CN107275599A - A kind of anode material for lithium-ion batteries and preparation method thereof - Google Patents
A kind of anode material for lithium-ion batteries and preparation method thereof Download PDFInfo
- Publication number
- CN107275599A CN107275599A CN201710393502.9A CN201710393502A CN107275599A CN 107275599 A CN107275599 A CN 107275599A CN 201710393502 A CN201710393502 A CN 201710393502A CN 107275599 A CN107275599 A CN 107275599A
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- Prior art keywords
- lithium
- anode material
- ion batteries
- graphene
- clad
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000010405 anode material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims description 12
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- 239000000178 monomer Substances 0.000 claims description 13
- 241000446313 Lamella Species 0.000 claims description 12
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 12
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- GZBSIABKXVPBFY-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OCC(CO)(CO)CO GZBSIABKXVPBFY-UHFFFAOYSA-N 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
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- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
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- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 2
- STUKNTHDFYCZOR-UHFFFAOYSA-N [Ba+2].[O-2].[Li+] Chemical compound [Ba+2].[O-2].[Li+] STUKNTHDFYCZOR-UHFFFAOYSA-N 0.000 claims description 2
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- 229910019142 PO4 Inorganic materials 0.000 description 1
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- 241000219000 Populus Species 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 150000008431 aliphatic amides Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000000217 alkyl group Polymers 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229960004050 aminobenzoic acid Drugs 0.000 description 1
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
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- 239000007998 bicine buffer Substances 0.000 description 1
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- 239000007767 bonding agent Substances 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- YQHLDYVWEZKEOX-UHFFFAOYSA-N cumene hydroperoxide Chemical compound OOC(C)(C)C1=CC=CC=C1 YQHLDYVWEZKEOX-UHFFFAOYSA-N 0.000 description 1
- FYLJKQFMQFOLSZ-UHFFFAOYSA-N cyclohexylperoxycyclohexane Chemical group C1CCCCC1OOC1CCCCC1 FYLJKQFMQFOLSZ-UHFFFAOYSA-N 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
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- 239000012188 paraffin wax Substances 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- IUGYQRQAERSCNH-UHFFFAOYSA-N pivalic acid Chemical compound CC(C)(C)C(O)=O IUGYQRQAERSCNH-UHFFFAOYSA-N 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229940113165 trimethylolpropane Drugs 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
- 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
- H01M4/58—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to energy storage research field, more particularly to a kind of anode material for lithium-ion batteries, including nuclear structure and shell structure, the shell structure is uniformly wrapped on the nuclear structure surface, the nuclear structure particle diameter is D1, and the shell structure thickness is h1, contains graphene in the shell structure, there is strong bond between 2≤100nm of the graphene sheet layer thickness h, the graphene sheet layer to make a concerted effort；So as to prepare the anode material for lithium-ion batteries of excellent electrochemical performance.
Description
Technical field
The invention belongs to energy storage material technical field, more particularly to a kind of anode material for lithium-ion batteries and its preparation side
Method.
Background technology
Lithium ion battery is with its fast charging and discharging, low temperature performance well, specific energy is big, self-discharge rate is small, small volume, lightweight
Etc. advantage, since its birth, revolutionary change just is brought to energy storage field, is widely used in various portable electronics
In equipment and electric automobile.However as the improvement of people's living standards, higher Consumer's Experience is proposed to lithium ion battery
Higher requirement：Longer stand-by time, more quick charge/discharge rates etc.；Had to look for solve the above problems new
The more excellent electrode material of performance.
Current commercialized anode material for lithium-ion batteries, be semiconductor or insulator substantially, and material granule is in itself
Electric conductivity is excessively poor, in order to solve the above problems, and prior art mainly has obtains two by pelletizing after material granule nanosizing
Conductive material with excellent conductive capability etc. is added in secondary grain structure, primary particle balling process, to improve positive pole material
Expect the electric conductivity of integral particle；Coating technology is used simultaneously, material surface is coated, so as to increase leading for material surface
Electrical property.
2004, extra large nurses (Andre K.Geim) of the strong K of peace moral of Univ Manchester UK etc. used mechanical stripping
Method prepares graphene (Graphene) first, has thus pulled open material preparation, the prelude of operational research.So-called graphite
Alkene, refers to a kind of plates arranged in hexagonal annular between carbon atom, is generally made up of single or multiple lift graphite flake layer, can be
Two-dimensional space infinitely extends, it may be said that be proper two-dimensional structure material.It has that specific surface area is big, electrical and thermal conductivity
Can the low outstanding advantages of excellent, thermal coefficient of expansion：Specifically, high specific surface area (calculated value：2630m2/g)；Height is led
Electrically, carrier transport rate (200000cm2/V·s)；High heat conductance (5000W/mK)；High intensity, high Young's modulus
(1100GPa), fracture strength (125GPa).Therefore it has pole in energy storage field, heat transfer field and Materials with High Strength field
Big utilization prospect.Specifically, because graphene has excellent electric conductivity, the quality of itself is extremely light, and with flexibility
Two-dimension plane structure, be ideal Surface coating material.But the unique two-dimension plane structure of grapheme material, to from
Son has obvious inhibition in transmitting procedure inside and outside lithium ion cell positive particle, so as to have influence on lithium ion battery just
The performance of pole material kinetics performance.Meanwhile, the intermolecular forces of graphene sheet layer are weaker, with the addition of the second particle of graphene just
Pole material structure is comparatively loose, and electrode cold pressing is to be easily broken in cell manufacturing process, so as to influence its chemical property
Performance.
In view of this, it is necessory to propose a kind of anode material for lithium-ion batteries and preparation method thereof, it can both give play to
The sharpest edges of graphene, are avoided that its negative effect to being brought after anode material for lithium-ion batteries Surface coating again.
The content of the invention
It is an object of the invention to：In view of the shortcomings of the prior art, a kind of anode material for lithium-ion batteries provided, bag
Nuclear structure and shell structure are included, the shell structure is uniformly wrapped on the nuclear structure surface, and the nuclear structure particle diameter is D1, institute
Shell structure thickness is stated for h1, contains graphene, 2≤100nm of the graphene sheet layer thickness h, the graphite in the shell structure
There is strong bond between alkene lamella to make a concerted effort；So as to prepare the anode material for lithium-ion batteries of excellent electrochemical performance.The present invention
With universality, it is adaptable to energy storage research field, institute's surface coated electrode material of progress in need, lithium ion is specifically included
Positive electrode, ion cathode material lithium (such as graphite, silicon-carbon, lithium titanate, alloy anode) and other battery capacitor equipment
Expect (such as lithium-air battery, fuel cell, sodium-ion battery, Zinc ion battery).
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of anode material for lithium-ion batteries, including nuclear structure and shell structure, the shell structure are uniformly wrapped on the core
Body structure surface, the nuclear structure particle diameter is D1, and 0.5 μm≤D1≤100 μm, the shell structure thickness is h1,10nm≤h1
≤ 5 μm, shell is too small, it is impossible to play covered effect, and shell is excessive, will hinder ion diffusion；Contain graphite in the shell structure
There is strong bond between alkene, 2≤100nm of the graphene sheet layer thickness h, the graphene sheet layer to make a concerted effort；Between graphene sheet layer
The graphene sheet layer being distributed in shell structure, can closely be combined together, so that it is steady to obtain structure by powerful bonding force
The fixed shell structure containing graphene sheet layer, is closely coated on the surface of anode material for lithium-ion batteries nuclear structure, reduction is just
The resistance of pole material, improves the chemical property of positive electrode.
Improved as one kind of anode material for lithium-ion batteries of the present invention, the nuclear structure is primary particle structure or secondary
Grain structure or multiple particle structure；In the nuclear structure comprising cobalt acid lithium, LiMn2O4, LiFePO4, nickel cobalt manganese, nickel cobalt aluminium,
At least one of lithium nickelate, lithium-barium oxide, lithium-rich anode material.
The key classification made a concerted effort as a kind of improvement of anode material for lithium-ion batteries of the present invention there is provided the strong bond is hydrogen bond
Or/and chemical bond；The graphene be small pieces layer graphene or/and porous graphene, now formed shell structure layer, to lithium from
Inhibition is lower when son is transmitted inside and outside positive electrode particle, and material has more preferable chemical property；The small lamella stone
Black alkene slice plane diameter d1, d1≤π * D1；Continuum width is d2, d2≤π * D1 between the porous graphene holes；
Make a concerted effort in addition, there can also be strong bond between the graphene and the nuclear structure, now, the material in the nuclear structure passes through
It is modified, it is such as the positive electrode nuclear structure particle after surface treatment.
Improved as one kind of anode material for lithium-ion batteries of the present invention, in the clad, also include traditional cladding
The polymer carbonization component that layer or/and monomer in situ polymerization are obtained.
Improved as one kind of anode material for lithium-ion batteries of the present invention, traditional clad is traditional clad raw material
Charing is obtained；Traditional clad raw material be phenolic resin, melamine resin, Vinylidene Chloride, pitch, polyethylene, stearic acid,
It is PVC, polyacrylonitrile, natural rubber, butadiene-styrene rubber, butadiene rubber, EP rubbers, polyethylene, polypropylene, polyamide, poly- to benzene
In naphthalate, nano cupric oxide, nano magnesia, nano-titanium oxide, nano aluminium oxide, nano-graphite, graphite flake
At least one；The monomer includes esters of acrylic acid, methyl acrylic ester, styrene, acrylonitrile, methacrylonitrile, poly-
Ethylene glycol dimethacrylate, polyethyleneglycol diacrylate, divinylbenzene, trimethylol propane trimethyl acrylic acid
Ester, methyl methacrylate, N, N- DMAAs, N- acryloyl morpholines, methyl acrylate, ethyl acrylate, propylene
Acid butyl ester, positive Hexyl 2-propenoate, 2- cyclohexyl acrylates, dodecyl acrylate, GDMA, polyethylene glycol
Dimethylacrylate, polyethylene glycol dimethacrylate, neopentylglycol diacrylate, 1,6-HD diacrylate
Ester, tetraethylene glycol diacrylate, tri (propylene glycol) diacrylate, ethoxyquin tetramethylol methane tetraacrylate, the third oxidation season
Penta tetrol acrylate, double-Glycerin tetraacrylate, pentaerythritol triacrylate, trimethylol propane trimethyl
Acrylate, glycerol propoxylate triacrylate, three (2- ethoxys) isocyanuric acid triacrylate trimethylolpropane tris third
Olefin(e) acid ester, propoxylation trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, ethoxylation
In trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, tetramethylol methane tetraacrylate
It is at least one.
Present invention additionally comprises a kind of preparation method of anode material for lithium-ion batteries, mainly comprise the following steps：
Step 1, selection nuclear structural materials are standby；
Step 2, the clad slurry containing modified graphene lamella is prepared；
Step 3, nuclear structural materials described in step 1 are placed in the slurry that step 2 is obtained and coated, reduced afterwards
Processing, is finally carbonized and obtains finished product anode material for lithium-ion batteries.
Or
Step 3 ', the nuclear structural materials that step 1 is obtained are placed in the clad slurry that step 2 is obtained, and carry out solvent heat
Reaction so that modified graphene is uniformly coated on nuclear structural materials surface；Filter afterwards, drying obtains lithium ion cell positive
Material.
Improved as one kind of method for preparing anode material of lithium-ion battery of the present invention, the modified graphene is graphene
The graphene of functional group is grafted with lamella；The functional group is included in carboxyl, hydroxyl, epoxy radicals, carbonyl, nitro, amino
It is at least one；The mass ratio that functional group's quality accounts for graphite olefinic constituent is 0.5%~40%.
Improve, polymerize when containing in the clad as one kind of method for preparing anode material of lithium-ion battery of the present invention
During thing monomer, after the step 3 cladding process, inducer need to be added and promote monomer in situ polymerization formation polymer, now,
Step 3 is：Nuclear structural materials described in step 1 are placed in the slurry that step 2 is obtained and coated, are subsequently placed in induction
Monomer in situ polymerization is induced in the environment that thing is present, then carries out reduction treatment, is finally carbonized and obtains finished product lithium-ion electric
Pond positive electrode.The inducer is initiator, and the initiator includes isopropyl benzene hydroperoxide, t-butyl hydrogen peroxide, mistake
Aoxidize the special butyl ester of diisopropylbenzene (DIPB), di-tert-butyl peroxide, dibenzoyl peroxide, dilauroyl peroxide, perbenzoic acid, mistake
Aoxidize at least one of the special butyl ester of pivalic acid, di-isopropyl peroxydicarbonate, di-cyclohexylperoxy di-carbonate.
Improved as one kind of method for preparing anode material of lithium-ion battery of the present invention, the preparation described in step 2 contains stone
During the clad slurry of black alkene lamella, surfactant can also be added, the surfactant includes the surface
Activating agent is that surfactant includes at least one of wetting agent, dispersant, bleeding agent, solubilizer, cosolvent, cosolvent；
The wetting agent is anionic or/and non-ionic wetting agent；The dispersant is fatty acid/aliphatic amide type/ester
An at least class in class dispersant, paraffin class, metal soap, low molecule wax class, HPMA；The bleeding agent for it is non-ionic or/
With anionic bleeding agent；The anionic wetting agents include alkyl sulfate, sulfonate, aliphatic acid or fatty acid ester sulfuric acid
At least one of salt, carboxylic acid soaps and phosphate；The non-ionic wetting agent includes polyoxyethylated alkyl phenol, polyoxy second
At least one of alkene fatty alcohol ether and polyoxyethylene polyoxypropylene block copolymer；The dispersant is vinyl stearic bicine diester
Amine, oleic acid acyl, glyceryl monostearate, glyceryl tristearate, atoleine, microcrystalline wax, barium stearate, zinc stearate,
At least one of calcium stearate, Tissuemat E and polyethylene glycol；The nonionic penetrant includes JFC, JFC-1, JFC-2
At least one of with JFC-E；The anionic bleeding agent comprising fast penetrant T, alkali-resistant penetrant OEP-70, alkaline-resisting ooze
Saturating at least one of agent AEP and seeping at high temperature agent JFC-M；The cosolvent includes benzoic acid, sodium benzoate, salicylic acid, water
At least one of poplar acid sodium, p-aminobenzoic acid, urethane, urea, acid amides, acetamide, borax and KI；It is described latent molten
Agent includes at least one of ethanol, glycerine, propane diols and polyethylene glycol.
The advantage of the invention is that：
1. flexible, the graphene coated structure of planar structure, it can be coated with significantly more efficient, reduce positive electrode
Resistance, improves the chemical property of material；
2. powerful bonding force between graphene sheet layer, can closely tie the graphene sheet layer being distributed in shell structure
It is combined, so that the constitutionally stable shell structure containing graphene sheet layer is obtained, efficiently against lithium ion cell positive material
The destruction that material is during battery core is prepared and battery core is during subsequent use so that clad is persistently effectively played
Protective effect, it is final to improve the cycle performance of positive electrode；
3. containing small molecule monomer in-situ polymerization component in clad, it can effectively improve each group inside clad and divide it
Between connection effect, and the electronic conductance effect between clad and nuclear structure, because small molecule monomer is easier and other
Component infiltration, uniform mixing.
4. small lamella or porous graphene are as clad, the inhibition that shell structure layer is passed through to ion is lower, system
Standby lithium ion cell positive finished-product material out has more excellent dynamic performance.
Embodiment
The present invention and its advantage are described in detail with reference to embodiment, but the embodiment party of the present invention
Formula not limited to this.
Comparative example, prepares the lithium iron phosphate positive material that particle diameter is 12 μm；
It is prepared by step 1. nuclear structure：100nm lithium iron phosphate particles are selected, uniformly mix laggard with super conductive carbon component
Row pelletizing, obtains the second particle nuclear structure that particle diameter is about 12 μm stand-by；
Step 2., as covering material, is coated to the nuclear structure that step 1 is prepared, is carbonized afterwards from pitch,
Obtain the anode material for lithium-ion batteries that particle diameter is 12 μm.
Embodiment 1, is that the present embodiment comprises the following steps with comparative example difference：
It is prepared by step 1. nuclear structure：100nm lithium iron phosphate particles are selected, uniformly mix laggard with super conductive carbon component
Row pelletizing, obtains the second particle nuclear structure that particle diameter is about 12 μm stand-by；
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl) content is the 0.5% of graphene gross weight, graphene sheet layer size is 5 μm) to be uniformly dispersed in NMP molten
In agent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
Step 3, nuclear structural materials described in step 1 are placed in the clad raw material that step 2 is obtained and coated, soaked afterwards
Bubble is reduced in the solution containing hydrazine hydrate so that the functional group between modified graphene lamella, which reacts, to be crosslinked
Form graphene network；Finally it is carbonized and obtains finished product lithium ion cell positive.
Embodiment 2, difference from Example 1 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content is the 2% of graphene gross weight, graphene sheet layer size is 5 μm) to be uniformly dispersed in NMP molten
In agent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 1, it is not repeated herein.
Embodiment 3, difference from Example 1 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content is the 5% of graphene gross weight, graphene sheet layer size is 5 μm) to be uniformly dispersed in NMP molten
In agent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 1, it is not repeated herein.
Embodiment 4, difference from Example 1 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content is the 15% of graphene gross weight, graphene sheet layer size is 5 μm) to be uniformly dispersed in NMP molten
In agent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 1, it is not repeated herein.
Embodiment 5, difference from Example 1 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content is the 20% of graphene gross weight, graphene sheet layer size is 5 μm) to be uniformly dispersed in NMP molten
In agent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 1, it is not repeated herein.
Embodiment 6, difference from Example 1 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content is the 25% of graphene gross weight, graphene sheet layer size is 5 μm) to be uniformly dispersed in NMP molten
In agent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 1, it is not repeated herein.
Embodiment 7, difference from Example 1 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content is the 40% of graphene gross weight, graphene sheet layer size is 5 μm) to be uniformly dispersed in NMP molten
In agent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 1, it is not repeated herein.
Embodiment 8, difference from Example 1 is, the present embodiment comprises the following steps：
It is prepared by step 1. nuclear structure：100nm lithium iron phosphate particles are selected, are made after uniformly being mixed with CNT
Ball, obtains the second particle nuclear structure that particle diameter is about 12 μm stand-by；
Step 2, clad slurry is prepared：By modified graphene (oxygen-containing functional group (predominantly carbonyl, hydroxyl, carboxyl etc.)
Content be graphene gross weight 15%, graphene sheet layer size be 5 μm) be uniformly dispersed in water formed solution coated
Layer slurry；
Step 3, nuclear structural materials described in step 1 are placed in the clad raw material that step 2 is obtained, carried out after being well mixed
Hydro-thermal reaction, now modified graphene lamella will be in nuclear structure surface formation clad；After the completion of question response, solid group is taken out
Point, drying；Thermal reduction processing is carried out again, is improved the electric conductivity of clad, is finally obtained finished product lithium ion cell positive.
It is other identical with embodiment 1, it is not repeated herein.
Embodiment 9, difference from Example 1 is, the present embodiment comprises the following steps：
Step 1, prepared by nuclear structure：100nm lithium iron phosphate particles are selected, pelletizing is carried out after uniformly being mixed with Ketjen black,
Obtain the second particle nuclear structure that particle diameter is about 12 μm stand-by；
Step 2, clad slurry is prepared：By trimethylol-propane trimethacrylate and modified graphene (oxygen-containing official
It is the 15% of graphene gross weight that (predominantly carbonyl, hydroxyl, carboxyl etc.) content, which can be rolled into a ball, and graphene sheet layer size is 5 μm) carry out
Mediate, be well mixed；It is well mixed afterwards with phenolic resin and obtains clad slurry；
Step 3, nuclear structural materials described in step 1 are placed in the clad slurry that step 2 is obtained and coated, it is rearmounted
In BPO solution, promote monomer to carry out in-situ polymerization generation polymer, the polymer of generation by inside clad, clad
It is closely joined together between nuclear structure；It is placed in again in the solution containing hydrazine hydrate, promotes modified graphene to occur reduction anti-
It should carry out being cross-linked to form graphene network；Finally it is carbonized and obtains finished product lithium ion cell positive.
It is other identical with comparative example 1, it is not repeated herein.
Embodiment 10, prepares the anode material for lithium-ion batteries that particle diameter is 100 μm；
Step 1：Prepared by nuclear structure, selection particle diameter is 200nm LiFePO4, cobalt acid lithium hybrid particles are as once
Grain, wherein LiFePO4 content are 90%；CNT, super conductive carbon mix are conductive agent component；By dodecyl sulphur
Sour sodium, primary particle mixing, add a small amount of N, N- dimethyl pyrrolidone solution is mediated, and obtains primary particle uniform afterwards
Scattered slurry；Conductive agent, PVP are mixed, a small amount of N is added afterwards, N- dimethyl pyrrolidone solution is mediated, and obtains stone
The dispersed slurry of black alkene；Two kinds of slurries are uniformly mixed, pelletizing obtains nuclear structure afterwards；
Step 2, clad slurry is prepared：By lamellar spacing for 100nm modified graphene (oxygen-containing functional group (predominantly
Carbonyl, hydroxyl, carboxyl etc.) content is the 15% of graphene gross weight, graphene sheet layer size is 5 μm), PVP, NMP be mixed into
Row is mediated, after being well mixed；It is well mixed afterwards with phenolic resin and obtains clad slurry；
It is other identical with embodiment 9, it is not repeated herein.
Embodiment 11, difference from Example 4 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content is the 15% of graphene gross weight, graphene sheet layer size is 1 μm) to be uniformly dispersed in NMP molten
In agent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 4, it is not repeated herein.
Embodiment 12, difference from Example 4 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content be graphene gross weight 15%, graphene sheet layer size be 37.68 μm) be uniformly dispersed in
In nmp solvent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 4, it is not repeated herein.
Embodiment 13, difference from Example 4 is, the present embodiment comprises the following steps：
Step 2, clad slurry is prepared：Pitch is heats liquefied；By modified graphene, (oxygen-containing functional group (is mainly carbonyl
Base, hydroxyl, carboxyl etc.) content be graphene gross weight 15%, graphene is continuum field width between porous graphene, holes
Spend for 5 μm) it is uniformly dispersed in nmp solvent, add afterwards in pitch；It is uniformly mixing to obtain clad raw material；
It is other identical with embodiment 4, it is not repeated herein.
Embodiment 14, difference from Example 4 is, the present embodiment comprises the following steps：
It is prepared by step 1. nuclear structure：100nm nickel cobalt manganese (NCM) particle is selected, is uniformly mixed with super conductive carbon component
After carry out pelletizing, obtain the second particle nuclear structure that particle diameter is about 12 μm stand-by；
It is other identical with embodiment 4, it is not repeated herein.
Battery is assembled：The positive electrode and conductive agent, bonding agent, stirring solvent that comparative example, each embodiment are prepared
Electrode slurry is obtained, applies form anode electrode on a current collector afterwards；By anode electrode, (graphite is active matter with negative electrode
Matter), barrier film assembling obtain naked battery core, bag entered afterwards carry out top side seal, drying, fluid injection, standing, chemical conversion, shaping, degasification to obtain
Resultant battery.
Material properties test：
Gram volume is tested：Each embodiment and comparative example silicon carbon material are prepared by following flow in 25 DEG C of environment
Battery core carries out gram volume test：Stand 3min；0.2C constant-current charges are to 4.2V, 4.2V constant-voltage charges to 0.05C；Stand 3min；
0.2C constant-current discharges obtain discharge capacity D1 to 3.0V；Stand 3min；0.2C constant-current discharges are to 3.85V；It is complete after standing 3min
Into volume test, the weight of silicon carbon material, that is, obtain negative pole gram volume, acquired results are shown in Table 1 in D1 divided by negative electricity pole piece.
Inner walkway：LiFePO 4 material in each embodiment and comparative example is prepared into by following flow in 25 DEG C of environment
The battery core arrived carries out inner walkway：Stand 3min；1C constant-current charges are to 3.85V, 3.85V constant-voltage charges to 0.1C；Stand 3min；
Electrochemical workstation is used again, the DCR values of battery core are tested, and acquired results are shown in Table 1.
High rate performance is tested：Each embodiment and comparative example silicon carbon material are prepared by following flow in 25 DEG C of environment
Battery core carry out high rate performance test：Stand 3min；0.2C constant-current charges are to 4.2V, 4.2V constant-voltage charges to 0.05C；Stand
3min；0.2C constant-current discharges obtain discharge capacity D1 to 3.0V；Stand 3min；0.2C constant-current charges to 4.2V, 4.2V constant pressures is filled
Electricity is to 0.05C；Stand 3min；2C constant-current discharges obtain discharge capacity D21 to 3.0V；Stand 3min；High rate performance is completed afterwards
Test, battery high rate performance=D2/D1*100%, acquired results are shown in Table 1.
Loop test:The electricity prepared in 25 DEG C of environment by following flow to each embodiment and comparative example silicon carbon material
Core carries out loop test：Stand 3min；0.2C constant-current charges are to 4.2V, 4.2V constant-voltage charges to 0.05C；Stand 3min；0.2C
Constant-current discharge obtains discharge capacity D1 to 3.0V；3min is stood, " 0.2C constant-current charges to 4.2V, 4.2V constant-voltage charges are extremely
0.05C；Stand 3min；0.2C constant-current discharges obtain discharge capacity Di to 3.0V；3min " is stood to repeat to obtain D300 299 times,
Loop test is completed afterwards, and calculating capability retention is D300/D1*100%, and acquired results are shown in Table 1.
The battery core chemical property table that table 1, different anode material for lithium-ion batteries are prepared
It can be obtained by table 1, anode material for lithium-ion batteries prepared by the present invention, with more outstanding chemical property：I.e.
Higher gram volume, more preferable circulation volume conservation rate and higher high rate performance.Specifically, comparative examples and embodiment
1- embodiments 7 can be obtained, with the increase of oxygen-containing functional group content in modified graphene in clad, gram of lithium ion cell positive
Capacity first increases to be reduced afterwards, and cycle performance is first lifted and keeps constant afterwards, DCR gradually increases after first remaining unchanged, and high rate performance is first
Gradually reduced after remaining unchanged；Because, functional group content is too low, it is impossible to forms enough crosslinking points, is tied enough
Real clad；Functional group content is more, and the graphene network crosslinking points in shell structure are more, and network structure is more stable；But
After crosslinking points are excessive, the network structure of formation will be finer and close, and the influence that it is transmitted to ion is bigger, and cell dynamics performance is got over
Difference.Comparative example 4, embodiment 11- embodiments 13 can be obtained, the stone of different lamella sizes (or continuum width between holes)
Black alkene is as coating layer material, and obtained LiFePO4 performance gap is larger.It can be obtained by each embodiment, the present invention has pervasive
Property, it is adaptable to energy storage research field, institute's surface coated electrode material of progress in need, specifically include lithium ion anode material
Material, ion cathode material lithium (such as graphite, silicon-carbon, lithium titanate, alloy anode) and other battery capacitor material (such as lithiums
Air cell, fuel cell, sodium-ion battery, Zinc ion battery etc.).
The announcement and teaching of book according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and changed.Therefore, the invention is not limited in above-mentioned embodiment, every those skilled in the art exist
Made any conspicuously improved, replacement or modification belong to protection scope of the present invention on the basis of the present invention.This
Outside, although having used some specific terms in this specification, these terms merely for convenience of description, not to the present invention
Constitute any limitation.
Claims (10)
1. a kind of anode material for lithium-ion batteries, including nuclear structure and shell structure, the shell structure are uniformly wrapped on the core knot
The surface of structure, it is characterised in that the particle diameter of the nuclear structure is D1, and the thickness of the shell structure is h1,
Contain graphene in the shell structure, lamellar spacing h2≤100nm of the graphene,
There is strong bond between the lamella of the graphene to make a concerted effort.
2. the anode material for lithium-ion batteries described in a kind of claim 1, it is characterised in that the nuclear structure is primary particle knot
In structure or second particle structure, the nuclear structure comprising cobalt acid lithium, LiMn2O4, LiFePO4, nickel cobalt manganese, nickel cobalt aluminium, lithium nickelate,
At least one of lithium-barium oxide, lithium-rich anode material.
3. the anode material for lithium-ion batteries described in a kind of claim 1, it is characterised in that the key class that the strong bond is made a concerted effort is provided
Wei not hydrogen bond or/and chemical bond.
4. the anode material for lithium-ion batteries described in a kind of claim 1, it is characterised in that also include in the shell structure
The polymer carbonization component that coating or/and monomer in situ polymerization are obtained.
5. the anode material for lithium-ion batteries described in a kind of claim 4, it is characterised in that the clad is traditional clad
Raw material charing is obtained；Traditional clad raw material is phenolic resin, melamine resin, Vinylidene Chloride, pitch, polyethylene, tristearin
Acid, PVC, polyacrylonitrile, natural rubber, butadiene-styrene rubber, butadiene rubber, EP rubbers, polyethylene, polypropylene, polyamide, poly- pair
PET, nano cupric oxide, nano magnesia, nano-titanium oxide, nano aluminium oxide, nano-graphite, graphite flake
At least one of；The polymer monomer includes esters of acrylic acid, methyl acrylic ester, styrene, acrylonitrile, methyl-prop
Alkene nitrile, polyethylene glycol dimethacrylate, polyethyleneglycol diacrylate, divinylbenzene, trimethylol propane trimethyl
Acrylate, methyl methacrylate, N, N- DMAAs, N- acryloyl morpholines, methyl acrylate, acrylic acid second
Ester, butyl acrylate, positive Hexyl 2-propenoate, 2- cyclohexyl acrylates, dodecyl acrylate, GDMA,
Polyethylene glycol dimethacrylate, polyethylene glycol dimethacrylate, neopentylglycol diacrylate, 1,6-HD two
Acrylate, tetraethylene glycol diacrylate, tri (propylene glycol) diacrylate, ethoxyquin tetramethylol methane tetraacrylate, third
Aoxidize pentaerythritol acrylate, double-Glycerin tetraacrylate, pentaerythritol triacrylate, trimethylolpropane
Trimethyl acrylic ester, glycerol propoxylate triacrylate, three (2- ethoxys) isocyanuric acid triacrylate trihydroxy methyls third
Alkane triacrylate, propoxylation trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, second
Epoxide trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, pentaerythrite tetrapropylene acid
At least one of ester.
6. the preparation method of the anode material for lithium-ion batteries described in a kind of claim 1, it is characterised in that mainly include as follows
Step：
Step 1, selection nuclear structural materials are standby；
Step 2, the clad slurry containing modified graphene lamella is prepared；
Step 3, nuclear structural materials described in step 1 are placed in the slurry that step 2 is obtained and coated, also original place is carried out afterwards
Reason, is finally carbonized and obtains finished product anode material for lithium-ion batteries；
Or
Step 3 ', the nuclear structural materials that step 1 is obtained are placed in the clad slurry that step 2 is obtained, solvent thermal reaction is carried out,
So that modified graphene is uniformly coated on nuclear structural materials surface；Filter afterwards, drying obtains anode material for lithium-ion batteries.
7. a kind of preparation method of the anode material for lithium-ion batteries described in claim 6, it is characterised in that the modified graphite
Alkene is the graphene that functional group is grafted with graphene sheet layer；The functional group includes carboxyl, hydroxyl, epoxy radicals, carbonyl, nitre
At least one of base, amino；The mass ratio that the quality of the functional group accounts for graphite olefinic constituent is 0.5%~40%.
8. a kind of preparation method of the anode material for lithium-ion batteries described in claim 6, it is characterised in that step 2 clad
Traditional clad raw material or/and polymer monomer can also be included in slurry.
9. the preparation method of the anode material for lithium-ion batteries described in a kind of claim 8, it is characterised in that when the clad
In when containing polymer monomer, after the step 3 cladding process, need to adding inducer, to promote monomer in situ polymerization to be formed poly-
Compound.
10. the preparation method of the anode material for lithium-ion batteries described in a kind of claim 6, it is characterised in that described in step 2
Surfactant, the surfactant bag have been additionally added during preparing the clad slurry containing modified graphene lamella
Include at least one of wetting agent, dispersant, bleeding agent, solubilizer, cosolvent, cosolvent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111106317A (en) * | 2018-10-26 | 2020-05-05 | 东丽先端材料研究开发（中国）有限公司 | Graphite oxide coated lithium ion battery anode material |
| CN119230803A (en) * | 2024-11-28 | 2024-12-31 | 湖南裕能新能源电池材料股份有限公司 | A composite positive electrode material and preparation method thereof |
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