CN105489891A - Preparation method for high-capacity silicon-based negative electrode material for lithium ion battery - Google Patents
Preparation method for high-capacity silicon-based negative electrode material for lithium ion battery Download PDFInfo
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- CN105489891A CN105489891A CN201510965400.0A CN201510965400A CN105489891A CN 105489891 A CN105489891 A CN 105489891A CN 201510965400 A CN201510965400 A CN 201510965400A CN 105489891 A CN105489891 A CN 105489891A
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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
- H01M4/58—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
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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
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- 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 discloses a preparation method for a high-capacity silicon-based negative electrode material for a lithium ion battery. The silicon-based negative electrode material for the lithium ion battery is prepared by adopting mesoporous carbon and nanometer silicon as raw materials in a compounding manner, wherein the mesoporous carbon and nanometer silicon are prepared by adopting a special process, so that the carbon and silicon are uniformly distributed and combined in a more tight manner; and therefore, when the composite material is used for the lithium ion battery, the obtained lithium ion battery is relatively high in conductivity, high in cycling stability, high in specific capacity and relatively long in service life.
Description
Art
The present invention relates to a kind of preparation method of lithium ion battery high power capacity silicon based anode material.
Background technology
Lithium ion battery as a kind of novel chemical power source, because its output voltage is high, specific energy is high, have extended cycle life, self discharge is little, safety, memory-less effect and environmental friendliness have become the emphasis that our times various countries develop in new energy materials field.Electrode material is the principal element affecting battery performance and cost, and research and development electrode material is to the great significance of lithium battery.Current commercial lithium ion battery negative adopts graphitized carbon, and as carbonaceous mesophase spherules MCMB and CMS material, in this kind of material doff lithium process, volumetric expansion is substantially below 9%, shows higher coulombic efficiency and excellent stable circulation performance.But the embedding lithium capacity of the theory of graphite is 372mAh/g, reality reaches 370mAh/g, therefore, the theoretical lithium storage content that graphite electrode itself is lower makes it be difficult to make a breakthrough again, and the electrode material that researcher is exploring a kind of Novel high-specific capacity flexible always carrys out alternative graphitized carbon material.The theoretical capacity of silicon, up to 4200mAh/g, uses silicium cathode significantly can improve the energy density of lithium ion battery, but silicon change in volume in charge and discharge process huge (about 300%), and cyclical stability is poor.In addition, the conductivity of silicon is not high, and intrinsic conductivity is very low.Therefore, developing a kind of conductance high and effectively can suppress the preparation technology of the bulk effect of silicon, is prepare high power capacity silicon based anode material to prepare one of difficult problem that high-capacity lithium ion cell field will solve.
Summary of the invention
For overcoming above-mentioned deficiency, the invention provides a kind of preparation method of lithium ion battery high power capacity silicon based anode material, the positive electrode using the method to prepare, has good electric conductivity and cyclical stability.
To achieve these goals, the preparation method of a kind of lithium ion battery high power capacity silicon based anode material provided by the invention, comprises the steps:
(1) silicon nanoparticle is prepared
Under an argon atmosphere silicon monoxide is heated, make it that disproportionated reaction occur, heating condition is react 8-12h at 1000-1200 DEG C, generate silicon dioxide coated nano silicon grain, silicon dioxide coated nano silicon grain is mixed with the hydrofluoric acid of 35-40wt% and carries out corrosion treatment, fallen by silicon dioxide etching again through being separated to obtain silicon nanoparticle, addition is pressed silicon dioxide and hydrofluoric acid mol ratio 1: 5-1: 10 in product and is calculated, and the corrosion treatment time is 10-20h;
(2) meso-porous carbon material is prepared
Resorcinol and surfactant F127 are dissolved in the mixed system of ethanol and distilled water, by the mol ratio 1:1-2 of resorcinol and surfactant F127, after vigorous stirring is all dissolved, add citric acid, after stirring 2-3h, add 37wt% formalin, the mol ratio of formaldehyde and citric acid is 3-15, continuing stirring makes it start slowly to be polymerized and obtain oligomeric compound, proceed in reactor after 2-4h is carried out in reaction, 70-90 DEG C of aging 20-40h, after obtain the whippy solids of salmon pink, then wash, dry, in nitrogen atmosphere, 800-1200 DEG C of carbonization 5-8h obtains meso-porous carbon material again,
(3) mesoporous carbon/silicon composite is prepared
Above-mentioned nano-silicon is mixed with the ratio of mesoporous carbon according to mass ratio 3:1-1:3, joining concentration is stir 1-2h in the hydrofluoric acid solution of 20-30wt%, ultrasonic disperse 4-5h afterwards, filtration after ultrasonic disperse completes, with distilled water water washing removing hydrofluoric acid, fluosilicic acid etc., 120-130 DEG C of desciccate obtains the carbon-silicon composite material that black product is composite Nano silicon particle between mesoporous carbon basis material space.
The silica-based composite negative pole material of lithium ion battery prepared by the present invention, have employed mesoporous carbon prepared by special process and nano-silicon is composited as raw material, carbon silicon is distributed uniformly and combines more tight, therefore this composite material is when for lithium ion battery, there is higher electric conductivity and good cyclical stability, make lithium ion battery have high specific capacity and longer useful life.
Embodiment
Embodiment one
Prepare silicon nanoparticle
Under an argon atmosphere silicon monoxide is heated, make it that disproportionated reaction occur, heating condition is react 12h at 1000 DEG C, generate silicon dioxide coated nano silicon grain, silicon dioxide coated nano silicon grain is mixed with the hydrofluoric acid of 35wt% and carries out corrosion treatment, fallen by silicon dioxide etching again through being separated to obtain silicon nanoparticle, addition is pressed silicon dioxide and hydrofluoric acid mol ratio 1: 5 in product and is calculated, and the corrosion treatment time is 10h.
Prepare meso-porous carbon material
Resorcinol and surfactant F127 are dissolved in the mixed system of ethanol and distilled water, by the mol ratio 1:1 of resorcinol and surfactant F127, after vigorous stirring is all dissolved, add citric acid, after stirring 2h, add 37wt% formalin, the mol ratio of formaldehyde and citric acid is 3, continuing stirring makes it start slowly to be polymerized and obtain oligomeric compound, proceed in reactor after 4h is carried out in reaction, 70 DEG C of aging 40h, after obtain the whippy solids of salmon pink, then wash, dry, in nitrogen atmosphere, 800 DEG C of carbonization 8h obtain meso-porous carbon material again.
Preparation mesoporous carbon/silicon composite
Above-mentioned nano-silicon is mixed with the ratio of mesoporous carbon according to mass ratio 3:1, joining concentration is stir 2h in the hydrofluoric acid solution of 20wt%, ultrasonic disperse 5h afterwards, filtration after ultrasonic disperse completes, with distilled water water washing removing hydrofluoric acid, fluosilicic acid etc., 120 DEG C of desciccates obtain the carbon-silicon composite material that black product is composite Nano silicon particle between mesoporous carbon basis material space.
Embodiment two
Prepare silicon nanoparticle
Under an argon atmosphere silicon monoxide is heated, make it that disproportionated reaction occur, heating condition is react 8h at 1200 DEG C, generate silicon dioxide coated nano silicon grain, silicon dioxide coated nano silicon grain is mixed with the hydrofluoric acid of 40wt% and carries out corrosion treatment, fallen by silicon dioxide etching again through being separated to obtain silicon nanoparticle, addition is pressed silicon dioxide and hydrofluoric acid mol ratio 1: 10 in product and is calculated, and the corrosion treatment time is 10h.
Prepare meso-porous carbon material
Resorcinol and surfactant F127 are dissolved in the mixed system of ethanol and distilled water, by the mol ratio 1:2 of resorcinol and surfactant F127, after vigorous stirring is all dissolved, add citric acid, after stirring 3h, add 37wt% formalin, the mol ratio of formaldehyde and citric acid is 15, continuing stirring makes it start slowly to be polymerized and obtain oligomeric compound, proceed in reactor after 2h is carried out in reaction, 90 DEG C of aging 20h, after obtain the whippy solids of salmon pink, then wash, dry, in nitrogen atmosphere, 1200 DEG C of carbonization 5h obtain meso-porous carbon material again.
Preparation mesoporous carbon/silicon composite
Above-mentioned nano-silicon is mixed with the ratio of mesoporous carbon according to mass ratio 1:3, joining concentration is stir 1h in the hydrofluoric acid solution of 30wt%, ultrasonic disperse 4h afterwards, filtration after ultrasonic disperse completes, with distilled water water washing removing hydrofluoric acid, fluosilicic acid etc., 130 DEG C of desciccates obtain the carbon-silicon composite material that black product is composite Nano silicon particle between mesoporous carbon basis material space.
Comparative example
0.1g silica flour (average grain diameter 100nm) and 0.0417g graphene oxide are dispersed in 100ml deionized water, ultrasonic 45min makes it be uniformly dispersed, then spraying dry is carried out, inlet temperature is at 200 DEG C, outlet temperature is at 110 DEG C, removing deionized water, obtains the composite material of graphene oxide and silicon; Then be placed in high temperature furnace, pass into the mist of hydrogen and argon gas, in the mist of hydrogen and argon gas, the volume content of hydrogen is 20%, first be warming up to 700 DEG C and carry out the high temperature anneal, be incubated 3 hours, graphene oxide is reduced, then naturally cools to room temperature, obtain silicon graphene composite negative pole material.
Above-described embodiment one, two and comparative example products therefrom are mixed with the binding agent of the 10wt% 1-METHYLPYRROLIDONE solution of the Kynoar of 0.02g/ml (solid content to be the butadiene-styrene rubber-sodium carboxymethylcellulose emulsion of 2wt% or concentration be) and the conductive agent (SuperP conductive carbon black) of 15wt%, be coated in after stirring on Copper Foil, put into baking oven 60 DEG C ~ 80 DEG C oven dry.Be washed into pole piece with the drift of diameter 12 ~ 16mm again, put into vacuum drying oven at 60 DEG C ~ 120 DEG C dry 4 ~ 12 hours, then transfer to and be full of in the glove box of argon gas.Be to electrode with metal lithium sheet, ENTEKPE perforated membrane is barrier film, and the ethylene carbonate of 1mol/L lithium hexafluoro phosphate and dimethyl carbonate (volume ratio 1:1) mixed solution are electrolyte, are assembled into CR2016 button cell.At probe temperature is 25 DEG C, carry out electric performance test, after tested this embodiment one with two material compared with the product of comparative example, specific capacity improves 47-56%, improves more than 1.6 times useful life.
Claims (1)
1. a lithium ion battery preparation method for high power capacity silicon based anode material, comprises the steps:
(1) silicon nanoparticle is prepared
Under an argon atmosphere silicon monoxide is heated, make it that disproportionated reaction occur, heating condition is react 8-12h at 1000-1200 DEG C, generate silicon dioxide coated nano silicon grain, silicon dioxide coated nano silicon grain is mixed with the hydrofluoric acid of 35-40wt% and carries out corrosion treatment, fallen by silicon dioxide etching again through being separated to obtain silicon nanoparticle, addition is pressed silicon dioxide and hydrofluoric acid mol ratio 1: 5-1: 10 in product and is calculated, and the corrosion treatment time is 10-20h;
(2) meso-porous carbon material is prepared
Resorcinol and surfactant F127 are dissolved in the mixed system of ethanol and distilled water, by the mol ratio 1:1-2 of resorcinol and surfactant F127, after vigorous stirring is all dissolved, add citric acid, after stirring 2-3h, add 37wt% formalin, the mol ratio of formaldehyde and citric acid is 3-15, continuing stirring makes it start slowly to be polymerized and obtain oligomeric compound, proceed in reactor after 2-4h is carried out in reaction, 70-90 DEG C of aging 20-40h, after obtain the whippy solids of salmon pink, then wash, dry, in nitrogen atmosphere, 800-1200 DEG C of carbonization 5-8h obtains meso-porous carbon material again,
(3) mesoporous carbon/silicon composite is prepared
Above-mentioned nano-silicon is mixed with the ratio of mesoporous carbon according to mass ratio 3:1-1:3, joining concentration is stir 1-2h in the hydrofluoric acid solution of 20-30wt%, ultrasonic disperse 4-5h afterwards, filtration after ultrasonic disperse completes, with distilled water water washing removing hydrofluoric acid, fluosilicic acid etc., 120-130 DEG C of desciccate obtains the carbon-silicon composite material that black product is composite Nano silicon particle between mesoporous carbon basis material space.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3336936A1 (en) * | 2016-12-16 | 2018-06-20 | Optimum Battery Co., Ltd. | Method for preparing negative electrode of lithium ion battery and lithium ion battery |
| EP3477748A1 (en) * | 2017-10-13 | 2019-05-01 | Volkswagen Aktiengesellschaft | Increase of the life of silicon-based negative electrodes by particles with silicon oxide and lipon coating |
| CN109786727A (en) * | 2018-12-29 | 2019-05-21 | 湖南中科星城石墨有限公司 | A method of preparing high-purity nm silicon |
| US10424786B1 (en) | 2018-12-19 | 2019-09-24 | Nexeon Limited | Electroactive materials for metal-ion batteries |
| US10508335B1 (en) | 2019-02-13 | 2019-12-17 | Nexeon Limited | Process for preparing electroactive materials for metal-ion batteries |
| CN110931744A (en) * | 2019-11-29 | 2020-03-27 | 深圳技术大学 | Silicon-carbon negative electrode material and preparation method thereof |
| US10964940B1 (en) | 2020-09-17 | 2021-03-30 | Nexeon Limited | Electroactive materials for metal-ion batteries |
| US11011748B2 (en) | 2018-11-08 | 2021-05-18 | Nexeon Limited | Electroactive materials for metal-ion batteries |
| US11165054B2 (en) | 2018-11-08 | 2021-11-02 | Nexeon Limited | Electroactive materials for metal-ion batteries |
| US11905593B2 (en) | 2018-12-21 | 2024-02-20 | Nexeon Limited | Process for preparing electroactive materials for metal-ion batteries |
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