CN108923023A - A kind of preparation method of lithium ion battery yolk structure Si-C composite material - Google Patents
A kind of preparation method of lithium ion battery yolk structure Si-C composite material Download PDFInfo
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- CN108923023A CN108923023A CN201810566698.1A CN201810566698A CN108923023A CN 108923023 A CN108923023 A CN 108923023A CN 201810566698 A CN201810566698 A CN 201810566698A CN 108923023 A CN108923023 A CN 108923023A
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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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- 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
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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
- 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
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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 kind of lithium ion battery preparation methods of yolk structure Si-C composite material, its step is to coat silicon nano by the hydrolysate of tetraethyl orthosilicate (TEOS), obtain predecessor, then polyvinylpyrrolidone (PVP) is coated to predecessor using spray drying process, the composite material with the carbon coating silicon of porous pomegranate shape structure is then obtained by the etching of carbonization and HF, wherein there is cavity between nano silicon particles and shell.The structure can alleviate Volumetric expansion of silicon nano during removal lithium embedded, synthesis technology is simple, at low cost, product purity is high, high production efficiency, easy to industrialized production, resulting Si-C composite material specific capacity with higher, good cyclical stability and excellent high rate performance.
Description
Technical field
The invention belongs to field of lithium ion battery material, and in particular to a kind of yolk structure lithium ion battery silicon-carbon cathode material
The preparation method of material.
Background technique
Silicon has that reversible capacity is high (4200mAh/g) as lithium ion battery negative material, highly-safe, to environment without
The advantages that pollution, it is considered to be the ideal chose of lithium ion battery negative material.But its poorly conductive, in charge and discharge process
Volume expansion is big (> 300%), and electrode material is caused dusting short circuit phenomenon occur, it is caused to be used as lithium ion battery negative material
When cyclical stability it is poor, it is difficult to be commercialized practical application.There are two types of the main methods for improving silicium cathode material disadvantages described above at present
Approach：First is that silicon is compound with conductive material, for example the electric conductivity of silicon materials can be improved by introducing carbon material.Second is that passing through
By silicon materials nanosizing, alleviate the volume expansion in silicon materials charge and discharge process.The preparation method of traditional Si-C composite material
There are high-energy ball milling, solid organic carbon cracking, electrochemical deposition etc..However the material that these methods obtain still is deposited in a practical situation
Poor in problems, such as silicon-carbon composite effect, structure is simpler, and production technology is more complex, usually simple clad structure
The space of silicon volume expansion is not buffered, specific surface area is lower, causes electrolyte and electrode material contacts area lower, such knot
Electric conductivity is deteriorated during structure can not effectively solve the problems, such as silicon volume expansion, and these problems lead to traditional Si-C composite material
Cycle life it is short, high rate performance is bad, and specific capacity is lower, constrains the extensive use of Si-C composite material.
Summary of the invention
To overcome the problems, such as disadvantages described above, the present invention is using silicon nano as core particle, tetraethyl orthosilicate
(TEOS) products therefrom as template sacrifice agent constructs space after hydrolysis oxidation, and polyvinylpyrrolidone (PVP) is used as carbon source, benefit
A kind of porous pomegranate shape structure is devised with spray drying process, microcosmic to be made of yolk structure Si-C composite material, wherein silicon is received
There is cavity between rice corpuscles and porous carbon shell, is used as lithium ion battery negative material.The space that the structure provides can be effective
The volume expansion of silicon is buffered, while effectively increasing electrode/electrolyte contact surface, promotes ion and electron-transport, this method synthesis
Simple process, it is at low cost, have the advantages that high production efficiency, be easy to industrialized production.
Realization of the invention mainly includes the following steps that：
1), that a certain amount of silicon nano is molten by the mixing of ultrasonic disperse to dehydrated alcohol and water (volume ratio 4: 1)
In liquid, a certain amount of concentrated ammonia liquor and TEOS stirring is added, using the hydrolysate of TEOS under alkaline condition to silicon nano
It is effectively coated, then three times, drying obtains solid powder for washing centrifugation.
2) solid powder for, taking a certain amount of step 1 to obtain is placed in distilled water and stirs, and PVP stirring is then added,
It is spray-dried under the conditions of 180 DEG C, the product after collecting spray drying obtains solid powder.
3), the solid powder for obtaining step 2 leads to inert gas in tube furnace, keeps the temperature and carries out under the conditions of certain temperature
Heat treatment, obtains solid powder.
4), step 3 obtained solid powder is dissolved in HF solution, the SiO as template layer is washed off by the etching of HF2,
Ethyl alcohol is washed dries afterwards three times, obtains the Si-C composite material with porous pomegranate shape, wherein silicon nano and outer layer carbon shell
Between have cavity.
Wherein, ultrasonic disperse, ultrasonic power 300W, jitter time 30min, drying are sufficiently mixed described in step 1)
Temperature is 80 DEG C, time 12h, and the mass ratio of silicon nano and TEOS are 1: 0.1-1: 1.
The mass ratio of solid powder described in step 2) and PVP are 1: 2~1: 1.
Inert gas described in step 3) can be one of nitrogen, argon gas, helium or a variety of.
Certain temperature described in step 3) refers to 500~1200 DEG C, soaking time 1-4h.
HF solution concentration described in step 4) is 5wt.%-30wt.%.
Compared with prior art, the beneficial effects of the invention are as follows use a kind of convenient and fast spray drying process to obtain with more
The Si-C composite material of the pomegranate shape structure in hole, porous structure are conducive to the infiltration of electrolyte, the transmission of lithium ion and electronics, silicon
Cavity between nanoparticle and carbon-coating can effectively buffer the volume expansion of silicon in charge and discharge process, and material can be improved in the presence of carbon
Electric conductivity, silicon provide high capacity.Therefore, the design of this composite structure can obtain higher capacity, excellent multiplying power
Performance and good cyclical stability.
Detailed description of the invention
The scanning electron microscopic picture of Fig. 1 Si-C composite material.
The transmission electron microscope picture of Fig. 2 Si-C composite material.
The X-ray diffractogram of Fig. 3 Si-C composite material.
The half-cell cycle performance comparison diagram of Fig. 4 Si-C composite material.
Embodiment
Comparative example：Take 400mg nano silica fume to be scattered in 800mL deionized water, be added the PVP of 800mg, stir after 4h in
It is spray-dried at 180 DEG C.It collects powder and leads to argon gas heat preservation two hours under the conditions of 900 DEG C in tube furnace.
Embodiment one：It takes 600mg nano silicon particles in the mixed solution of 320mL dehydrated alcohol and 80mL distilled water, surpasses
Washing centrifugation is dried three times after 2.5mL concentrated ammonia liquor and 1mL TEOS stirring 12h are added after sound dispersion 30min.Take the above-mentioned baking of 400mg
The PVP of 800mg is added in 800mL deionized water in powder after dry, is spray-dried at 180 DEG C after stirring 4h.Collect powder
End leads to argon gas under the conditions of 900 DEG C in tube furnace and keeps the temperature two hours.It collects sample and washes off SiO with 5%HF2, it is then centrifuged for second
Vacuum drying oven dries to obtain composite material after alcohol is washed three times.By the composite material, acetylene black, PVDF according to 8: 1: 1 grinding and with
Slurry is made as solvent in N-Methyl pyrrolidone (NMP), is uniformly applied on copper foil.Then copper foil vacuum is transferred to do
Under the conditions of 110 DEG C of dry case it is dry for 24 hours, after with slicer be cut into the piece that diameter is 1cm, piece is transferred to glove box and carries out lithium battery
Assembling.From top to bottom assembling sequence successively be CR2016 anode cover, pole piece, diaphragm, lithium battery electrolytes, nickel foam and
CR2016 negative electrode casing.It in voltage range is 0~2V by the blue electrical measurement test system of battery, under conditions of current density is 100mAh/g
It is tested, obtained battery performance is as shown in Fig. 4.
Embodiment two：It takes 600mg nano silicon particles in the mixed solution of 320mL dehydrated alcohol and 80mL distilled water, surpasses
Washing centrifugation is dried three times after 2.5mL concentrated ammonia liquor and 1mL TEOS stirring 12h are added after sound dispersion 30min.Take the above-mentioned baking of 800mg
The PVP of 800mg is added in 800mL deionized water in powder after dry, is spray-dried at 180 DEG C after stirring 4h.Collect powder
End leads to nitrogen under the conditions of 500 DEG C in tube furnace and keeps the temperature two hours.It collects sample and washes off SiO with 5%HF2Template layer, then
Centrifugation alcohol washes three dries to obtain composite material inferior to vacuum drying oven.The Integration Assembly And Checkout condition of battery is same as Example 1.
Embodiment three：It takes 600mg nano silicon particles in the mixed solution of 320mL dehydrated alcohol and 80mL distilled water, surpasses
Washing centrifugation is dried three times after 2.5mL concentrated ammonia liquor and 1mL TEOS stirring 12h are added after sound dispersion 30min.Take the above-mentioned baking of 800mg
The PVP of 800mg is added in 800mL deionized water in powder after dry, is spray-dried at 180 DEG C after stirring 4h.Collect powder
End leads to nitrogen under the conditions of 1200 DEG C in tube furnace and keeps the temperature two hours.It collects sample and washes off SiO with 5%HF2Template layer, then
Centrifugation alcohol washes three dries to obtain composite material inferior to vacuum drying oven.The Integration Assembly And Checkout condition of battery is same as Example 1.
Example IV：It takes 600mg nano silicon particles in the mixed solution of 320mL dehydrated alcohol and 80mL distilled water, surpasses
Washing centrifugation is dried three times after 2.5mL concentrated ammonia liquor and 1mL TEOS stirring 12h are added after sound dispersion 30min.Take the above-mentioned baking of 800mg
The PVP of 800mg is added in 800mL deionized water in powder after dry, is spray-dried at 180 DEG C after stirring 4h.Collect powder
End leads to nitrogen under the conditions of 700 DEG C in tube furnace and keeps the temperature two hours.It collects sample and washes off SiO with 30%HF2Template layer, then
Centrifugation alcohol washes three dries to obtain composite material inferior to vacuum drying oven.The Integration Assembly And Checkout condition of battery is same as Example 1.
Embodiment five：It takes 600mg nano silicon particles in the mixed solution of 320mL dehydrated alcohol and 80mL distilled water, surpasses
Washing centrifugation is dried three times after 2.5mL concentrated ammonia liquor and 1mL TEOS stirring 12h are added after sound dispersion 30min.Take the above-mentioned baking of 800mg
Powder is added the PVP of 800mg, is done at 180 DEG C after stirring 4h and say capable spray drying in 800mL deionized water after dry.Collect powder
Helium injection gas keeps the temperature two hours under the conditions of 700 DEG C in tube furnace at end.It collects sample and washes off SiO with 30%HF2Template layer, then
Centrifugation alcohol washes three dries to obtain composite material inferior to vacuum drying oven.The Integration Assembly And Checkout condition of battery is same as Example 1.
1 it can be seen that yolk structure preparation of silicon carbon composite materials proposed by the present invention with comparative example through the foregoing embodiment
Method greatly improves the specific capacity and cyclical stability of Si-C composite material.
Claims (6)
1. a kind of lithium ion battery preparation method of yolk structure Si-C composite material, includes the following steps：
1) a certain amount of silicon nano, is passed through into ultrasonic disperse into the mixed solution of dehydrated alcohol and water (volume ratio 4: 1),
A certain amount of concentrated ammonia liquor and tetraethyl orthosilicate (TEOS) stirring is added, using the hydrolysate of TEOS under alkaline condition to silicon
Nanoparticle is effectively coated, and then three times, drying obtains solid powder for washing centrifugation；
2) solid powder for, taking a certain amount of step 1 to obtain is placed in distilled water and stirs, and polyvinylpyrrolidone is then added
(PVP) it stirs, is spray-dried under the conditions of 180 DEG C, the product after collecting spray drying obtains solid powder；
3), the solid powder for obtaining step 2 leads to inert gas in tube furnace, is heat-treated under certain temperature, obtains solid powder
End；
4), step 3 obtained solid powder is dissolved in HF solution, the SiO as template layer is washed off by the etching of HF2, ethyl alcohol washes
It dries afterwards three times, obtains the Si-C composite material with porous pomegranate shape.
2. a kind of preparation method of lithium ion battery yolk structure Si-C composite material according to claim 1, special
Sign is：The ultrasonic disperse, ultrasonic power 300W, jitter time 30min, drying temperature are 80 DEG C, and the time is
The mass ratio of 12h, silicon nano and TEOS are 1: 0.1-1: 1.
3. a kind of preparation method of lithium ion battery yolk structure Si-C composite material according to claim 1, special
Sign is：The mass ratio of obtained solid powder and polyvinylpyrrolidone is 1: 2~1: 1 in step 1).
4. a kind of preparation method of lithium ion battery yolk structure Si-C composite material according to claim 1, special
Sign is：The inert gas can be one of nitrogen, argon gas, helium or a variety of.
5. a kind of preparation method of lithium ion battery yolk structure Si-C composite material according to claim 1, special
Sign is：The heat treatment temperature that is carbonized is 500-1200 DEG C, time 1-4h.
6. a kind of preparation method of lithium ion battery yolk structure Si-C composite material according to claim 1, special
Sign is：The HF solution concentration is 5wt.%-30wt.%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109671935A (en) * | 2018-12-20 | 2019-04-23 | 江苏大学 | A kind of preparation method and its usage of silica/biology carbon composite |
| CN109888228A (en) * | 2019-02-28 | 2019-06-14 | 蜂巢能源科技有限公司 | Negative electrode material of lithium ion battery and preparation method thereof |
| CN109980194A (en) * | 2019-02-27 | 2019-07-05 | 福建翔丰华新能源材料有限公司 | A kind of preparation method of lithium ion battery silicon-carbon cathode material |
| CN110085842A (en) * | 2019-05-10 | 2019-08-02 | 山西大学 | A kind of silicon-carbon composite cathode material and preparation method thereof |
| CN110148743A (en) * | 2019-07-05 | 2019-08-20 | 珠海冠宇电池有限公司 | A kind of silicon-carbon composite cathode material and preparation method thereof and lithium ion battery |
| CN113206236A (en) * | 2021-05-06 | 2021-08-03 | 合肥国轩高科动力能源有限公司 | Preparation method of NCM ternary positive electrode material with Yolk-shell structure and prepared material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109671935A (en) * | 2018-12-20 | 2019-04-23 | 江苏大学 | A kind of preparation method and its usage of silica/biology carbon composite |
| CN109671935B (en) * | 2018-12-20 | 2021-09-10 | 江苏大学 | Preparation method and application of silicon dioxide/biochar composite material |
| CN109980194A (en) * | 2019-02-27 | 2019-07-05 | 福建翔丰华新能源材料有限公司 | A kind of preparation method of lithium ion battery silicon-carbon cathode material |
| CN109888228A (en) * | 2019-02-28 | 2019-06-14 | 蜂巢能源科技有限公司 | Negative electrode material of lithium ion battery and preparation method thereof |
| CN110085842A (en) * | 2019-05-10 | 2019-08-02 | 山西大学 | A kind of silicon-carbon composite cathode material and preparation method thereof |
| CN110148743A (en) * | 2019-07-05 | 2019-08-20 | 珠海冠宇电池有限公司 | A kind of silicon-carbon composite cathode material and preparation method thereof and lithium ion battery |
| CN113206236A (en) * | 2021-05-06 | 2021-08-03 | 合肥国轩高科动力能源有限公司 | Preparation method of NCM ternary positive electrode material with Yolk-shell structure and prepared material |
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