples were assembled as negative electrode materials for lithium ion batteries to form button cells, which were designated as A1, A2, A3, and B1, respectively.
The preparation method comprises the following steps: in the lithium ion battery cathode materialAdding binder, conductive agent and solvent into the material, stirring and pulping, coating the mixture on copper foil, and drying and rolling the mixture to prepare a negative plate; the binder is LA132, the conductive agent is SP, the solvent is NMP, and the dosage ratio of the anode material to SP, PVDF, NMP is 95g:1g:4g:220mL; liPF in electrolyte 6 As electrolyte, a mixture of EC and DEC in a volume ratio of 1:1 is used as a solvent; the metal lithium sheet is a counter electrode, and the diaphragm adopts a polypropylene (PP) film. The button cell assembly was performed in an argon filled glove box. Electrochemical performance was carried out on a wuhan blue electric CT2001A type battery tester with a charge-discharge voltage ranging from 0.005V to 2.0V and a charge-discharge rate of 0.1C.
The test results are shown in Table 1.
TABLE 1
As can be seen from the data in table 1, the specific capacity and the first time efficiency of the silica composite material prepared in the examples of the present invention are significantly better than those of the comparative examples. The reasons for this may be: amorphous carbon deposited by phenolic aldehyde chemical reaction has the characteristics of high density, low impedance, good isotropy and the like, so that the tap density is reduced, the powder conductivity is high, and meanwhile, the reduced impedance improves the exertion of specific capacity of the material and the primary efficiency.
(3) Soft package battery test:
the silicon-oxygen composite materials in examples 1-3 and comparative example are doped with 90% of artificial graphite as a negative electrode material to prepare a negative electrode plate, and NCM532 is used as a positive electrode material; liPF in electrolyte 6 As electrolyte, a mixture of EC and DEC in a volume ratio of 1:1 is used as a solvent; a5 Ah soft package battery, labeled C1, C2, C3, D1, was prepared using Celgard 2400 membrane as the separator. And respectively testing the liquid absorption and retention capacity, the reverse elasticity and the cycle performance of the negative plate.
a. Liquid absorption capacity test
And (3) adopting a 1mL burette, sucking electrolyte VmL, dripping one drop on the surface of the pole piece, timing until the electrolyte is absorbed, recording time t, and calculating the liquid suction speed V/t of the pole piece. The test results are shown in Table 2.
b. Liquid retention rate test
Calculating theoretical liquid absorption m of the pole piece according to the pole piece parameters 1 And weigh the weight m of the pole piece 2 Then the pole piece is placed into electrolyte to be soaked for 24 hours, and the weight of the pole piece is weighed to be m 3 Calculating the liquid absorption m of the pole piece 3 -m 2 And calculated according to the following formula: retention = (m) 3 -m 2 ) 100%/m1. The test results are shown in Table 2.
TABLE 2
As can be seen from Table 2, the liquid absorption and retention capacities of the silicone composites obtained in examples 1-3 are significantly higher than those of the comparative examples. Experimental results show that the silica composite material has higher liquid absorption and retention capacity. The reasons for this may be: the material of the embodiment has high specific surface area, thereby improving the liquid absorbing and retaining capacity of the material.
c. Pole piece rebound rate test
Firstly, testing the average thickness D1 of a pole piece by adopting a thickness gauge, then placing the pole piece in a vacuum drying oven at 80 ℃ for drying for 48 hours, testing the thickness D2 of the pole piece, and calculating according to the following formula: rebound rate= (D2-D1) ×100%/D1. The test results are shown in Table 3.
d. Pole piece resistivity test
The resistivity of the pole pieces was measured using a resistivity tester, and the test results are shown in table 3.
TABLE 3 Table 3
As can be seen from the data in Table 3, the negative electrode sheets prepared using the silica composites obtained in examples 1-3 have significantly lower rebound and resistivity than comparative examples 1 and 2, i.e., the negative electrode sheets prepared using the inventive silica-carbon composites have lower rebound and resistivity. The reasons for this may be: the amorphous carbon on the surface of the silicon-oxygen composite material in the embodiment has high isotropy, reduces the expansion and rebound, has low powder conductivity, and reduces the resistivity of the pole piece.
e. Cycle performance test
The cycle performance of the battery was tested at 25.+ -. 3 ℃ with a charge/discharge rate of 1C/1C and a voltage range of 2.5V-4.2V. The test results are shown in Table 4.
TABLE 4 Table 4
As can be seen from Table 4, the cycle performance of the battery prepared from the silica composite material of the invention is obviously superior to that of the comparative example, and the reason is probably that the pole piece prepared from the silica composite material of the invention has lower expansion rate, and the structure of the pole piece is more stable in the charge and discharge process, so that the cycle performance of the pole piece is improved. In addition, the amorphous carbon coated on the surface of the silica composite material has the characteristics of high density, strong structural stability and isotropy, and the cycle performance of the silica composite material is improved.
The above description is only a few preferred embodiments of the present invention, and any person skilled in the art may make modifications to the above described embodiments or make modifications to the same. Accordingly, the corresponding simple modifications or equivalent changes according to the technical scheme of the present invention fall within the scope of the claimed invention.
Claims (4)
1. A preparation method of a silicon-oxygen composite material for a lithium ion battery is characterized by comprising the following steps:
(1) Adding ferrocenyl formaldehyde into an organic solution to prepare a solution with the weight percent of 0.5-5%, and then adding a silicon oxide material and a dispersing agent to uniformly disperse to obtain a solution A;
mass ratio, ferrocenyl formaldehyde: silica: dispersant=1-10:100:0.5-2;
(2) Dripping a phenolic solution and an organic catalyst into the solution A, uniformly dispersing by ultrasonic, transferring into a high-pressure reaction kettle, carrying out hydrothermal reaction for 6-24 hours at the temperature of 100-200 ℃, washing by adopting 0.1mol/L dilute hydrochloric acid, carrying out vacuum drying for 24 hours at the temperature of 80 ℃, and crushing to obtain a composite material B;
mass ratio, solution a: phenolic solution: organic catalyst=100:1-10:0.5-2;
(3) Transferring the composite material B into a tube furnace, then introducing inert gas to remove air in the tube, then introducing carbon source gas, and carbonizing for 1-6h at 700-1100 ℃ to obtain a silicon-oxygen composite material;
the dispersing agent in the step (1) is one of amino trimetaphosphate, polyacrylamide and sodium polyacrylate;
the organic solution in the step (1) is one of cyclohexane, N-methyl pyrrolidone and carbon tetrachloride.
2. The method for preparing the silicon-oxygen composite material for the lithium ion battery according to claim 1, which is characterized in that: the organic catalyst in the step (2) is one of ethylene oxide, propylene oxide and cyclohexyl oxide.
3. The method for preparing the silicon-oxygen composite material for the lithium ion battery according to claim 1, which is characterized in that: the phenols in the step (2) are one of phenol, aminophenol and naphthol.
4. The method for preparing the silicon-oxygen composite material for the lithium ion battery according to claim 1, which is characterized in that: and (3) the carbon source gas in the step (3) is one of methane, acetylene and ethane.
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