CN105977463A - Method for preparing SiOx composite anode material - Google Patents

Method for preparing SiOx composite anode material Download PDF

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Publication number
CN105977463A
CN105977463A CN201610470670.9A CN201610470670A CN105977463A CN 105977463 A CN105977463 A CN 105977463A CN 201610470670 A CN201610470670 A CN 201610470670A CN 105977463 A CN105977463 A CN 105977463A
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China
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siox
slurry
temperature
anode material
spray drying
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CN201610470670.9A
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唐仁衡
肖方明
王英
孙泰
黄玲
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Guangdong Institute of Rare Metals
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Guangdong Institute of Rare Metals
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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

Abstract

The invention relates to a method for preparing a SiOx composite anode material. The method is characterized by comprising the following steps of: thermally processing SiOx powder with the average grain diameter of 1-20 mu m under argon protection at 900-1200 DEG C for 1-10 h, and naturally cooling to room temperature; adding deionized water or absolute ethyl alcohol, the mass of which is 3-10 times of that of the SiOx powder, into the SiOx powder, and grinding for 0.5-10 h so as to obtain uniformly dispersed slurry; and, uniformly mixing the slurry with a conductive agent and a binding agent, performing spray drying, wherein the inlet temperature for spray drying is at 200-350 DEG C; the outlet temperature for spray drying is at 80-140 DEG C; and thus, the SiOx composite anode material is obtained. The SiOx composite anode material prepared by the invention has the advantages of being relatively high in first-time charging and discharging efficiency, better in cycle performance and the like, and is applied to application of an anode material of a lithium ion battery; and the method disclosed by the invention is simple in process, relatively low in cost and convenient for industrial production.

Description

A kind of preparation method of SiOx composite negative pole material
Technical field
The present invention relates to lithium ion battery negative material field, especially relate to the preparation of a kind of SiOx composite negative pole material Method.
Background technology
In recent years, to have that specific capacity is higher, voltage platform is relatively low, the cost of raw material is cheap etc. excellent for the sub-silicium cathode material of oxidation Point, has applications well prospect in field of lithium ion battery.But SiOx negative material occurs with lithium metal in process of intercalation first Reaction, some inert fractions such as oxidate for lithium or lithium silicates of in-situ preparation, it is no longer participate in electrode reaction, additionally, aoxidize silica-based The electronic conductance ability of material, also have impact on the performance of its chemical property, thus causes the most irreversible appearance of SiOx material Measure bigger problem.At present in addition to using composite means and reducing the change in volume of SiOx, also by constructing some special knots The method of structure, reserves certain volumetric expansion space at material internal, improves structural stability and the chemical property of material.This Outward, effectively control the interfacial reaction between material and electrolyte by changing the surface texture of material and state, reduce because of with electricity Solve irreversible specific capacity and electrode failure that liquid generation side reaction is caused, improve initial coulomb efficiency and the cyclicity of material Energy.
Summary of the invention
The present invention is directed to the problem that existing SiOx material first charge-discharge efficiency is relatively low, cycle performance is poor, it is provided that a kind of There is the higher preparation method with cycle performance preferable SiOx composite negative pole material of first charge-discharge efficiency.
The concrete technical scheme of the present invention: by SiOx powder that mean diameter is 1 ~ 20 μm under argon shield, temperature 900 ~ 1200 DEG C, heat treatment time 1 ~ 10 hour, naturally cool to room temperature；Above-mentioned SiOx powder adds its quality 3 ~ 10 times go from Sub-water or dehydrated alcohol, grind 0.5 ~ 10 hour, obtain homodisperse slurry；Slurry is mixed all with conductive agent and binding agent Even, it is spray-dried, the inlet temperature of spray drying is 200 ~ 350 DEG C, and outlet temperature is 80 ~ 140 DEG C, obtains described SiOx and is combined Negative material.
Conductive agent is CNT or Graphene, and addition is the 0.5 ~ 10% of SiOx mass.
Binding agent is sodium carboxymethyl cellulose, butadiene-styrene rubber, polyvinyl alcohol, acrylate polymer emulsion, styrene-propene One in acid polymer emulsion, amino resins, VAE emulsion, Kynoar or epoxy resin or More than one, addition is the 1 ~ 10% of SiOx mass.
Heat treatment can be effectively improved first effect and the discharge capacity of material；Add CNT or Graphene is made conductive agent and can be shown Write the electric conductivity improving material.
SiOx composite wood negative pole material prepared by the present invention has that first charge-discharge efficiency is higher and cycle performance is preferably etc. excellent Point, is suitable for lithium ion battery negative pole materials'use.The preparation method technique of the present invention is simple, cost is relatively low, it is simple to industry Metaplasia is produced.
Accompanying drawing explanation
Fig. 1 is the SiOx composite negative pole material SEM figure of embodiment 1 preparation.
Detailed description of the invention
Embodiment 1
By SiOx powder that mean diameter is 10 μm under the conditions of argon shield, temperature is 900 DEG C, heat treatment time is 5 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 5 times, grind 5 hours in sand mill, obtain Homodisperse slurry；After the slurry obtained is mixed homogeneously with carbon nano tube paste, sodium carboxymethyl cellulose and butadiene-styrene rubber, Being spray-dried, the inlet temperature of spray drying is 250 DEG C, and outlet temperature is 120 DEG C, obtains spheroidal particle SiOx composite negative pole material Material.
The addition of CNT, sodium carboxymethyl cellulose and butadiene-styrene rubber is respectively 5%, 0.3% and of SiOx opaque amount 2%, the solid content 5% of carbon nano tube paste.
Embodiment 2
By SiOx powder that mean diameter is 8 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 3 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 10 times, grind 8 hours in sand mill, To homodisperse slurry；After the slurry obtained is mixed homogeneously with Graphene slurry and acrylate polymer emulsion, spray dried Dry, the inlet temperature of spray drying is 300 DEG C, and outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material.
The addition of Graphene and acrylate polymer emulsion is respectively the 2% and 5% of SiOx opaque amount, Graphene slurry Solid content 6%.
Embodiment 3
By SiOx powder that mean diameter is 3 μm under the conditions of argon shield, temperature is 1050 DEG C, heat treatment time is 3 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 10 times, grind 8 hours in sand mill, To homodisperse slurry；By the slurry that obtains and carbon nano tube paste and polyvinyl alcohol uniformly after, be spray-dried, spraying The inlet temperature being dried is 300 DEG C, and outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material.
The addition of CNT and polyvinyl alcohol is respectively the 5% and 4% of SiOx opaque amount, and consolidating of carbon nano tube paste contains Amount 6%.
Embodiment 4
By SiOx powder that mean diameter is 1 μm under the conditions of argon shield, temperature is 1100 DEG C, heat treatment time is 2 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 5 times, grind 3 hours in sand mill, obtain Homodisperse slurry；After the slurry obtained is mixed homogeneously with Graphene slurry and amino resins, it is spray-dried, is spray-dried Inlet temperature be 300 DEG C, outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material.
The addition of Graphene and amino resins is respectively the 2% and 5% of SiOx opaque amount, the solid content of Graphene slurry 6%。
Embodiment 5
By SiOx powder that mean diameter is 5 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 3 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 8 times, grind 5 hours in sand mill, obtain Homodisperse slurry；The slurry obtained is mixed all with the N-Methyl pyrrolidone solution of Graphene slurry and Kynoar After even, being spray-dried, the inlet temperature of spray drying is 200 DEG C, and outlet temperature is 100 DEG C, obtains spheroidal particle SiOx and is combined Negative material.
The addition of Graphene and Kynoar is respectively the 3% and 2% of SiOx opaque amount, the solid content of Graphene slurry 6%。
Embodiment 6
By SiOx powder that mean diameter is 20 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 6 hours, Cool to room temperature with the furnace；In the SiOx powder processed, add the deionized water of its quality 10 times, grind 10 hours in sand mill, Obtain homodisperse slurry；After the slurry obtained is mixed homogeneously with carbon nano tube paste and epoxy resin, it is spray-dried, spray The inlet temperature that mist is dried is 200 DEG C, and outlet temperature is 100 DEG C, obtains spheroidal particle SiOx composite negative pole material.
The addition of CNT and epoxy resin is respectively the 5% and 3% of SiOx opaque amount, and consolidating of carbon nano tube paste contains Amount 6%.
Embodiment 7
By SiOx powder that mean diameter is 5 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 3 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 6 times, grind 3 hours in sand mill, obtain Homodisperse slurry；After the slurry obtained is mixed homogeneously with Graphene slurry and styrene acrylic polymer emulsion, spray Mist is dried, and the inlet temperature of spray drying is 300 DEG C, and outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material Material.
The addition of Graphene and styrene acrylic polymer emulsion is respectively the 2% and 5% of SiOx opaque amount, graphite The solid content 6% of alkene slurry.
Embodiment 8
By SiOx powder that mean diameter is 10 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 3 hours, Cool to room temperature with the furnace；In the SiOx powder processed, add the deionized water of its quality 10 times, grind 5 hours in sand mill, Obtain homodisperse slurry；The slurry obtained is mixed all with Graphene slurry and VAE emulsion After even, being spray-dried, the inlet temperature of spray drying is 300 DEG C, and outlet temperature is 130 DEG C, obtains spheroidal particle SiOx and is combined Negative material.
The addition of Graphene and VAE emulsion is respectively the 2% and 4% of SiOx opaque amount, stone The solid content 6% of ink alkene slurry.
Embodiment 9
By SiOx powder that mean diameter is 5 μm under the conditions of argon shield, temperature is 950 DEG C, heat treatment time is 8 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 8 times, grind 5 hours in sand mill, obtain Homodisperse slurry；After the slurry obtained is mixed homogeneously with carbon nano tube paste, sodium carboxymethyl cellulose and butadiene-styrene rubber, Being spray-dried, the inlet temperature of spray drying is 250 DEG C, and outlet temperature is 120 DEG C, obtains spheroidal particle SiOx composite negative pole material Material.
The addition of CNT, sodium carboxymethyl cellulose and butadiene-styrene rubber is respectively 2%, 0.3% and of SiOx opaque amount 4%, the solid content 5% of carbon nano tube paste.
Embodiment 10
By SiOx powder that mean diameter is 15 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 6 hours, Cool to room temperature with the furnace；In the SiOx powder processed, add the deionized water of its quality 8 times, grind 8 hours in sand mill, To homodisperse slurry；After the slurry obtained is mixed homogeneously with Graphene slurry and acrylate polymer emulsion, spray dried Dry, the inlet temperature of spray drying is 300 DEG C, and outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material.
The addition of Graphene and acrylate polymer emulsion is respectively the 3% and 3% of SiOx opaque amount, Graphene slurry Solid content 6%.
Embodiment 11
By SiOx powder that mean diameter is 5 μm under the conditions of argon shield, temperature is 1050 DEG C, heat treatment time is 3 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 10 times, grind 4 hours in sand mill, To homodisperse slurry；By the slurry that obtains and carbon nano tube paste and polyvinyl alcohol uniformly after, be spray-dried, spraying The inlet temperature being dried is 300 DEG C, and outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material.
The addition of CNT and polyvinyl alcohol is respectively the 4% and 5% of SiOx opaque amount, and consolidating of carbon nano tube paste contains Amount 6%.
Embodiment 12
By SiOx powder that mean diameter is 1 μm under the conditions of argon shield, temperature is 1100 DEG C, heat treatment time is 2 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 5 times, grind 3 hours in sand mill, obtain Homodisperse slurry；After the slurry obtained is mixed homogeneously with Graphene slurry and amino resins, it is spray-dried, is spray-dried Inlet temperature be 300 DEG C, outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material.
The addition of Graphene and amino resins is respectively the 3% and 3% of SiOx opaque amount, the solid content of Graphene slurry 6%。
Embodiment 13
By SiOx powder that mean diameter is 8 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 3 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 10 times, grind 5 hours in sand mill, To homodisperse slurry；The slurry obtained is mixed with the N-Methyl pyrrolidone solution of Graphene slurry and Kynoar After Jun Yun, being spray-dried, the inlet temperature of spray drying is 200 DEG C, and outlet temperature is 100 DEG C, obtains spheroidal particle SiOx multiple Close negative material.
The addition of the N-Methyl pyrrolidone solution of Graphene and Kynoar is respectively 3% He of SiOx opaque amount 5%, the solid content 6% of Graphene slurry.
Embodiment 14
By SiOx powder that mean diameter is 10 μm under the conditions of argon shield, temperature is 1100 DEG C, heat treatment time is 2 hours, Cool to room temperature with the furnace；In the SiOx powder processed, add the deionized water of its quality 8 times, grind 6 hours in sand mill, To homodisperse slurry；After the slurry obtained is mixed homogeneously with carbon nano tube paste and epoxy resin, it is spray-dried, spraying The inlet temperature being dried is 200 DEG C, and outlet temperature is 100 DEG C, obtains spheroidal particle SiOx composite negative pole material.
The addition of CNT and epoxy resin is respectively the 3% and 6% of SiOx opaque amount, and consolidating of carbon nano tube paste contains Amount 6%.
Embodiment 15
By SiOx powder that mean diameter is 8 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 3 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 8 times, grind 5 hours in sand mill, obtain Homodisperse slurry；After the slurry obtained is mixed homogeneously with Graphene slurry and styrene acrylic polymer emulsion, spray Mist is dried, and the inlet temperature of spray drying is 300 DEG C, and outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material Material.
The addition of Graphene and styrene acrylic polymer emulsion is respectively the 2% and 3% of SiOx opaque amount, graphite The solid content 6% of alkene slurry.
Embodiment 16
By SiOx powder that mean diameter is 3 μm under the conditions of argon shield, temperature is 1000 DEG C, heat treatment time is 3 hours, with Stove is cooled to room temperature；In the SiOx powder processed, add the deionized water of its quality 10 times, grind 3 hours in sand mill, To homodisperse slurry；After the slurry obtained is mixed homogeneously with Graphene slurry and VAE emulsion, Being spray-dried, the inlet temperature of spray drying is 300 DEG C, and outlet temperature is 130 DEG C, obtains spheroidal particle SiOx composite negative pole material Material.
The addition of Graphene and VAE emulsion is respectively the 2% and 6% of SiOx opaque amount, graphite The solid content 6% of alkene slurry.
SiOx composite negative pole material, conductive black and the binding agent CMC and the binding agent SBR that are prepared by above-described embodiment press Mass ratio 80:10:4:6, adds deionized water, and quickly stirring forms slurry.Slurry is evenly applied to 20 μ m-thick, a diameter of Make wet electrode on the Cu paper tinsel disk of 12mm, then wet electrode be placed at 60 DEG C be dried, wait be dried to half-dried after, use tablet machine Electrode is compacted, is vacuum dried 12h subsequently at 80 DEG C, prepares working electrode.By work in the vacuum glove box of full argon Electrode, metal lithium sheet, Celgard2400 barrier film, EC+DEC+EMC(volume ratio 1:1:1 of 1mol/L LiPF6) electrolyte assembling Becoming 2032 type button cells, button cell carries out electric performance test after standing 24 hours, and voltage range is 0.01 ~ 1.5V.
Carrying out testing material electrochemical performance test with 100mA/g current charge-discharge electricity, test result is as shown in table 1.
Table 1 SiOx composite negative pole material chemical property
Can be seen that from the result of table 1, SiOx composite negative pole material prepared by the present invention has good chemical property, from Fig. 1 SEM figure can be seen that, the SiOx composite negative pole material of preparation is spherical, wherein embodiment 7 SiOx composite negative pole material electrification Combination property is preferable, and its specific discharge capacity can reach 1280mAh/g, and first charge-discharge efficiency can reach 77.3%.

Claims (1)

1. a preparation method for SiOx composite negative pole material, is characterized in that method is as follows: be 1 ~ 20 μm by mean diameter SiOx powder under argon shield, temperature 900 ~ 1200 DEG C, heat treatment time 1 ~ 10 hour, naturally cool to room temperature；Above-mentioned SiOx powder adds deionized water or the dehydrated alcohol of its quality 3 ~ 10 times, grinds 0.5 ~ 10 hour, obtain homodisperse slurry Material；Being mixed homogeneously with conductive agent and binding agent by slurry, be spray-dried, the inlet temperature of spray drying is 200 ~ 350 DEG C, outlet Temperature is 80 ~ 140 DEG C, obtains described SiOx composite negative pole material.
CN201610470670.9A 2016-06-24 2016-06-24 Method for preparing SiOx composite anode material Pending CN105977463A (en)

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EP4131499A4 (en) * 2020-03-31 2023-07-26 Ningde Amperex Technology Limited Negative electrode material, negative electrode sheet, electrochemical device, and electronic device

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