CN105789590A - Preparation method of SiOx/C cathode material - Google Patents

Preparation method of SiOx/C cathode material Download PDF

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Publication number
CN105789590A
CN105789590A CN201610209607.XA CN201610209607A CN105789590A CN 105789590 A CN105789590 A CN 105789590A CN 201610209607 A CN201610209607 A CN 201610209607A CN 105789590 A CN105789590 A CN 105789590A
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siox
temperature
cathode material
preparation
room temperature
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唐仁衡
肖方明
王英
孙泰
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Guangdong Institute of Rare Metals
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Guangzhou Research Institute of Non Ferrous 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
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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 of a SiOx/C cathode material. The preparation method comprises the following steps: performing thermal treatment of silicon (II) oxide powder in an argon protection condition at a temperature of 800-1,100 DEG C, and cooling to room temperature along with furnace; uniformly mixing the treated silicon (II) oxide powder and an organic carbon source; adding deionized water or absolute ethyl alcohol; grinding the mixture to obtain nano slurry; performing spray drying of the obtained nano slurry to obtain a spherical particle precursor, wherein the entrance temperature of the spray drying is 200-350 DEG C, and the exit temperature is 90-150 DEG C; roasting the precursor for 2-12 hours at 500-900 DEG C in a nitrogen or argon protection atmosphere; cooling to room temperature; and crushing and sieving to obtain the SiOx/C composite cathode material. The SiOx/C composite cathode material prepared by the preparation method has the advantages of relatively high charge/discharge efficiency, relatively good cycle performance and the like and is suitable to be used as a cathode material of a lithium ion battery. According to the preparation method disclosed by the invention, the technology is simple, the cost is relatively low, and industrial production is facilitated.

Description

A kind of SiOx/C cathode material preparation method
Technical field
The present invention relates to lithium ion battery negative material field, the preparation method especially relating to a kind of SiOx/C negative material.
Background technology
From lithium ion battery 1991 by SONY industrialization so far, commodity lithium ion battery negative material is just monopolized by graphite-like material with carbon element always, through the development of more than 20 years, its energy density has been developed that to close to theoretical value level (theoretical specific capacity 372mAh/g), thus limiting the further raising of lithium ion battery energy density.Therefore, exploitation high-energy-density, high security, the Novel anode material of low cost and application technology thereof are the urgent tasks of field of batteries development.The sub-advantages such as silicium cathode material has specific capacity higher (theoretical specific capacity is more than 2000mAh/g), voltage platform is relatively low, the cost of raw material is cheap of oxidation, have applications well prospect in field of lithium ion battery.But there is the problems such as electric conductivity is poor, first charge-discharge efficiency is relatively low in the sub-silicium cathode material of oxidation.
For the problems referred to above that the sub-silicium cathode material of oxidation presently, there are, CN201310187373.X adopts a kind of surfactant to be template, PVP is that first auxiliary template agent prepares meso pore silicon oxide material, then carries out compound with carbon source, obtains aoxidizing sub-silicon/carbon composite by Technology for Heating Processing.Chinese patent 201310412962.3 discloses a kind of lithium ion battery cathode material and its preparation method, this preparation method by adding aluminum in the sub-silicon of raw material oxidation, obtaining aoxidizing the negative material of sub-silicon and aluminium oxide after heat treatment, this material first charge-discharge efficiency and specific capacity are improved.By above-mentioned improvement, the sub-silicium cathode material electrochemical performance of oxidation is improved, but cycle performance and first charge-discharge rate also need to improve.
Summary of the invention
Silicon materials first charge-discharge efficiency is relatively low, cycle performance is poor to the present invention is directed to existing oxidation Asia, it is provided that the preparation method of a kind of SiOx/C composite negative pole material.
The concrete technical scheme of the present invention:
1., by oxidation Asia silica flour that mean diameter is 1 ~ 20 μm when argon shield, temperature is 800 ~ 1100 DEG C, temperature retention time is carry out heat treatment in 1 ~ 10 hour, cools to room temperature with the furnace；
2. oxidation Asia silica flour step 1. processed and organic carbon source are in mass ratio for 1:1 ~ 10:1 Homogeneous phase mixing, it is subsequently adding deionized water or the dehydrated alcohol of solid mixture weight 0.5 ~ 5 times, said mixture is ground 0.5 ~ 6 hour, obtains homodisperse nano pulp；
3. nano pulp step 2. obtained carries out spray drying, and the inlet temperature of spray drying is 200 ~ 350 DEG C, and outlet temperature is 90 ~ 150 DEG C, obtains spheroidal particle presoma；
4. the presoma 3. step obtained under nitrogen or argon atmosphere, 500 ~ 900 DEG C of roastings 2 ~ 12 hours, be cooled to room temperature, then crush, sieve, obtain SiOx/C composite negative pole material.
Described organic carbon source is glucose, sucrose or phenolic resin.
Adopting the sub-silicon of common micro level oxidation is raw material, after high-temperature heat treatment, by dismutation reaction, forms certain proportion elemental silicon in the sub-silicon of oxidation.Oxidation Asia silicon powder after treatment, through nano ball grinding, mixes with organic carbon source, after spray drying, pyrolysis, obtains spherical SiO x/C composite wood negative pole material.SiOx/C composite wood negative pole material prepared by the present invention has that first charge-discharge efficiency is higher and the advantage such as cycle performance is better, is suitable for lithium ion battery negative pole materials'use.The preparation method technique of the present invention is simple, less costly, it is simple to industrialized production.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the SiOx/C composite negative pole material of embodiment 1,2 and 3 preparation；
Fig. 2 is the SiOx/C composite negative pole material SEM figure of embodiment 4 preparation；
Fig. 3 is SiOx/C composite negative pole material cycle performance curve (200mA/g) of embodiment 4 preparation.
Detailed description of the invention
Embodiment 1
By the oxidation Asia silica flour of mean diameter 5 μm in atmosphere protection stove, under argon shield, 950 DEG C of heat treatment 5h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and glucose, Homogeneous phase mixing by weight 5:1, be subsequently adding deionized water, mix homogeneously, the slurry of mix homogeneously is ground 3 hours in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 300 DEG C, and outlet temperature is 120 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under nitrogen protection atmosphere, 600 DEG C of roastings 6 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
Embodiment 2
By the oxidation Asia silica flour of mean diameter 8 μm in atmosphere protection stove, under argon shield, 1000 DEG C of heat treatment 3h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and sucrose, Homogeneous phase mixing by weight 4:1, be subsequently adding deionized water, mix homogeneously, the slurry of mix homogeneously is ground 5 hours in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 320 DEG C, and outlet temperature is 130 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under nitrogen protection atmosphere, 700 DEG C of roastings 5 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
Embodiment 3
By the oxidation Asia silica flour of mean diameter 3 μm in atmosphere protection stove, under argon shield, 1050 DEG C of heat treatment 5h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and phenolic resin, Homogeneous phase mixing by weight 5:1, be subsequently adding dehydrated alcohol, mix homogeneously, the slurry of mix homogeneously is ground 2 hours in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 250 DEG C, and outlet temperature is 90 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under argon atmosphere, 800 DEG C of roastings 3 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
Embodiment 4
By the oxidation Asia silica flour of mean diameter 1 μm in atmosphere protection stove, under argon shield, 1000 DEG C of heat treatment 3h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and glucose, Homogeneous phase mixing by weight 4:1, be subsequently adding deionized water, mix homogeneously, the slurry of mix homogeneously is ground 1 hour in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 340 DEG C, and outlet temperature is 140 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under argon atmosphere, 800 DEG C of roastings 6 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
Embodiment 5
By the oxidation Asia silica flour of mean diameter 3 μm in atmosphere protection stove, under argon shield, 900 DEG C of heat treatment 8h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and sucrose, Homogeneous phase mixing by weight 4:1, be subsequently adding deionized water 1000mL, mix homogeneously, the slurry of mix homogeneously is ground 3 hours in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 320 DEG C, and outlet temperature is 130 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under argon atmosphere, 900 DEG C of roastings 3 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
Embodiment 6
By the oxidation Asia silica flour of mean diameter 5 μm in atmosphere protection stove, under argon shield, 950 DEG C of heat treatment 5h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and phenolic resin, Homogeneous phase mixing by weight 5:1, be subsequently adding dehydrated alcohol, mix homogeneously, the slurry of mix homogeneously is ground 3 hours in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 280 DEG C, and outlet temperature is 90 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under nitrogen protection atmosphere, 700 DEG C of roastings 6 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
Embodiment 7
By the oxidation Asia silica flour of mean diameter 3 μm in atmosphere protection stove, under argon shield, 900 DEG C of heat treatment 5h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and glucose, Homogeneous phase mixing by weight 5:1, be subsequently adding deionized water, mix homogeneously, the slurry of mix homogeneously is ground 1 hour in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 340 DEG C, and outlet temperature is 140 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under nitrogen protection atmosphere, 700 DEG C of roastings 6 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
Embodiment 8
By the oxidation Asia silica flour of mean diameter 5 μm in atmosphere protection stove, under argon shield, 1000 DEG C of heat treatment 8h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and sucrose, Homogeneous phase mixing by weight 4:1, be subsequently adding deionized water 1000mL, mix homogeneously, the slurry of mix homogeneously is ground 3 hours in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 320 DEG C, and outlet temperature is 130 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under argon atmosphere, 800 DEG C of roastings 3 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
Embodiment 9
By the oxidation Asia silica flour of mean diameter 8 μm in atmosphere protection stove, under argon shield, 1000 DEG C of heat treatment 5h, it is cooled to room temperature.Weigh the oxidation Asia silica flour after process and phenolic resin, Homogeneous phase mixing by weight 5:1, be subsequently adding dehydrated alcohol 1000mL, mix homogeneously, the slurry of mix homogeneously is ground 3 hours in sand mill, obtain homodisperse nano oxidized sub-silicon slurry.The dry inlet temperature of adjustable spraying is 280 DEG C, and outlet temperature is 90 DEG C, spray-dried, obtains spheroidal particle presoma；By presoma under argon atmosphere, 900 DEG C of roastings 6 hours, be cooled to room temperature, then broken, cross 200 mesh sieves, obtain SiOx/C composite negative pole material.
SiOx/C composite negative pole material, conductive black and binding agent (CMC and the SBR) 80:10:4:6 in mass ratio prepared by above-described embodiment, adds deionized water, and quickly stirring forms slurry.Slurry is evenly applied to 20 μ m-thick, diameter is make wet electrode on the Cu paper tinsel disk of 12mm, then wet electrode is placed at 60 DEG C dry, wait be dried to half-dried after, use tablet machine electrode compacting, vacuum drying 12h at 80 DEG C, prepares working electrode subsequently.In the vacuum glove box of full argon by working electrode, metal lithium sheet, Celgard2400 barrier film, 1mol/LLiPF6 EC+DEC+EMC(volume ratio 1:1:1) electrolyte is assembled into 2032 type button cells, button cell carries out electric performance test after standing 24 hours, and voltage range is 0.01 ~ 1.5V.
Table 1SiOx/C composite negative pole material chemical property
Carrying out test material specific capacity with 100mA/g current charge-discharge electricity, carry out the cycle performance test of material with 200mA/g current charge-discharge electricity, test result is as shown in table 1.
From Fig. 1 different heat treatment temperature, the XRD figure of (embodiment 1 ~ 3) is found out, along with the raising of heat treatment temperature, the diffraction maximum of silicon becomes strong, and in material, the ratio of elemental silicon increases.Can be seen that from the result of table 1, adopt SiOx/C composite negative pole material prepared by the present invention to have good chemical property.Can be seen that from the SEM figure of Fig. 2, the SiOx/C composite negative pole material of preparation is spherical, wherein under embodiment 4 condition, the SiOx/C composite negative pole material chemical property of preparation is better (see table 1 and Fig. 3), its specific capacity can reach 1357mAh/g, and first charge-discharge efficiency is 76.7%, carries out with 200mA/g current charge-discharge electricity, after 50 times circulate, its special capacity fade rate is 2.2%.

Claims (2)

1. a SiOx/C cathode material preparation method, is characterized in that being made up of following steps:
1., by oxidation Asia silica flour that mean diameter is 1 ~ 20 μm when argon shield, temperature is 800 ~ 1100 DEG C, temperature retention time is carry out heat treatment in 1 ~ 10 hour, cools to room temperature with the furnace；
2. oxidation Asia silica flour step 1. processed and organic carbon source are in mass ratio for 1:1 ~ 10:1 Homogeneous phase mixing, it is subsequently adding deionized water or the dehydrated alcohol of solid mixture weight 0.5 ~ 5 times, said mixture is ground 0.5 ~ 6 hour, obtains homodisperse nano pulp；
3. nano pulp step 2. obtained carries out spray drying, and the inlet temperature of spray drying is 200 ~ 350 DEG C, and outlet temperature is 90 ~ 150 DEG C, obtains spheroidal particle presoma；
4. the presoma 3. step obtained under nitrogen or argon atmosphere, 500 ~ 900 DEG C of roastings 2 ~ 12 hours, be cooled to room temperature, then crush, sieve, obtain SiOx/C composite negative pole material.
2. SiOx/C cathode material preparation method according to claim 1, is characterized in that described organic carbon source is glucose, sucrose or phenolic resin.
CN201610209607.XA 2016-04-06 2016-04-06 Preparation method of SiOx/C cathode material Pending CN105789590A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108493438A (en) * 2018-04-27 2018-09-04 天津巴莫科技股份有限公司 A kind of lithium ion battery SiOxBase composite negative pole material and preparation method thereof
CN109888224A (en) * 2019-02-27 2019-06-14 福建翔丰华新能源材料有限公司 A kind of lithium ion battery negative material preparation method of silicon oxygen carbon and alumina composite
CN110518203A (en) * 2019-08-06 2019-11-29 内蒙古凯金新能源科技有限公司 Compound soft carbon negative electrode material and preparation method thereof, lithium ion battery
CN111115639A (en) * 2019-12-25 2020-05-08 湖北万润新能源科技发展有限公司 Preparation of SiO by centering reactionxMethod and application of @ C material
CN112103467A (en) * 2020-08-06 2020-12-18 双登集团股份有限公司 Lithium ion battery cathode
CN112421008A (en) * 2020-11-23 2021-02-26 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of carbon-coated silicon monoxide material for lithium ion battery cathode, product and application thereof
CN113948686A (en) * 2021-09-13 2022-01-18 惠州市贝特瑞新材料科技有限公司 Porous spherical silicon-based composite anode material, preparation method thereof and battery

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103413922A (en) * 2013-08-14 2013-11-27 宁波奈克斯特新材料科技有限公司 Lithium ion battery negative electrode material and preparation method thereof
CN104022257A (en) * 2014-06-16 2014-09-03 深圳市贝特瑞新能源材料股份有限公司 Silicon dioxide composite anode material for lithium ion battery, as well as preparation method and application of silicon dioxide composite anode material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103413922A (en) * 2013-08-14 2013-11-27 宁波奈克斯特新材料科技有限公司 Lithium ion battery negative electrode material and preparation method thereof
CN104022257A (en) * 2014-06-16 2014-09-03 深圳市贝特瑞新能源材料股份有限公司 Silicon dioxide composite anode material for lithium ion battery, as well as preparation method and application of silicon dioxide composite anode material

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108493438A (en) * 2018-04-27 2018-09-04 天津巴莫科技股份有限公司 A kind of lithium ion battery SiOxBase composite negative pole material and preparation method thereof
CN109888224A (en) * 2019-02-27 2019-06-14 福建翔丰华新能源材料有限公司 A kind of lithium ion battery negative material preparation method of silicon oxygen carbon and alumina composite
CN110518203A (en) * 2019-08-06 2019-11-29 内蒙古凯金新能源科技有限公司 Compound soft carbon negative electrode material and preparation method thereof, lithium ion battery
CN111115639A (en) * 2019-12-25 2020-05-08 湖北万润新能源科技发展有限公司 Preparation of SiO by centering reactionxMethod and application of @ C material
CN112103467A (en) * 2020-08-06 2020-12-18 双登集团股份有限公司 Lithium ion battery cathode
CN112421008A (en) * 2020-11-23 2021-02-26 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of carbon-coated silicon monoxide material for lithium ion battery cathode, product and application thereof
CN112421008B (en) * 2020-11-23 2022-09-02 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of carbon-coated silicon monoxide material for lithium ion battery cathode, product and application thereof
CN113948686A (en) * 2021-09-13 2022-01-18 惠州市贝特瑞新材料科技有限公司 Porous spherical silicon-based composite anode material, preparation method thereof and battery

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