CN118495501A - Spherical porous silicon-carbon composite material and preparation method and application thereof - Google Patents
Spherical porous silicon-carbon composite material and preparation method and application thereof Download PDFInfo
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- CN118495501A CN118495501A CN202410540998.8A CN202410540998A CN118495501A CN 118495501 A CN118495501 A CN 118495501A CN 202410540998 A CN202410540998 A CN 202410540998A CN 118495501 A CN118495501 A CN 118495501A
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- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 52
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000077 silane Inorganic materials 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000000151 deposition Methods 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000004793 Polystyrene Substances 0.000 claims abstract description 14
- 239000004005 microsphere Substances 0.000 claims abstract description 14
- 229920002223 polystyrene Polymers 0.000 claims abstract description 14
- 229910003481 amorphous carbon Inorganic materials 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000012924 metal-organic framework composite Substances 0.000 claims abstract description 9
- 238000003763 carbonization Methods 0.000 claims abstract description 8
- 125000005842 heteroatom Chemical group 0.000 claims abstract description 8
- 238000002161 passivation Methods 0.000 claims abstract description 8
- 238000007740 vapor deposition Methods 0.000 claims abstract description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010000 carbonizing Methods 0.000 claims abstract description 6
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- -1 scandium methacrylate Chemical compound 0.000 claims description 7
- DBTMQFKUVICLQN-UHFFFAOYSA-K scandium(3+);triacetate Chemical compound [Sc+3].CC([O-])=O.CC([O-])=O.CC([O-])=O DBTMQFKUVICLQN-UHFFFAOYSA-K 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 6
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 6
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000013110 organic ligand Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- IQCIMEXIXLKXNO-UHFFFAOYSA-N propan-1-olate;scandium(3+) Chemical compound [Sc+3].CCC[O-].CCC[O-].CCC[O-] IQCIMEXIXLKXNO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052706 scandium Inorganic materials 0.000 claims description 5
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 4
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims description 4
- MSYLJRIXVZCQHW-UHFFFAOYSA-N formaldehyde;6-phenyl-1,3,5-triazine-2,4-diamine Chemical compound O=C.NC1=NC(N)=NC(C=2C=CC=CC=2)=N1 MSYLJRIXVZCQHW-UHFFFAOYSA-N 0.000 claims description 4
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 3
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 3
- HSSYVKMJJLDTKZ-UHFFFAOYSA-N 3-phenylphthalic acid Chemical compound OC(=O)C1=CC=CC(C=2C=CC=CC=2)=C1C(O)=O HSSYVKMJJLDTKZ-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 3
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 3
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 2
- YYQRGCZGSFRBAM-UHFFFAOYSA-N Triclofos Chemical compound OP(O)(=O)OCC(Cl)(Cl)Cl YYQRGCZGSFRBAM-UHFFFAOYSA-N 0.000 claims description 2
- 235000004279 alanine Nutrition 0.000 claims description 2
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims description 2
- 239000010405 anode material Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 2
- 229960001147 triclofos Drugs 0.000 claims description 2
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 230000003213 activating effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- 238000012360 testing method Methods 0.000 description 16
- 239000012621 metal-organic framework Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 238000005056 compaction Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 229910013870 LiPF 6 Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000005543 nano-size silicon particle Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000011148 porous material Substances 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
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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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
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01M4/36—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Composite Materials (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a spherical porous silicon-carbon composite material, and a preparation method and application thereof, and belongs to the technical field of lithium ion battery material preparation. The preparation method of the spherical porous silicon-carbon composite material comprises the following steps: adding polystyrene microspheres into a resin solution, adding scandium-metal organic framework composite materials, dispersing uniformly, carbonizing at 700-900 ℃ after drying, activating with water vapor at 1050-1250 ℃ to obtain a porous carbon material, transferring into a fluidized bed, heating to 400-600 ℃, introducing silane mixed gas, depositing for 30-300min under the negative pressure condition, introducing heteroatom gas for passivation, and depositing amorphous carbon by a vapor deposition method to obtain the silicon-carbon composite material. According to the invention, the compressive strength of the material is improved by utilizing the specific capacity of the internal scandium-doped lifting material and the porous structure formed after carbonization of the metal frame, so that the expansion is reduced, and the cycle performance is improved.
Description
Technical Field
The invention relates to the technical field of lithium ion battery material preparation, in particular to a spherical porous silicon-carbon composite material and a preparation method and application thereof.
Background
The silicon-carbon material is used as a silicon-based material with high capacity, high first efficiency and low expansion, but the electron conductivity of the material is poor due to a porous structure, so that the quick charge performance and the compaction density of the material are reduced. The reason for the deviation of the quick charge performance of the material is mainly that the ionic or electronic conductivity of the material is poor, and the rate performance of the material is poor. The material with high electron conductivity is doped in the material core and the material with high electron or ion conductivity is coated in the material shell. Meanwhile, the silicon carbon is in a granular structure, so that the compressive capacity deviation of the material is caused, and the compaction density of the material is reduced. Compared with the granular structure, the spherical structure has strong deformation capability, so that the material has strong pressure resistance; however, the spherical structure causes deviation of electronic conductivity due to small contact area between the balls, affects the rate performance of the spherical structure, and needs to be doped to improve the rate performance of the material.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a spherical porous silicon-carbon composite material, and a preparation method and application thereof, and solves the technical problems of low compaction density and energy density and poor quick charge performance of the silicon-carbon material.
In order to achieve the above purpose, the technical scheme adopted by the invention comprises the following steps:
the technical purpose of the first aspect of the invention is to provide a preparation method of a spherical porous silicon-carbon composite material, which comprises the following steps:
Uniformly mixing carboxylated polystyrene microspheres, a resin solution and a scandium-metal organic framework composite material, drying, and sequentially carbonizing and pore-forming to obtain a porous carbon material;
And depositing the porous carbon material in the mixed gas of silane and nitrogen by adopting a vapor deposition method, passivating in the heteroatom gas, and finally depositing amorphous carbon in the carbon source gas to obtain the porous carbon material.
According to the invention, the scandium-metal organic framework structure is prepared, nano silicon is deposited and passivated, and the spherical porous silicon-carbon composite material is prepared by coating. According to the invention, the specific capacity of the material is improved by utilizing the scandium doped inside, and the compressive strength of the material can be improved by the porous structure formed after carbonization of the metal frame, so that the expansion is reduced, and the cycle performance is improved.
Further, the preparation method of the scandium-metal organic framework composite material comprises the following steps: according to the mass ratio, the metal salt: organic ligand: functional material: the organic solvent is 10-50:100:1-5:500-1000, adding metal salt, organic ligand and functional material into organic solvent, dispersing uniformly; then ball milling and dispersing for 60-600min under the conditions of 50-120 ℃ and 10-100 rpm; and finally, washing with DMF and dichloromethane respectively and drying to obtain the product.
Further, the metal salt comprises one or more than two of scandium n-propoxide, scandium methacrylate, scandium acetate, scandium n-propoxide, scandium methacrylate, scandium alanine, scandium acetate or scandium acetate; the organic ligand comprises one or more than two of terephthalic acid, biphenyl dicarboxylic acid, 2-methylimidazole, trimesic acid or tetra-carboxyl phenyl porphyrin; the functional material comprises one or more than two organic phosphorus compounds selected from trimethyl phosphate, triethyl phosphate, triphenyl phosphate, tributyl phosphate and trichloroethyl phosphate; the organic solvent comprises one or more of diethyl ether, dimethyl ether, ethylene glycol dimethyl ether, dibutyl ether or isopropyl ether.
Further, the mass ratio of the carboxylated polystyrene microspheres to the resin solution to the scandium-metal organic framework composite material is 5-20:100:1-10;
the resin in the resin solution is one or more than two of urea formaldehyde resin, melamine formaldehyde resin or benzoguanamine formaldehyde resin; the solvent of the resin solution is one or more of benzene, methylene dichloride or dimethylbenzene;
In the resin solution, the concentration of the resin is 1-5wt%.
Further, the carbonization temperature is 700-900 ℃, and the carbonization time is 1-6 hours;
The pore-forming method comprises the following steps: the temperature is raised to 1050-1250 ℃ and steam is introduced for 1-6h.
Further, the temperature of the porous carbon material deposited in the mixed gas of silane and nitrogen is 400-600 ℃, the pressure is-0.05 to-0.1 Mpa, and the deposition time is 30-300min;
In the mixed gas of silane and nitrogen, the volume ratio of the silane to the nitrogen is 0.5-2:10;
The flow rate of the mixed gas of silane and nitrogen is 100-500mL/min.
Further, the heteroatom gas comprises one or more than two of ammonia gas, phosphine gas, sulfur dioxide gas or hydrogen boride gas;
the passivation temperature is 400-600 ℃, the passivation time is 30-300min, and the flow rate of the heteroatom gas introduced during passivation is 100-500mL/min.
Further, the carbon source gas comprises one or more than two of methane gas, ethane gas, acetylene gas or ethylene gas;
The amorphous carbon is deposited at 600-800 deg.c for 30-300min.
Specifically, the preparation method of the spherical porous silicon-carbon composite material comprises the following steps:
Step S1:
Carboxylated polystyrene microspheres according to the mass ratio: resin: scandium-metal organic framework=5-20: 100:1-10, adding carboxylated polystyrene microspheres into a resin solution with the weight percent of 1-5%, adding scandium-metal organic frameworks, dispersing uniformly, spray drying, transferring into a tube furnace, carbonizing for 1-6h at the temperature of 700-900 ℃, and heating to 1050-1250 ℃ for steam activation for 1-6h to obtain a porous carbon material;
Step S2:
Transferring the porous carbon material into a fluidized bed, heating to 400-600 ℃, then introducing silane mixed gas (volume ratio, silane: nitrogen=0.5-2:10, flow 100-500 ml/min), depositing for 30-300min under negative pressure, introducing heteroatom gas, passivating for 30-300min at 400-600 ℃ and flow 100-500ml/min, transferring into a rotary furnace, and introducing carbon source gas at 600-800 ℃ for amorphous carbon deposition for 30-300min by a vapor deposition method to obtain the silicon-carbon composite material.
The technical purpose of the second aspect of the invention is to provide a spherical porous silicon-carbon composite material prepared by the preparation method.
The technical purpose of the third aspect of the invention is to provide an application of a spherical porous silicon-carbon composite material in preparing a lithium ion battery anode material.
The implementation of the embodiment of the invention has the following beneficial effects:
1) The silicon-carbon composite material utilizes the specific capacity of the internal scandium-doped lifting material and the compressive strength of the porous structure formed after carbonization of the metal framework of the silicon-carbon composite material to reduce expansion.
2) The scandium-metal organic framework has the characteristics of high strength, high compressive capacity, high pore volume and the like, and the deposition amount of nano silicon is improved, so that the specific capacity of the material is improved; meanwhile, the porous structure formed after carbonization of the metal organic frame buffers the expansion of nano silicon in the charge and discharge process, so that the cycle performance is improved; and the scandium-metal framework contains the electronic conductivity of the scandium-promoting material, so that the rate performance is improved.
3) The carboxylated polystyrene microsphere has a spherical structure, and resin is coated on the surface of the material to form the spherical structure, so that the carboxylated polystyrene microsphere has the characteristics of high compaction density, low expansion and the like.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Wherein:
fig. 1 is an SEM image (2000×) of the silicon carbon composite material prepared in example 1.
Fig. 2 is an SEM image (500×) of the silicon carbon composite material prepared in example 1.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled 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
A method for preparing scandium-metal organic framework, comprising the following steps:
Adding 30g of scandium n-propoxide, 100g of terephthalic acid and 3g of trimethyl phosphate into 800g of dimethyl ether organic solvent, uniformly dispersing, then adding into a sand mill, performing ball milling, and dispersing for 300min under the conditions of 80 ℃ and 50 revolutions per minute to obtain a corresponding MOFs material; and then sequentially and respectively ultrasonically washing with DMF and dichloromethane, and finally drying in vacuum at 80 ℃ for 24 hours to obtain scandium-metal organic frame composite materials (MOFs for short).
A preparation method of spherical porous silicon-carbon composite material comprises the following steps:
Step S1:
10g of carboxylated polystyrene microspheres are added into 500g of methylene dichloride solution containing urea resin (the concentration of the urea resin is 2wt percent in the methylene dichloride solution containing urea resin), 5g of scandium-metal organic framework composite material prepared in the embodiment is added, uniformly dispersed, spray-dried, transferred into a tube furnace, carbonized for 3 hours at 800 ℃, and then heated to 1150 ℃ and activated for 3 hours by introducing steam (the flow rate is 100 mL/min), so as to obtain a porous carbon material;
Step S2:
Transferring the porous carbon material into a fluidized bed, heating to 500 ℃, then introducing a mixed gas of silane and nitrogen (volume ratio of silane: nitrogen=1:10, flow rate of 300 mL/min), depositing for 120min under negative pressure (-0.05 Mpa), then introducing ammonia gas, performing passivation treatment for 120min at 500 ℃ and flow rate of 300mL/min, transferring into a rotary furnace, and performing amorphous carbon deposition for 120min at 700 ℃ by introducing methane gas (flow rate of 100 mL/min) by a vapor deposition method to obtain the silicon-carbon composite material.
Example 2
A method for preparing scandium-metal organic framework complex, comprising the following steps:
Adding 10g of scandium methacrylate, 100g of biphenyl dicarboxylic acid and 1g of triethyl phosphate into 500g of ethylene glycol dimethyl ether, uniformly dispersing, adding into a sand mill, performing ball milling, and dispersing for 600min at the temperature of 50 ℃ and the speed of 10 r/min to obtain a corresponding MOFs material; and then sequentially and respectively ultrasonically washing with DMF and dichloromethane, and finally drying at 80 ℃ in vacuum for 24 hours to obtain scandium-metal organic frame composite materials (MOFs for short).
A preparation method of spherical porous silicon-carbon composite material comprises the following steps:
Step S1:
Adding 5g of carboxylated polystyrene microspheres into 1000g of a xylene solution containing melamine formaldehyde resin (the concentration of the melamine formaldehyde resin is 1wt percent), adding 1g of scandium-metal organic framework composite material prepared in the embodiment, uniformly dispersing, spray drying, transferring into a tube furnace, carbonizing for 6h at 700 ℃, and heating to 1050 ℃, and introducing steam (the flow rate is 100 mlL/min) to activate for 6h to obtain a porous carbon material;
Step S2:
transferring the porous carbon material into a fluidized bed, heating to 400 ℃, then introducing a mixed gas of silane and nitrogen (volume ratio, silane: nitrogen=0.5:10, flow rate of 100 mL/min), depositing for 300min under negative pressure (-0.05 Mpa), then introducing phosphine gas, passivating for 300min at 400 ℃ and flow rate of 100mL/min, transferring into a rotary furnace, and introducing ethylene gas (flow rate of 100 mL/min) at 600 ℃ for amorphous carbon deposition for 300min by a vapor deposition method to obtain the silicon-carbon composite material.
Example 3
A method for preparing scandium-metal organic framework, comprising the following steps:
Adding 50g scandium acetate, 100g 2-methylimidazole and 5g tributyl phosphate into 1000g dibutyl ether organic solvent, uniformly dispersing, adding into a sand mill, performing ball milling, and dispersing for 60min at the temperature of 120 ℃ and the speed of 100 rpm to obtain a corresponding MOFs material; and then sequentially and respectively ultrasonically washing with DMF and dichloromethane, and finally drying at 80 ℃ in vacuum for 24 hours to obtain scandium-metal organic frame composite materials (MOFs for short).
A preparation method of spherical porous silicon-carbon composite material comprises the following steps:
Step S1:
adding 20g of carboxylated polystyrene microspheres into 400g of benzene solution containing benzoguanamine formaldehyde resin (the concentration of benzoguanamine formaldehyde resin is 5wt percent), adding 10g of scandium-metal organic frame composite material prepared in the embodiment, uniformly dispersing, spray drying, transferring into a tube furnace, carbonizing for 1h at 900 ℃, and heating to 1250 ℃ to activate for 1h by steam (the flow rate is 100 mL/min) to obtain a porous carbon material;
Step S2:
transferring the porous carbon material into a fluidized bed, heating to 600 ℃, then introducing a mixed gas of silane and nitrogen (volume ratio, silane: nitrogen=2:10, flow rate of 500 mL/min), depositing for 30min under negative pressure (-0.05 Mpa), then introducing hydrogen boride gas, passivating for 30min at 600 ℃ and flow rate of 500mL/min, transferring into a rotary furnace, and introducing acetylene gas (flow rate of 100 mL/min) for amorphous carbon deposition for 30min at 800 ℃ by a vapor deposition method to obtain the silicon-carbon composite material.
Comparative example 1
This comparative example provides a method for producing a porous silicon-carbon composite material, which is different from example 1 in that scandium-metal organic framework complex is not added in step S1, and otherwise is the same as example 1.
Comparative example 2
This comparative example provides a method for preparing a porous silicon carbon composite material, which is different from example 1 in that carboxylated polystyrene microspheres are not added in step S1, and otherwise is the same as example 1.
Comparative example 3
As a comparative example, a granular silicon carbon material (manufacturer: lanxi Zhiden New energy technologies Co., ltd., model: SO 310) on the market was used.
To conduct comparative verification of the effects of the above examples and comparative examples, the composites obtained in the above examples 1 to 3 and comparative examples 1 to 3 were subjected to the following physicochemical tests according to the present application:
(1) SEM test: FIGS. 1-2 are SEM images of the silicon-carbon composite material prepared in example 1, and as can be seen from FIGS. 1-2, the material has a spherical structure and a core has a pore structure; the size of the material granularity D50 is between 5 and 10 mu m, and the size distribution is reasonable.
(2) Physical and chemical property test:
testing the specific surface area and tap density of each silicon-carbon composite material by referring to national standard GB/T38823-2020 silicon-carbon, testing the powder resistivity of each silicon-carbon composite material by adopting a four-probe tester, and testing the silicon grains of each silicon-carbon composite material by XRD; placing the powder material at 45 ℃ for 48 hours, and testing the gas production of the material; the test results are shown in table 1 below.
Button cell test:
The silicon-carbon composite materials corresponding to the examples 1-3 and the comparative examples 1-3 are used as negative electrode materials of lithium ion batteries to prepare button cells according to the following method:
Adding a binder, a conductive agent and a solvent into each corresponding silicon-carbon composite material, stirring and pulping, coating the mixture on a copper foil, and drying and rolling the mixture to prepare a negative plate; the adhesive is LA136D, the conductive agent is SP (conductive carbon black), the solvent is NMP, and the dosage ratio of SP to LA136D, NMP is 95g to 1g to 4g to 220mL; the electrolyte is a solution taking LiPF 6 as electrolyte, the concentration is 1mol/L, wherein the solvent adopts a mixture of EC and DEC with the volume ratio of 1:1; the metal lithium sheet is a counter electrode, and the diaphragm adopts a polypropylene (PP) film.
Each button cell is assembled in a glove box filled with argon, and then electrochemical performance is tested on a Wuhan blue electric CT2001A type cell tester, wherein the charge-discharge voltage range is 0.005V to 2.0V, and the charge-discharge rate is 0.1C; the test results are shown in Table 1 below.
The negative plate of the button cell is also subjected to full-charge expansion, and the specific test process is as follows: the rolled button cell pole piece was tested for the thickness D 1 of the negative pole piece, then the button cell was fully charged to the full charge thickness D 2 of the anatomical negative pole piece at 100% soc, and then the full charge expansion ratio was calculated (full charge expansion ratio= (D 2-D1)/D1 x 100%)), and the test results are shown in table 1 below.
TABLE 1
As can be seen from the data in the above Table 1, the silicon-carbon composite materials prepared in the embodiments 1 to 3 of the present application are significantly better than those of the comparative examples 1 to 3 in terms of the first efficiency, the full-charge expansion and the resistivity thereof, because the spherical structure prepared by doping the polystyrene microspheres in the materials reduces the expansion, and the scandium element is doped to reduce the impedance of the porous carbon, and the specific capacity of the materials is improved to exert and the first efficiency thereof.
(3) Soft package performance test:
The silicon-carbon composite materials corresponding to the examples 1-3 and the comparative examples 1-3 are doped with 95% of artificial graphite as a negative electrode material (namely, a negative electrode plate), and are assembled with a positive ternary material (LiNi 1/3Co1/3Mn1/3O2), an electrolyte and a diaphragm to form a soft-package battery of 5 Ah; wherein the diaphragm is celegard 2400, the electrolyte is LiPF 6 solution (the solvent is a mixed solution of EC and DEC with volume ratio of 1:1, and the concentration of LiPF 6 is 1.1 mol/L) to prepare the soft-package battery.
The following performance tests were performed on each of the pouch cells:
a. Multiplying power test: the constant current ratios of examples 1 to 3 and comparative examples 1 to 3 under 2C conditions were simultaneously tested, with constant current ratio=2c constant current capacity/(2c constant current capacity+0.1c constant voltage capacity).
B. And (3) testing the cycle performance: and carrying out cycle performance test on each prepared soft package battery, wherein the test conditions of the cycle performance test are as follows: the charge-discharge voltage range is 2.5-4.2V, the temperature is 25+/-3.0 ℃, the charge-discharge multiplying power is 1.0C/1.0C, and the cycle times are 500 times; the test results are shown in Table 2 below.
TABLE 2
| Constant current ratio of 2C | Cycle performance | |
| Example 1 | 93.7％ | 94.8％ |
| Example 2 | 92.2％ | 95.1％ |
| Example 3 | 94.3％ | 94.2％ |
| Comparative example 1 | 87.8％ | 91.6％ |
| Comparative example 2 | 89.9％ | 90.3％ |
| Comparative example 3 | 90.5％ | 89.5％ |
As can be seen from table 2 above, the rate capability, cycle performance and liquid absorption capacity of the soft-packed lithium ion batteries prepared by using the silicon-carbon composite materials provided in examples 1-3 are significantly better than those of comparative examples 1-3, because the materials of the examples have high specific surface area to improve the liquid absorption capacity of the materials and low full-charge expansion to improve the cycle performance. Meanwhile, scandium metal is doped in the material of the embodiment to reduce the powder resistivity, improve the constant current ratio of the material and improve the rate capability.
The foregoing disclosure is illustrative of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. The preparation method of the spherical porous silicon-carbon composite material is characterized by comprising the following steps of:
Uniformly mixing carboxylated polystyrene microspheres, a resin solution and a scandium-metal organic framework composite material, drying, and sequentially carbonizing and pore-forming to obtain a porous carbon material;
And depositing the porous carbon material in the mixed gas of silane and nitrogen by adopting a vapor deposition method, passivating in the heteroatom gas, and finally depositing amorphous carbon in the carbon source gas to obtain the porous carbon material.
2. The method of producing the scandium-metal organic framework composite material according to claim 1, comprising the steps of: according to the mass ratio, the metal salt: organic ligand: functional material: the organic solvent is 10-50:100:1-5:500-1000, adding metal salt, organic ligand and functional material into organic solvent, dispersing uniformly; then ball milling and dispersing for 60-600min under the conditions of 50-120 ℃ and 10-100 rpm; and finally, washing with DMF and dichloromethane respectively and drying to obtain the product.
3. The production method according to claim 2, wherein the metal salt comprises one or more of scandium n-propoxide, scandium methacrylate, scandium acetate, scandium n-propoxide, scandium methacrylate, scandium alanine, scandium acetate, or scandium acetate; the organic ligand comprises one or more than two of terephthalic acid, biphenyl dicarboxylic acid, 2-methylimidazole, trimesic acid or tetra-carboxyl phenyl porphyrin; the functional material comprises one or more than two organic phosphorus compounds selected from trimethyl phosphate, triethyl phosphate, triphenyl phosphate, tributyl phosphate and trichloroethyl phosphate; the organic solvent comprises one or more of diethyl ether, dimethyl ether, ethylene glycol dimethyl ether, dibutyl ether or isopropyl ether.
4. The preparation method according to claim 1, wherein the mass ratio of the carboxylated polystyrene microspheres, the resin solution and the scandium-metal organic framework composite material is 5-20:100:1-10;
the resin in the resin solution is one or more than two of urea formaldehyde resin, melamine formaldehyde resin or benzoguanamine formaldehyde resin; the solvent of the resin solution is one or more of benzene, methylene dichloride or dimethylbenzene;
In the resin solution, the concentration of the resin is 1-5wt%.
5. The method according to claim 1, wherein the carbonization temperature is 700 to 900 ℃ and the carbonization time is 1 to 6 hours;
The pore-forming method comprises the following steps: the temperature is raised to 1050-1250 ℃ and steam is introduced for 1-6h.
6. The preparation method according to claim 1, wherein the porous carbon material is deposited in a mixed gas of silane and nitrogen at a temperature of 400-600 ℃, a pressure of-0.05 to-0.1 Mpa, and a deposition time of 30-300min;
In the mixed gas of silane and nitrogen, the volume ratio of the silane to the nitrogen is 0.5-2:10;
The flow rate of the mixed gas of silane and nitrogen is 100-500mL/min.
7. The production method according to claim 1, wherein the heteroatom gas includes one or two or more of ammonia gas, phosphine gas, sulfur dioxide gas, or hydrogen boride gas;
the passivation temperature is 400-600 ℃, the passivation time is 30-300min, and the flow rate of the heteroatom gas introduced during passivation is 100-500mL/min.
8. The production method according to claim 1, wherein the carbon source gas comprises one or more of methane gas, ethane gas, acetylene gas, and ethylene gas;
The amorphous carbon is deposited at 600-800 deg.c for 30-300min.
9. A spherical porous silicon-carbon composite material prepared by the preparation method of any one of claims 1 to 8.
10. Use of the spherical porous silicon-carbon composite material according to claim 9 for preparing a lithium ion battery anode material.
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