CN115986124B - Silicon-carbon composite material for lithium ion battery and preparation method thereof - Google Patents
Silicon-carbon composite material for lithium ion battery and preparation method thereof Download PDFInfo
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- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 57
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 19
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000077 silane Inorganic materials 0.000 claims abstract description 17
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 150000007524 organic acids Chemical class 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 6
- 230000021523 carboxylation Effects 0.000 claims description 6
- 238000006473 carboxylation reaction Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- OISVCGZHLKNMSJ-UHFFFAOYSA-N 2,6-dimethylpyridine Chemical compound CC1=CC=CC(C)=N1 OISVCGZHLKNMSJ-UHFFFAOYSA-N 0.000 claims description 4
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 4
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- 150000003927 aminopyridines Chemical class 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 claims description 2
- HPYNZHMRTTWQTB-UHFFFAOYSA-N dimethylpyridine Natural products CC1=CC=CN=C1C HPYNZHMRTTWQTB-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 abstract description 7
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 238000012360 testing method Methods 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- 229910052710 silicon Inorganic materials 0.000 description 13
- 239000010703 silicon Substances 0.000 description 13
- 238000005336 cracking Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003792 electrolyte Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 239000013543 active substance Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000007773 negative electrode material Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000011149 active material Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- 101150058243 Lipf gene Proteins 0.000 description 2
- QZKDJVMWPRBTMV-UHFFFAOYSA-N argon quinoline Chemical compound N1=CC=CC2=CC=CC=C12.[Ar] QZKDJVMWPRBTMV-UHFFFAOYSA-N 0.000 description 2
- GZCHAGSCCHLLJZ-UHFFFAOYSA-N argon;pyridin-2-amine Chemical compound [Ar].NC1=CC=CC=N1 GZCHAGSCCHLLJZ-UHFFFAOYSA-N 0.000 description 2
- UBOIOTWHERUBJL-UHFFFAOYSA-N argon;pyridine Chemical compound [Ar].C1=CC=NC=C1 UBOIOTWHERUBJL-UHFFFAOYSA-N 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001228 Li[Ni1/3Co1/3Mn1/3]O2 (NCM 111) Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
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- 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
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Abstract
The invention relates to the technical field of preparation of lithium ion battery materials, and provides a silicon-carbon composite material for a lithium ion battery and a preparation method thereof. The preparation method of the silicon-carbon composite material for the lithium ion battery comprises the following steps: s1, carboxylating the activated carbon by using organic acid to obtain carboxylated activated carbon; s2, under negative pressure, silane gas is cracked and deposited in carboxylated activated carbon to obtain a nano silicon/activated carbon composite material; and S3, depositing the carbon source mixed gas on the nano silicon/activated carbon composite material to obtain the silicon-carbon composite material. The silicon-carbon composite material for the lithium ion battery is prepared by the preparation method. By the technical scheme, the problems of large expansion and poor cycle performance of the silicon-carbon material prepared in the prior art are solved.
Description
Technical Field
The invention relates to the technical field of lithium ion battery material preparation, in particular to a silicon-carbon composite material for a lithium ion battery and a preparation method thereof.
Background
The silicon-carbon material has high energy density and wide material source and is applied to the fields of electric tools, digital codes and the like, but the defects of high full-charge expansion, poor cycle performance and the like can not meet the requirements of the fields of electric automobiles and the like. The reason why the silicon-carbon material expands is mainly that nano silicon grains in the silicon-carbon material are larger, so that the reduction of the expansion of the silicon-carbon material is required to start from the aspect of reducing the size of the silicon grains.
The nano silicon prepared by the silane cracking method has the advantages of small silicon crystal grain (3 nm), low expansion, high specific capacity and the like, and becomes a proper material for reducing the expansion of silicon and carbon, but because the silicon crystal grain is small and has high activity, the contact between the silicon crystal grain and the outside air is required to be reduced by cladding, the side reaction is reduced, the high-temperature performance is improved, meanwhile, the impedance of the silicon and carbon prepared by the silane cracking method is higher, the preparation condition is harsh, the preparation period is long, and the industrialized application of the silicon and carbon is influenced.
Disclosure of Invention
The invention provides a silicon-carbon composite material for a lithium ion battery and a preparation method thereof, which solve the problems of swelling and poor cycle performance of the silicon-carbon material prepared in the prior art.
The technical scheme of the invention is as follows:
the preparation method of the silicon-carbon composite material for the lithium ion battery comprises the following steps:
s1, carboxylating the activated carbon by using organic acid to obtain carboxylated activated carbon;
s2, under negative pressure, silane gas is cracked and deposited in carboxylated activated carbon to obtain a nano silicon/activated carbon composite material;
and S3, depositing the carbon source mixed gas on the nano silicon/activated carbon composite material to obtain the silicon-carbon composite material.
As a further technical scheme, in the S1, the reaction temperature of carboxylation is 50-150 ℃ and the reaction time is 1-6 h.
As a further technical scheme, in the S1, the mass ratio of the activated carbon to the organic acid is 1:10-50.
As a further technical scheme, in the S1, the particle size of the porous carbon material in the activated carbon is 1-20 mu m, the porosity is 20% -60%, and the specific surface area is 100-500 m 2 /g。
As a further technical scheme, in the S1, the organic acid is one or more of tartaric acid, citric acid and acetic acid.
As a further technical scheme, in the S2, the negative pressure is minus 0.9 to minus 0.1MPa.
As a further technical scheme, in the step S2, the deposition temperature is 200-500 ℃, and the deposition time is 1-6 hours.
As a further technical scheme, in the step S3, the deposition temperature is 500-700 ℃ and the deposition time is 30-240 min.
As a further technical scheme, in S3, the carbon source mixed gas is a mixed gas of a carbon source gas and argon, and the carbon source gas is one of a pyridine gas, an aminopyridine gas, a picoline gas, a lutidine gas, a pyrimidine gas, a quinoline gas, a piperazine gas, or a piperidine gas.
The invention also provides a silicon-carbon composite material for the lithium ion battery, which is prepared according to the preparation method of the silicon-carbon composite material for the lithium ion battery.
The working principle and the beneficial effects of the invention are as follows:
1. according to the invention, the surface of the activated carbon is subjected to carboxylation modification, so that the defect of the surface of the activated carbon is reduced, nano silicon obtained by cracking silane is easier to deposit in the pores of the activated carbon, and meanwhile, after carboxylation, the nano silicon is less in the nano pore diameter, so that the nano silicon is easier to deposit in the pores of the activated carbon, the expansion of the silicon is restrained, the compactness of the silicon-carbon composite material is improved, and the tap density and the powder conductivity of the silicon-carbon composite material are improved, so that the cycle performance of the silicon-carbon composite material is improved, and the expansion of the silicon-carbon composite material is reduced.
2. In the invention, the silane cracking is performed under negative pressure, so that the size of silicon grains is reduced, the expansion of the silicon-carbon composite material is reduced, and the first efficiency of the silicon-carbon composite material is improved.
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
Fig. 1 is an SEM image of a silicon carbon composite material prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
S1, adding 100g of activated carbon into 300g of tartaric acid, reacting for 3 hours at the temperature of 100 ℃, filtering, and vacuum drying for 24 hours at the temperature of 80 ℃ to obtain carboxylated activated carbon; wherein the particle diameter of the activated carbon is 10 mu m, the porosity is 40%, and the specific surface area is 200m 2 /g；
S2, transferring carboxylated activated carbon into a vacuum reaction kettle, and introducing SiH under negative pressure of-0.5 Mpa at a flow rate of 100mL/min by a silane cracking method 4 Silane gas is deposited in carboxylated activated carbon at 300 ℃ for 3 hours to obtain a nano silicon/activated carbon composite material;
s3, transferring the nano silicon/activated carbon composite material into a tube furnace, and introducing a pyridine-argon mixed gas, wherein the volume ratio of pyridine to argon in the pyridine-argon mixed gas is 1: and 10, depositing at 600 ℃ for 120min to obtain the silicon-carbon composite material.
Example 2
S1, adding 10g of activated carbon into 100g of citric acid, reacting for 6 hours at 50 ℃, filtering, and vacuum drying for 24 hours at 80 ℃ to obtain carboxylated activated carbon; wherein the particle diameter of the activated carbon is 1 mu m, the porosity is 60%, and the specific surface area is 1500m 2 /g；
S2, transferring carboxylated activated carbon into a vacuum reaction kettle, and introducing SiH under negative pressure of-0.1 Mpa at a flow rate of 100mL/min by a silane cracking method 4 Silane gas is deposited in carboxylated activated carbon at 200 ℃ for 6 hours to obtain a nano silicon/activated carbon composite material;
s3, transferring the nano silicon/activated carbon composite material into a tube furnace, and introducing aminopyridine argon mixed gas, wherein the volume ratio of aminopyridine to argon in the aminopyridine argon mixed gas is 1: and 10, depositing at 500 ℃ for 240min to obtain the silicon-carbon composite material.
Example 3
S1, adding 10g of activated carbon into 300g of tartaric acid, reacting for 1h at 150 ℃, filtering, and vacuum drying at 80 ℃ for 24h to obtain carboxylated activated carbon; wherein the particle diameter of the activated carbon is 20 mu m, the porosity is 20%, and the specific surface area is 100m 2 /g；
S2, transferring carboxylated activated carbon into a vacuum reaction kettle, and introducing SiH under negative pressure of-0.9 Mpa at a flow rate of 100mL/min by a silane cracking method 4 Silane gas is deposited in carboxylated activated carbon at 500 ℃ for 1h to obtain a nano silicon/activated carbon composite material;
s3, transferring the nano silicon/activated carbon composite material into a tube furnace, and introducing a quinoline-argon mixed gas, wherein the volume ratio of quinoline to argon in the quinoline-argon mixed gas is 1: and 10, depositing at 700 ℃ for 30min to obtain the silicon-carbon composite material.
Comparative example 1
Transferring the activated carbon into a vacuum reaction kettle, and introducing SiH at a flow rate of 100mL/min under normal pressure by a silane cracking method 4 And (3) depositing silane gas in the activated carbon at 600 ℃ for 3 hours to obtain the silicon-carbon composite material.
The following tests were performed on the resulting silicon carbon composite material:
1. SEM test
SEM test of the silicon carbon composite material of example 1 shows that the particle size of the silicon carbon composite material obtained in example 1 is 5 to 15. Mu.m, as can be seen from the graph.
2. Physical and chemical property test
According to the method specified in the national standard GB/T38823-2020 silicon charcoal, the silicon carbon composite materials obtained in examples 1-3 and comparative example 1 are subjected to performance tests such as powder conductivity, tap density, specific surface area, granularity D50 and the like, and meanwhile, the silicon grain size of the materials is tested by XRD, and the test results are shown in Table 1:
TABLE 1 physicochemical Property test results
As can be seen from table 1, compared with the silicon-carbon composite material of comparative example 1, the powder conductivity of the silicon-carbon composite material of examples 1 to 3 is significantly improved, the tap density and specific surface area are increased, and the silicon grain size is reduced, which indicates that the tap density, specific surface area and powder conductivity of the silicon-carbon composite material prepared by the method of examples 1 to 3 are significantly improved, because in the preparation method of examples 1 to 3, the activated carbon is subjected to carboxylation modification, the carboxylated activated carbon reduces the surface defects, so that nano silicon obtained by silane pyrolysis is easier to deposit in the pores of the silicon-carbon composite material, and meanwhile, after carboxylation, the nano pore diameter of the activated carbon is smaller, so that nano silicon is easier to deposit in the pores of the silicon-carbon composite material, and the tap density and powder conductivity of the silicon-carbon composite material are improved; in addition, the silane cracking deposition is carried out under negative pressure in the preparation method, so that the silicon crystal grain growth is smaller.
3. Button cell testing
The silicon-carbon composite materials of examples 1 to 3 and comparative example 1 were used as active materials to prepare pole pieces according to the following method: adding 9g of active substances, 0.5g of conductive agent SP and 0.5g of binder LA133 into 220mL of deionized water, uniformly stirring to obtain slurry, and coating the slurry on a copper foil current collector to obtain a pole piece; and the pole piece with the silicon-carbon composite material of example 1 as an active substance is marked as A, the pole piece with the silicon-carbon composite material of example 2 as an active substance is marked as B, the pole piece with the silicon-carbon composite material of example 3 as an active substance is marked as C, and the pole piece with the silicon-carbon composite material of comparative example 1 as an active substance is marked as D.
Respectively taking the pole pieces A-D as positive electrodes, and assembling the positive electrodes, the lithium pieces, the electrolyte and the diaphragm into a button cell in a glove box with oxygen and water content lower than 0.1ppm, and marking the button cell as A-1, B-1, C-1 and D-1; wherein the separator is cellegard 2400; the electrolyte is LiPF 6 EC+DMC, liPF in electrolyte 6 The concentration of (C) is 1.2mol/L, and the weight ratio of EC to DMC is 1:1.
the performance of the button cell is tested by adopting a blue-ray tester, and the test conditions are as follows: the charge and discharge rate of 0.1C is 0.005-2V, the cycle is stopped after 3 weeks, then the full-charge expansion of the negative electrode plate is tested, and the test results are shown in the following table:
table 2 button cell test results
As can be seen from the data in the above table, compared with the button cell prepared by using the silicon-carbon composite material of comparative example 1 as the active material, the first discharge capacity and the first efficiency of the button cell prepared by using the silicon-carbon composite material of examples 1 to 3 as the active material are remarkably improved, and the full-charge expansion is remarkably reduced, which means that the preparation method of examples 1 to 3 of the present invention can remarkably improve the first efficiency of the silicon-carbon composite material and reduce the expansion of the silicon-carbon composite material.
4. Soft package battery test
Respectively taking the silicon-carbon composite materials of examples 1-3 and comparative example 1 doped with 90% of artificial graphite as a negative electrode material, and assembling the negative electrode material, the positive electrode material, the electrolyte and the diaphragm into a soft package battery of 5Ah, and marking the soft package battery as A-2, B-2, C-2 and D-2; wherein the positive electrode material is LiNi 1/3 Co 1/3 Mn 1/3 O 2 The electrolyte is LiPF 6 EC+DEC, liPF in electrolyte 6 The concentration of (C) is 1.3mol/L, and the volume ratio of EC to DEC is 1:1.
the assembled pouch cell was subjected to the following performance tests:
(1) Dissecting the soft package battery after constant volume, testing the thickness D1 of the negative pole piece, cycling each soft package battery for 100 times (1C/1 C@25+/-3 ℃ @2.5-4.2V), fully charging the soft package battery, dissecting the thickness D2 of the negative pole piece after the cycling again, and calculating the expansion rate according to the following formula:
expansion ratio =
，
(2) And (3) performing cycle performance test and multiplying power test on the soft package battery: the cycle performance test conditions were: the charge-discharge voltage range is 2.5-4.2V, the temperature is 25+/-3.0 ℃, and the charge-discharge multiplying power is 1.0C/1.0C; multiplying power test: testing the constant current ratio of the material under the condition of 2C;
the test results are shown in table 3:
table 3 soft pack battery test results
As can be seen from the data in the above table, compared with the soft-pack battery prepared by using the silicon-carbon composite material of comparative example 1 as the negative electrode material, the soft-pack battery prepared by using the silicon-carbon composite material of examples 1 to 3 as the negative electrode material has significantly improved cycle performance, and the expansion rate of the negative electrode sheet is significantly reduced, and the preparation method of examples 1 to 3 is illustrated to significantly reduce the expansion of the silicon-carbon composite material and improve the cycle performance of the silicon-carbon composite material.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. The preparation method of the silicon-carbon composite material for the lithium ion battery is characterized by comprising the following steps of:
s1, carboxylating the activated carbon by using organic acid to obtain carboxylated activated carbon;
s2, under negative pressure, silane gas is cracked and deposited in carboxylated activated carbon to obtain a nano silicon/activated carbon composite material;
s3, depositing the carbon source mixed gas on the nano silicon/activated carbon composite material to obtain a silicon-carbon composite material;
in the step S1, the reaction temperature of carboxylation is 50-150 ℃ and the reaction time is 1-6 h;
in the step S1, the mass ratio of the activated carbon to the organic acid is 1:10-50.
2. The method for preparing the silicon-carbon composite material for the lithium ion battery according to claim 1, wherein in the S1, the particle size of the activated carbon is 1-20 μm, the porosity is 20% -60%, and the specific surface area is 100-500 m 2 /g。
3. The method for preparing a silicon-carbon composite material for a lithium ion battery according to claim 1, wherein in S1, the organic acid is one or more of tartaric acid, citric acid and acetic acid.
4. The method for preparing the silicon-carbon composite material for the lithium ion battery according to claim 1, wherein in the step S2, the negative pressure is minus 0.9 to minus 0.1MPa.
5. The method for preparing the silicon-carbon composite material for the lithium ion battery according to claim 1, wherein in the step S2, the deposition temperature is 200-500 ℃ and the deposition time is 1-6 h.
6. The method for preparing the silicon-carbon composite material for the lithium ion battery according to claim 1, wherein in the step S3, the deposition temperature is 500-700 ℃ and the deposition time is 30-240 min.
7. The method for preparing a silicon-carbon composite material for a lithium ion battery according to claim 1, wherein in S3, the carbon source mixed gas is a mixed gas of a carbon source gas and argon gas, and the carbon source gas is one of a pyridine gas, an aminopyridine gas, a picoline gas, a lutidine gas, a pyrimidine gas, a quinoline gas, a piperazine gas, or a piperidine gas.
8. The silicon-carbon composite material for the lithium ion battery, which is characterized by being prepared by the preparation method of the silicon-carbon composite material for the lithium ion battery according to any one of claims 1-7.
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| CN103545493A (en) * | 2013-11-01 | 2014-01-29 | 中南大学 | Preparation method of silicon/carbon multi-component composite negative electrode material |
| CN112340730A (en) * | 2020-11-24 | 2021-02-09 | 海南大学 | Preparation method of microporous carbon-rich material based on carboxylation anchoring effect |
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| CN104103821B (en) * | 2014-06-20 | 2016-08-24 | 浙江瓦力新能源科技有限公司 | The preparation method of silicon-carbon cathode material |
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Effective date of registration: 20231207 Address after: 653100 Longquan District, high tech Zone, Yuxi City, Yunnan Province (Sanjie community, Dajie street, Jiangchuan District) Patentee after: Yunnan Kuntian New Energy Co.,Ltd. Address before: 050000 No. 8, kuntian Avenue, Suyang Township, Yuanshi County, Shijiazhuang City, Hebei Province Patentee before: Hebei kuntian new energy Co.,Ltd. |