CN106356515A - Preparation method of silicon oxide composite material - Google Patents
Preparation method of silicon oxide composite material Download PDFInfo
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- CN106356515A CN106356515A CN201610965923.XA CN201610965923A CN106356515A CN 106356515 A CN106356515 A CN 106356515A CN 201610965923 A CN201610965923 A CN 201610965923A CN 106356515 A CN106356515 A CN 106356515A
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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
- H01M4/366—Composites as layered products
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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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Abstract
The invention provides a preparation method of a silicon oxide composite material, relating to the field of lithium ion battery negative electrode materials. The preparation method comprises the following steps: in an argon protective atmosphere, carrying out heat treatment on silicon oxide powder; adding deionized water or anhydrous ethanol, and grinding to obtain a nano slurry; adding an organic carbon source and a conductive nano material, and uniformly mixing to obtain a nano mixed slurry; carrying out spray drying on the nano mixed slurry to obtain a precursor; and in a nitrogen or argon protective atmosphere, roasting the precursor to obtain the silicon oxide composite material. The silicon oxide composite material prepared by the invention has the advantages of first charge/discharge coulomb efficiency, favorable cycle performance and the like. The preparation method has the advantages of simple technique and lower cost, is convenient for industrial production, and is suitable for lithium ion battery negative electrode materials.
Description
Technical field
The present invention relates to lithium ion battery negative material field, it is specifically related to a kind of silicon oxide composite material (siox)
Preparation method.
Background technology
From lithium ion battery industrialization so far, commodity lithium ion just has been used up graphite-like material with carbon element (theoretical specific capacity
372mah/g) as cell negative electrode material, its energy density has been developed that to close to theoretical value level at present, thus limiting lithium
The raising further of ion battery energy density.Therefore, exploitation high-energy-density, high security, the new negative pole material of low cost
Material and its application technology are the urgent tasks that field of batteries develops.The going out of silicon based anode material (theoretical specific capacity 4200mah/g)
It is now that the research of lithium ion battery with high energy density provides material foundation, middle change in volume that then crystalline silicon is embedding, de- lithium comes
Up to 300%, so big change in volume causes material structure and destroys and mechanical efflorescence, makes between active material and activity
Separate between material and collector, lead to its capacity attenuation, cycle performance deteriorates, and the conductivity of crystalline silicon is low, limits further
Make its commercial applications.
The sub- silicon materials of oxidation have higher specific capacity (theoretical specific capacity is more than 2000mah/g), during de- lithium easily
Generate electrochemistry can not anti-phase li2O has cushioning effect, and there is the si- strong compared with si-si key in the sub- silicium cathode material of oxidation
O key, therefore aoxidizes sub- bulk effect (change in volume about 170%) in charge and discharge process for the silicium cathode material compared with silicon based electrode material
Material is less, cycle performance is also superior compared with silicon based electrode.But the sub- silicium cathode material of oxidation exists, and electric conductivity is poor, first charge-discharge effect
The problems such as rate is relatively low, and cycle life does not reach market application requirement yet.
The problems referred to above that presently, there are for the sub- silicium cathode material of oxidation, cn201410268192.4 pass through silicon dioxide and
The sub- silicon of oxidation prepared by metallic silicon, then adopts kneading, roller sheet and the technique such as compressing to realize the carbon-coating cladding of the sub- silicon of oxidation
Structure, thermally treated obtains aoxidizing sub- silicon-carbon composite cathode material.Coulombic efficiency is 77 ~ 78% to this material first, reversible specific capacity
It is up to more than 1600mah/g, but cycle life low (circulation volume conservation rate was 70% about in 50 weeks).
Cn201510026862.6 discloses a kind of lithium ion battery silicon monoxide composite cathode material and preparation method thereof, purposes.Its
Preparation method is by siox after high-temperature process, obtains presoma, presoma by high temperature by organic carbon source gas
Silicon monoxide composite cathode material is obtained by mechanical fusion, coulombic efficiency is 78% to this material first, and reversible specific capacity is
1650mah/g, but cycle life low (circulation volume conservation rate was 70% in 50 weeks).By above-mentioned improvement, the sub- silicon composite cathode of oxidation
Material initial coulomb efficiency and conductivity are increased, but cycle performance still reaches to less than market application requirement.
Content of the invention
The present invention is directed to that the sub- silicon composite first charge-discharge efficiency of existing oxidation is relatively low, cycle performance is poor, provides one
Plant the preparation method of silicon oxide composite material (siox).
The present invention provides a kind of preparation method of silicon oxide composite material, provides the silicon oxide particles containing si crystal to make
For core, and coating comprises organic carbon source and the electrical-conductive nanometer material of carbon, Ran Houjin at least a portion surface of described core
Row heat treatment is to form the shell as coating.
Technical scheme is as follows:
(1), in 800 ~ 1100 DEG C of temperature, under argon gas atmosphere protection, mean diameter is 1 ~ 20 μm of oxidation Asia silicon (sio) powder heat
After processing 1 ~ 10 hour, cool to room temperature with the furnace；
(2) the oxidation Asia silica flour after step (1) heat treatment is crossed 60 mesh sieves, add the deionization of sub- 2 ~ 15 times of the silica flour quality of oxidation
Water or dehydrated alcohol, grind 0.5 ~ 6 hour, obtain nano pulp；Add aoxidize the organic carbon source of sub- siliceous amount 20 ~ 50% and 0 ~
15% electrical-conductive nanometer material, uses dispersed with stirring 0.5 ~ 3 hour after mix homogeneously, obtains a nanometer mixed slurry；
(3) the nanometer mixed slurry obtaining step (2) is in 200 ~ 350 DEG C of inlet temperature, under the conditions of 90 ~ 150 DEG C of outlet temperature
It is spray-dried, obtain presoma；
(4) presoma obtaining step (3) is under nitrogen or argon atmosphere, 500 ~ 900 DEG C of sintering temperature, the time 2 ~ 12
Hour, it is cooled to room temperature, obtain described silicon oxide composite material.
Described organic carbon source is Polyvinylpyrrolidone, polyaerylic acid, polyethylene glycol oxide or carboxylic styrene butadiene latex.
Described electrical-conductive nanometer material is in Graphene, carbon nano-fiber or CNT.
Aoxidizing sub- silicon (sio) using common micro level is raw material, after high-temperature heat treatment, is formed certain in the sub- silicon of oxidation
Ratio elemental silicon, can increase the specific capacity of composite.Oxidation Asia silicon powder after heat treatment is after nano ball grinding, and organic
Carbon source and electrical-conductive nanometer material dispersion mixing uniformly, obtain silicon oxide composite material after being spray-dried, being pyrolyzed.
The coating of the carbonaceous material of the present invention for the carbon-coating of organic carbon source cracking formation or the carbon of organic carbon source cracking and is led
The compound carbon-coating that electric nano material is formed.The silicon oxide composite material of the inventive method preparation has first charge-discharge coulomb effect
The advantages of rate is higher, cycle performance is preferable, preparation method process is simple, cost is relatively low, is easy to industrialized production, be suitable for lithium from
Sub- cell negative electrode material uses.
Brief description
Fig. 1 is the xrd figure of the silicon oxide composite material of embodiment 1,2 and 3 preparation.
Fig. 2 is the silicon oxide composite material tem figure of embodiment 9 preparation, wherein 1. c layers, 2. si and siox mixed layer,
3. siox.
Silicon oxide composite material cycle performance curve (200ma/g) that Fig. 3 is prepared for embodiment 1-9.
The silicon oxide composite material cyclic process that Fig. 4 is prepared for embodiment 1-9, capability retention (200ma/g).
Specific embodiment
Embodiment 1
By sub- for 5 μm of oxidation of mean diameter silicon (sio) powder under argon gas atmosphere protection, 950 DEG C of heat treatment 5h, it is cooled to room temperature；
Oxidation Asia silica flour after heat treatment is crossed 60 mesh sieves, is subsequently adding 10 times of the sub- silica flour quality of oxidation of deionized water, grinds 3 little
When, obtain homodisperse nano pulp；It is subsequently adding the polyethylene glycol oxide aoxidizing sub- siliceous amount 20% in slurry, mix homogeneously
Disperseed 1 hour with high velocity dispersators afterwards, obtain finely dispersed nanometer mixed slurry.Adjustable spraying is dried inlet temperature
300 DEG C, outlet temperature is 120 DEG C, spray-dried, obtains presoma；By presoma under nitrogen protection atmosphere, 700 DEG C of roastings
Burn 3 hours, be cooled to room temperature, then crush, cross 200 mesh sieves, obtain silicon oxide composite material.
Embodiment 2
By sub- for 10 μm of oxidation of mean diameter silicon (sio) powder under argon gas atmosphere protection, 1000 DEG C of heat treatment 4h, it is cooled to room
Temperature；Oxidation Asia silica flour after heat treatment is crossed 60 mesh sieves, is subsequently adding 11 times of the sub- silica flour quality of oxidation of deionized water, grinds
5 hours, obtain homodisperse nano pulp；It is subsequently adding the polyaerylic acid aoxidizing sub- siliceous amount 25% in slurry, mix homogeneously
Disperseed 0.5 hour with high velocity dispersators afterwards, obtain finely dispersed nanometer mixed slurry.Adjustable spraying is dried inlet temperature
For 320 DEG C, outlet temperature is 130 DEG C, spray-dried, obtains presoma；By presoma under nitrogen protection atmosphere, 800 DEG C
Roasting 5 hours, is cooled to room temperature, then crushes, crosses 200 mesh sieves, obtains silicon oxide composite material.
Embodiment 3
By sub- for 4 μm of oxidation of mean diameter silicon (sio) powder under argon gas atmosphere protection, 1050 DEG C of heat treatment 4h, it is cooled to room temperature.
Oxidation Asia silica flour after heat treatment is crossed 60 mesh sieves, is subsequently adding 9 times of the sub- silica flour quality of oxidation of dehydrated alcohol, grinds 3 little
When, obtain homodisperse nano pulp；It is subsequently adding the Polyvinylpyrrolidone aoxidizing sub- siliceous amount 30% in slurry, mixing
Disperseed 0.5 hour with high velocity dispersators after uniformly, obtain finely dispersed nanometer mixed slurry.Adjustable spraying is dried import
Temperature is 250 DEG C, and outlet temperature is 90 DEG C, spray-dried, obtains presoma；By presoma under nitrogen protection atmosphere, 700
DEG C roasting 3 hours, is cooled to room temperature, then crushes, crosses 200 mesh sieves, obtains silicon oxide composite material.
Embodiment 4
By sub- for 1 μm of oxidation of mean diameter silicon (sio) powder under argon gas atmosphere protection, 1000 DEG C of heat treatment 3h, it is cooled to room temperature.
Oxidation Asia silica flour after heat treatment is crossed 60 mesh sieves, is subsequently adding 8 times of the sub- silica flour quality of oxidation of deionized water, grinds 1 little
When, obtain homodisperse nano pulp；It is subsequently adding the carboxylic styrene butadiene latex aoxidizing sub- siliceous amount 25% in slurry, mixing is all
Disperseed 0.5 hour with high velocity dispersators after even, obtain finely dispersed nanometer mixed slurry.Adjustable spraying is dried import temperature
Spend for 240 DEG C, outlet temperature is 140 DEG C, spray-dried, obtains presoma；By presoma under nitrogen protection atmosphere, 600
DEG C roasting 6 hours, is cooled to room temperature, then crushes, crosses 200 mesh sieves, obtains silicon oxide composite material.
Embodiment 5
By sub- for 3 μm of oxidation of mean diameter silicon (sio) powder under argon gas atmosphere protection, 900 DEG C of heat treatment 8h, it is cooled to room temperature.
Oxidation Asia silica flour after heat treatment is crossed 60 mesh sieves, is subsequently adding 12 times of the sub- silica flour quality of oxidation of deionized water, grinds 3 little
When, obtain homodisperse nano pulp；It is subsequently adding the Polyvinylpyrrolidone that aoxidizes sub- siliceous amount 25% in slurry and 5%
Graphene, is disperseed 1 hour with high velocity dispersators after mix homogeneously, obtains finely dispersed nanometer mixed slurry.Adjust spray
Mist is dried inlet temperature and is 320 DEG C, and outlet temperature is 130 DEG C, spray-dried, obtains presoma；Presoma is protected in nitrogen
Under shield atmosphere, 700 DEG C of roastings 3 hours, it is cooled to room temperature, then crush, cross 200 mesh sieves, obtain silicon oxide composite material.
Embodiment 6
By sub- for 5 μm of oxidation of mean diameter silica flour under argon gas atmosphere protection, 950 DEG C of heat treatment 6h, it is cooled to room temperature.At heat
60 mesh sieves crossed by oxidation Asia silica flour after reason, are subsequently adding 11 times of the sub- silica flour quality of oxidation of dehydrated alcohol, grind 3 hours, obtain
To homodisperse nano pulp；It is subsequently adding the polyaerylic acid aoxidizing sub- siliceous amount 20% in slurry and 10% CNT,
Disperseed 2 hours with high velocity dispersators after mix homogeneously, obtain finely dispersed nanometer mixed slurry.Adjustable spraying is dried
Mouth temperature is 280 DEG C, and outlet temperature is 90 DEG C, spray-dried, obtains presoma；By presoma under nitrogen protection atmosphere,
800 DEG C of roastings 6 hours, are cooled to room temperature, then crush, cross 200 mesh sieves, obtain silicon oxide composite material.
Embodiment 7
By sub- for 3 μm of oxidation of mean diameter silica flour under argon gas atmosphere protection, 900 DEG C of heat treatment 5h, it is cooled to room temperature.At heat
60 mesh sieves crossed by oxidation Asia silica flour after reason, are subsequently adding 11 times of the sub- silica flour quality of oxidation of deionized water mix homogeneously, grind 3
Hour, obtain homodisperse nano pulp；It is subsequently adding the polyethylene glycol oxide that aoxidizes sub- siliceous amount 30% in slurry and 11%
Carbon nano-fiber, is disperseed 2 hours with high velocity dispersators after mix homogeneously, obtains finely dispersed nanometer mixed slurry.Adjust
Section is spray-dried inlet temperature and is 340 DEG C, and outlet temperature is 140 DEG C, spray-dried, obtains presoma；By presoma in nitrogen
Under gas shielded atmosphere, 900 DEG C of roastings 5 hours, it is cooled to room temperature, then crush, cross 200 mesh sieves, obtain Si oxide composite wood
Material.
Embodiment 8
By sub- for 5 μm of oxidation of mean diameter silica flour under argon gas atmosphere protection, 1000 DEG C of heat treatment 8h, it is cooled to room temperature.By heat
60 mesh sieves crossed by oxidation Asia silica flour after process, are subsequently adding 10 times of the sub- silica flour quality of oxidation of deionized water mix homogeneously, grind
Mill 3 hours, obtains homodisperse nano pulp；Be subsequently adding aoxidize in slurry sub- siliceous amount 15% carboxylic styrene butadiene latex and
10% CNT, is disperseed 1.5 hours with high velocity dispersators after mix homogeneously, obtains finely dispersed nanometer mixing slurry
Material.Adjustable spraying is dried inlet temperature and is 320 DEG C, and outlet temperature is 130 DEG C, spray-dried, obtains presoma；By presoma
Under nitrogen protection atmosphere, 700 DEG C of roastings 3 hours, it is cooled to room temperature, then crush, cross 200 mesh sieves, obtain Si oxide multiple
Condensation material.
Embodiment 9
By sub- for 8 μm of oxidation of mean diameter silica flour under argon gas atmosphere protection, 1000 DEG C of heat treatment 6h, it is cooled to room temperature.By heat
60 mesh sieves crossed by oxidation Asia silica flour after process, are subsequently adding 10 times of the sub- silica flour quality of oxidation of dehydrated alcohol mix homogeneously, grind
Mill 5 hours, obtains homodisperse nano pulp；Be subsequently adding aoxidize in slurry sub- siliceous amount 15% carboxylic styrene butadiene latex and
5% Graphene, is disperseed 1 hour with high velocity dispersators after mix homogeneously, obtains finely dispersed nanometer mixed slurry.Adjust
Section is spray-dried inlet temperature and is 280 DEG C, and outlet temperature is 90 DEG C, spray-dried, obtains presoma；By presoma in nitrogen
Under protective atmosphere, 700 DEG C of roastings 4 hours, it is cooled to room temperature, then crush, cross 200 mesh sieves, obtain silicon oxide composite material.
Quality pressed by silicon oxide composite material, conductive black and binding agent (cmc and sbr) that above-described embodiment is obtained
Ratio 80:10:4:6, adds deionized water, and quick stirring forms slurry.Slurry is evenly applied to 20 μ m-thick, a diameter of 12mm
Make wet electrode on cu paper tinsel disk, then wet electrode be placed at 60 DEG C be dried, wait be dried to half-dried after, using tablet machine electrode
Compacting, is subsequently vacuum dried 12h at 80 DEG C, obtains working electrode.In the vacuum glove box full of argon by working electrode,
Metal lithium sheet, celgard2400 barrier film, ec+dec+emc(volume ratio 1:1:1 of 1mol/llipf6) electrolyte is assembled into 2032
Type button cell, button cell standing carries out electric performance test in 24 hours afterwards, and test voltage scope is 0.01 ~ 1.5v.
Test material specific capacity is carried out with 100ma/g current charge-discharge electricity, following of material is carried out with 200ma/g current charge-discharge electricity
Ring performance test, test result is as shown in table 1.
Silicon oxide composite material in above-described embodiment is carried out xrd, tem and eds quantitative analyses.
Table 1 is silicon oxide composite material chemical property and x value analysis result.
Find out from the xrd figure of Fig. 1, the sub- silica flour of oxidation becomes strong, in material with the raising of heat treatment temperature, the diffraction maximum of silicon
The ratio of elemental silicon increases.Can be seen that from table 1 test result, the silicon oxide composite material using present invention preparation has well
Chemical property,.Can be seen that from the tem figure of Fig. 2, the silicon oxide composite material granule of preparation is by simple substance si and the sub- silicon of oxidation
(siox) form, on a part of surface and comprise the coating of material with carbon element.Under the conditions of embodiment 9, the Si oxide of preparation is combined
Preferably (being shown in Table 1, Fig. 3 and Fig. 4), its specific capacity can reach 1410.2mah/g to material electrochemical performance, and first charge-discharge efficiency is
76.1%, carried out with 200ma/g current charge-discharge electricity, after 50 circulations, its special capacity fade rate is 3.0%.
Table 1 silicon oxide composite material chemical property
Claims (3)
1. a kind of silicon oxide composite material preparation method, is characterized in that comprising the steps of:
(1) in 800 ~ 1100 DEG C of temperature, under argon gas atmosphere protection, by mean diameter be 1 ~ 20 μm oxidation Asia silica flour heat treatment 1 ~
After 10 hours, cool to room temperature with the furnace；
(2) the oxidation Asia silica flour after step (1) heat treatment is crossed 60 mesh sieves, add the deionization of sub- 2 ~ 15 times of the silica flour quality of oxidation
Water or dehydrated alcohol, grind 0.5 ~ 6 hour, obtain nano pulp；Add aoxidize the organic carbon source of sub- siliceous amount 20 ~ 50% and 0 ~
15% electrical-conductive nanometer material, uses dispersed with stirring 0.5 ~ 3 hour after mix homogeneously, obtains a nanometer mixed slurry；
(3) the nanometer mixed slurry obtaining step (2) is in 200 ~ 350 DEG C of inlet temperature, under the conditions of 90 ~ 150 DEG C of outlet temperature
It is spray-dried, obtain presoma；
(4) presoma obtaining step (3) is under nitrogen or argon atmosphere, 500 ~ 900 DEG C of sintering temperature, the time 2 ~ 12
Hour, it is cooled to room temperature, obtain described silicon oxide composite material.
2. silicon oxide composite material preparation method according to claim 1, is characterized in that described organic carbon source is poly- second
Alkene pyrrolidone, polyaerylic acid, polyethylene glycol oxide or carboxylic styrene butadiene latex.
3. silicon oxide composite material preparation method according to claim 1, is characterized in that described electrical-conductive nanometer material is
Graphene, carbon nano-fiber or CNT.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807870A (en) * | 2018-04-25 | 2018-11-13 | 福建翔丰华新能源材料有限公司 | A kind of preparation method of lithium-ion negative pole high power capacity composite material |
| 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 |
| CN112467102A (en) * | 2020-11-13 | 2021-03-09 | 合肥国轩高科动力能源有限公司 | Preparation method of SiOx-Si @ C @ CNTs composite material |
| CN112670467A (en) * | 2020-11-23 | 2021-04-16 | 深圳石墨烯创新中心有限公司 | Preparation method of silicon oxide/carbon/graphite negative electrode material of lithium ion battery |
| CN112993214A (en) * | 2019-12-18 | 2021-06-18 | 新疆硅基新材料创新中心有限公司 | Method and device for coating SiOx material surface |
| CN113903892A (en) * | 2021-09-13 | 2022-01-07 | 惠州市贝特瑞新材料科技有限公司 | Silicon monoxide composite negative electrode material and preparation method 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 |
| CN114937763A (en) * | 2022-05-19 | 2022-08-23 | 广东省科学院资源利用与稀土开发研究所 | Silicon oxide composite negative electrode material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108807870A (en) * | 2018-04-25 | 2018-11-13 | 福建翔丰华新能源材料有限公司 | A kind of preparation method of lithium-ion negative pole high power capacity composite material |
| CN112993214A (en) * | 2019-12-18 | 2021-06-18 | 新疆硅基新材料创新中心有限公司 | Method and device for coating SiOx material surface |
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| 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 |
| CN112467102A (en) * | 2020-11-13 | 2021-03-09 | 合肥国轩高科动力能源有限公司 | Preparation method of SiOx-Si @ C @ CNTs composite material |
| CN112670467A (en) * | 2020-11-23 | 2021-04-16 | 深圳石墨烯创新中心有限公司 | Preparation method of silicon oxide/carbon/graphite negative electrode material of lithium ion battery |
| CN113903892A (en) * | 2021-09-13 | 2022-01-07 | 惠州市贝特瑞新材料科技有限公司 | Silicon monoxide composite negative electrode material and preparation method 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 |
| CN114937763A (en) * | 2022-05-19 | 2022-08-23 | 广东省科学院资源利用与稀土开发研究所 | Silicon oxide composite negative electrode material and preparation method thereof |
| CN114937763B (en) * | 2022-05-19 | 2024-02-02 | 广东省科学院资源利用与稀土开发研究所 | Silicon oxide composite anode material and preparation method thereof |
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