CN110190250A - A kind of high circulation performance silicon-carbon cathode material and preparation method thereof - Google Patents
A kind of high circulation performance silicon-carbon cathode material and preparation method thereof Download PDFInfo
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- CN110190250A CN110190250A CN201910369748.1A CN201910369748A CN110190250A CN 110190250 A CN110190250 A CN 110190250A CN 201910369748 A CN201910369748 A CN 201910369748A CN 110190250 A CN110190250 A CN 110190250A
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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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- 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
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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
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Abstract
The invention discloses a kind of high circulation performance silicon-carbon cathode materials and preparation method thereof, belong to Material Field, and micron order silicon monoxide powder is passed through ball-milling treatment, it passes sequentially through again and titanium, carbon nanotube and carbon carry out compound rear high-temperature process, then grind thin rear sieving and obtain negative electrode material.The invention has the benefit that the small-size effect after silicon monoxide ball milling, it can be with titanium, carbon nanotube and carbon are preferably compound, can sufficiently offset since volume expansion bring cycle performance sharply declines, improve cycle performance.
Description
Technical field
The invention belongs to Material Fields, specifically, being related to a kind of high circulation performance silicon-carbon cathode material and its preparation side
Method.
Background technique
In recent years, with the extensive use of electric car and fast development, sharply to dynamical system-power battery demand
Increase, the lithium ion battery property excellent with its high capacity, high voltage, high circulation stability, high-energy density, non-environmental-pollution etc.
It can gain great popularity.In order to make lithium ion battery meet electric car development demand, energy density needs lasting promoted.Lithium
Ion battery is common energy storage and conversion equipment in the modern life, and the development of renewable energy and electric car is to next
Increasingly higher demands are proposed for the energy density of lithium ion battery.In order to improve the energy density of lithium ion battery, need
Develop high capacity, the negative electrode material of long-life, the theoretical storage lithium specific capacity of silicon (Si) is 4200mAh/g, it is all being capable of alloy
In the element for changing storage lithium, the specific capacity of silicon is highest.At room temperature, at most combinable 3.75 lithium atoms of each silicon atom,
Li15Si4 alloy phase is obtained, corresponding practical storage lithium specific capacity is up to 3579mAh/g, about graphite theoretical specific capacity
10 times of (372mAh/g) are the most potential novel anode materials for replacing graphite.However, the charge and discharge process of Si is along with huge
Big bulk effect, volume expansion have reached 300% or more, and bulk effect huge in this way can cause strong mechanical stress,
Cause the dusting of material granule and the destruction of electrode interior conductive network, causes to lose between electrode active material and collector
Contact, causes the rapid decaying of electrode reversible capacity, and cycle life shortens.In recent years, a kind of emerging silicon oxygen negative electrode material
SiOx (0 < x < 2) starts for lithium ion battery negative material, and shows advantage: the introducing of oxygen can be in embedding lithium Shi Shengcheng for the first time
Inert component advantageously reduces absolute volume variation of silicon during removal lithium embedded.CN201711183806 provides a kind of oxygen
Change the preparation method of sub- silicon based anode material, but its cycle performance is comparatively poor.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of high circulation performance silicon-carbon cathode material and its preparation side
Method, SiO have carried out ball-milling treatment, particle refinement, the small-size effect after silicon monoxide ball milling, can with titanium, carbon nanotube with
And carbon is preferably compound, can sufficiently offset since volume expansion bring cycle performance sharply declines, improve cycle performance.
The technical scheme is that a kind of high circulation performance silicon-carbon cathode material preparation method, the specific steps are as follows:
Step 1: choosing silicon monoxide powder；
Step 2: the silicon monoxide powder of selection is placed in planetary ball mill ball milling, sieving after ball milling is complete；
Step 3: cladding TiO2；
Step 4: enveloped carbon nanometer tube；
Step 5: carbon coating；
Step 6: being again placed in planetary ball mill ball milling, sieving after ball milling is complete；
Step 7: sintering；
Step 8: grinding forms silicon-carbon cathode material.
Preferably, the silicon monoxide powder particle size chosen in step 1 is at 1-30 microns.
Preferably, in step 2 and step 6, the ball-milling medium of planetary ball mill ball milling is steel ball or zirconium ball.
Preferably, in step 2 and step 6, the rotational speed of ball-mill of planetary ball mill ball milling is 300-500r/min.
Preferably, TiO2 is coated in step 3 to coat using liquid phase method, solution used is methanol, ethyl alcohol, isopropanol, third
The combination of one or more of ketone, espeleton, methylisobutylketone.
Preferably, carbon-coated covering material is pitch, in polystyrene, polyacrylonitrile, phenolic resin in step 5
A combination of one or more.
Preferably, sintering method is divided into two steps in step 7, pre-processes in 150-350 degrees Celsius of air of the first step, second
600-1000 degrees Celsius of step fills protective gas processing.
Preferably, the protective gas is one of helium, neon, argon gas.
Preferably, the silicon-carbon cathode material particle size that formation is ground in step 8 is 0.1-10 microns.
The height that the high circulation performance silicon-carbon cathode material preparation method according to that the present invention also provides a kind of is prepared
Cycle performance silicon-carbon cathode material.
The present invention also provides a kind of electrodes prepared using the high circulation performance silicon-carbon cathode material.
The beneficial effects of the present invention are: providing a kind of high circulation performance silicon-carbon cathode material and preparation method thereof, SiO is carried out
Ball-milling treatment, particle refinement, small-size effect after silicon monoxide ball milling can be with titanium, and carbon nanotube and carbon are compound
Preferably, it can sufficiently offset since volume expansion bring cycle performance sharply declines, improve cycle performance.Existing silicon-carbon
The cycle performance highest of negative electrode material can reach 50-80 times, the silicon-carbon cathode material being prepared using preparation method of the present invention
The cycle performance of material can reach 300 times or more.
Specific embodiment
The present invention is described in detail with reference to embodiments, but the present embodiment cannot be used for the limitation present invention, all
Using similar method and its similar variation of the invention, protection scope of the present invention should all be included in.
Embodiment 1
It takes 30g (3-5 microns of partial size) SiO to be placed in ball grinder, 120g steel ball is added, be filled with argon gas protection, revolving speed 300r/
Min, ball milling 3h take out, and cross 400 mesh screens.
1.8g butyl titanate is added in 30ml dehydrated alcohol, magnetic agitation 1h, and above-mentioned dried material 15g is added, then
After magnetic agitation 3h, dry while stirring, it is stand-by after dry.
3.0g carbon nanotube is dispersed in 30ml deionized water, the material after above-mentioned drying is added, after 3h is sufficiently stirred, side
Stirring side is evaporated, stand-by after dry.
160g steel ball is added in material mixing and ball milling after 2g pitch and above-mentioned drying, is filled with argon gas protection, revolving speed 400r/
Min, ball milling 6h take out, and cross 400 mesh screens.
Material after above-mentioned sieving is placed in tube furnace, 200 degree of pre-oxidation after the completion of pre-oxidation, naturally cool to room
800 degree of Wen Houzai are filled protective gas sintering, are cooled to room temperature after the completion of sintering.
By above-mentioned material ball mill grinding after cooling, 400 mesh screens are crossed, obtain material particles having a size of 1-5 microns.It applies
Cloth assembles battery in glove box, tests battery charging and discharging cycle performance.
Embodiment 2
It takes 40g (3-5 microns of partial size) SiO to be placed in ball grinder, 180g steel ball is added, be filled with argon gas protection, revolving speed 400r/
Min, ball milling 4h take out, and cross 400 mesh screens.
2.7g butyl titanate is added in 40ml dehydrated alcohol, magnetic agitation 1h, and above-mentioned dried material 18g is added, then
After magnetic agitation 4h, dry while stirring, it is stand-by after dry.
3.8g carbon nanotube is dispersed in 45ml deionized water, the material after above-mentioned drying is added, after 3h is sufficiently stirred, side
Stirring side is evaporated, stand-by after dry.
2.6gPAN and the material mixing and ball milling after above-mentioned drying, are added 160g steel ball, are filled with argon gas protection, revolving speed 300r/
Min, ball milling 4h take out, and cross 400 mesh screens.
Material after above-mentioned sieving is placed in tube furnace, 300 degree of pre-oxidation after the completion of pre-oxidation, naturally cool to room
950 degree of Wen Houzai are filled protective gas sintering, are cooled to room temperature after the completion of sintering.
By above-mentioned material ball mill grinding after cooling, 400 mesh screens are crossed, obtain material particles having a size of 2-4 microns.It applies
Cloth assembles battery in glove box, tests battery charging and discharging cycle performance.
Embodiment 3
It takes 42g (3-5 microns of partial size) SiO to be placed in ball grinder, 180g zirconium ball is added, be filled with argon gas protection, revolving speed 350r/
Min, ball milling 4h take out, and cross 400 mesh screens.
3.6g butyl titanate is added in 50ml dehydrated alcohol, magnetic agitation 1h, and above-mentioned dried material 16g is added, then
After magnetic agitation 3h, dry while stirring, it is stand-by after dry.
4.3g carbon nanotube is dispersed in 50ml deionized water, the material after above-mentioned drying is added, after 4h is sufficiently stirred, side
Stirring side is evaporated, stand-by after dry.
Material after 3.1g phenolic resin and above-mentioned drying mixes ball milling, and 220g zirconium ball is added, and is filled with argon gas guarantor
It protects, after revolving speed 400/min, ball milling 6h, it is spare to cross 400 mesh screens.
Material after above-mentioned drying is placed in tube furnace, 350 degree of pre-oxidation after the completion of pre-oxidation, naturally cool to room
900 degree of Wen Houzai are filled protective gas sintering, are cooled to room temperature after the completion of sintering.
By above-mentioned material ball mill grinding after cooling, 400 mesh screens are crossed, obtain material particles having a size of 1.5-3.5 microns.
Battery is assembled in coating in glove box, tests battery charging and discharging cycle performance.
Embodiment 4
It takes 45g (3-5 microns of partial size) SiO to be placed in ball grinder, 200g zirconium ball is added, be filled with argon gas protection, revolving speed 500r/
Min, ball milling 2h take out, and cross 400 mesh screens.
4.6g butyl titanate is added in 60ml dehydrated alcohol, magnetic agitation 2h, and above-mentioned dried material 18g is added, then
After magnetic agitation 3h, dry while stirring, it is stand-by after dry.
4.8g carbon nanotube is dispersed in 65ml deionized water, the material after above-mentioned drying is added, after 5h is sufficiently stirred, side
Stirring side is evaporated, stand-by after dry.
Material after 3.8g polystyrene and above-mentioned drying mixes ball milling, and 260g zirconium ball is added, and is filled with argon gas guarantor
It protects, after revolving speed 500/min, ball milling 8h, it is spare to cross 300 mesh screens.
Material after above-mentioned sieving is placed in tube furnace, 320 degree of pre-oxidation after the completion of pre-oxidation, naturally cool to room
850 degree of Wen Houzai are filled protective gas sintering, are cooled to room temperature after the completion of sintering.
By above-mentioned material ball mill grinding after cooling, 400 mesh screens are crossed, obtain material particles having a size of 1.0-3.0 microns.
Battery is assembled in coating in glove box, tests battery charging and discharging cycle performance.
Carry out charge and discharge cycles test to the button cell: charge and discharge are 0.01-1.5V by voltage, and charging and discharging currents are equal
0.2C, the specific data of first charge-discharge are shown in Table 1, and table 1 is lithium ion battery negative material prepared by the embodiment of the present invention 1~4
Electrochemical data.
Table 1
SiO of the present invention has carried out ball-milling treatment, particle refinement, the small-size effect after silicon monoxide ball milling, can with titanium,
Carbon nanotube and carbon are preferably compound, can sufficiently offset since volume expansion bring cycle performance sharply declines, improve
Cycle performance.The cycle performance highest of existing silicon-carbon cathode material can reach 50-80 times, using preparation method of the present invention
The cycle performance for the silicon-carbon cathode material being prepared can reach 300 times or more.
This hair can be understood and applied the above description of the embodiments is intended to facilitate those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to case study on implementation, and described herein one
As principle be applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to implementation cases here
Example, those skilled in the art's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be
Within protection scope of the present invention.
Claims (10)
1. a kind of high circulation performance silicon-carbon cathode material preparation method, it is characterised in that: specific step is as follows:
Step 1: choosing silicon monoxide powder；
Step 2: the silicon monoxide powder of selection is placed in planetary ball mill ball milling, sieving after ball milling is complete；
Step 3: cladding TiO2；
Step 4: enveloped carbon nanometer tube；
Step 5: carbon coating；
Step 6: being again placed in planetary ball mill ball milling, sieving after ball milling is complete；
Step 7: sintering；
Step 8: grinding forms silicon-carbon cathode material.
2. a kind of high circulation performance silicon-carbon cathode material preparation method according to claim 1, it is characterised in that: step 1
The silicon monoxide powder particle size of middle selection is at 1-30 microns.
3. a kind of high circulation performance silicon-carbon cathode material preparation method according to claim 1, it is characterised in that: step 2
In step 6, the ball-milling medium of planetary ball mill ball milling is steel ball or zirconium ball.
4. a kind of high circulation performance silicon-carbon cathode material preparation method according to claim 1, it is characterised in that: step 2
In step 6, the rotational speed of ball-mill of planetary ball mill ball milling is 300-500r/min.
5. a kind of high circulation performance silicon-carbon cathode material preparation method according to claim 1, it is characterised in that: step 3
Middle cladding TiO2 is coated using liquid phase method, and solution used is methanol, ethyl alcohol, isopropanol, acetone, espeleton, methylisobutylketone
One or more of combination.
6. a kind of high circulation performance silicon-carbon cathode material preparation method according to claim 1, it is characterised in that: step 5
In carbon-coated covering material be one or more of pitch, polystyrene, polyacrylonitrile, phenolic resin combination.
7. a kind of high circulation performance silicon-carbon cathode material preparation method according to claim 1, it is characterised in that: step 7
Middle sintering method is divided into two steps, pre-processes in 150-350 degrees Celsius of air of the first step, and 600-1000 degrees Celsius of second step is filled protection
Gas treatment.
8. a kind of high circulation performance silicon-carbon cathode material preparation method according to claim 7, it is characterised in that: the guarantor
Shield gas is one of helium, neon, argon gas.
9. a kind of height that -8 any high circulation performance silicon-carbon cathode material preparation methods are prepared according to claim 1
Cycle performance silicon-carbon cathode material.
10. a kind of electrode prepared using high circulation performance silicon-carbon cathode material as claimed in claim 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110828794A (en) * | 2019-10-28 | 2020-02-21 | 珠海格力绿色再生资源有限公司 | Preparation method of multiple modified silicon-manganese alloy composite negative electrode material |
| CN114267830A (en) * | 2021-12-13 | 2022-04-01 | 荆门亿纬创能锂电池有限公司 | Method for preparing antimony-loaded silicon-carbon composite negative electrode material by using peanut shells, composite negative electrode material and lithium ion battery |
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| CN102306759A (en) * | 2011-09-16 | 2012-01-04 | 奇瑞汽车股份有限公司 | Silicon monoxide composite cathode material for lithium ion battery, and preparation method thereof |
| CN107623113A (en) * | 2017-09-08 | 2018-01-23 | 赣州市瑞富特科技有限公司 | A kind of porous long circulating silicon-carbon cathode material preparation method |
| WO2018093998A1 (en) * | 2016-11-17 | 2018-05-24 | Worcester Polytechnic Institute | Kinetic batteries |
| CN108183200A (en) * | 2017-11-23 | 2018-06-19 | 上海颐行高分子材料有限公司 | A kind of preparation method of the sub- silicon based anode material of oxidation for lithium ion battery |
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2019
- 2019-05-06 CN CN201910369748.1A patent/CN110190250A/en active Pending
Patent Citations (4)
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| CN102306759A (en) * | 2011-09-16 | 2012-01-04 | 奇瑞汽车股份有限公司 | Silicon monoxide composite cathode material for lithium ion battery, and preparation method thereof |
| WO2018093998A1 (en) * | 2016-11-17 | 2018-05-24 | Worcester Polytechnic Institute | Kinetic batteries |
| CN107623113A (en) * | 2017-09-08 | 2018-01-23 | 赣州市瑞富特科技有限公司 | A kind of porous long circulating silicon-carbon cathode material preparation method |
| CN108183200A (en) * | 2017-11-23 | 2018-06-19 | 上海颐行高分子材料有限公司 | A kind of preparation method of the sub- silicon based anode material of oxidation for lithium ion battery |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110828794A (en) * | 2019-10-28 | 2020-02-21 | 珠海格力绿色再生资源有限公司 | Preparation method of multiple modified silicon-manganese alloy composite negative electrode material |
| CN114267830A (en) * | 2021-12-13 | 2022-04-01 | 荆门亿纬创能锂电池有限公司 | Method for preparing antimony-loaded silicon-carbon composite negative electrode material by using peanut shells, composite negative electrode material and lithium ion battery |
| CN114267830B (en) * | 2021-12-13 | 2024-06-11 | 荆门亿纬创能锂电池有限公司 | Method for preparing antimony-loaded silicon-carbon composite negative electrode material by adopting peanut shell, composite negative electrode material and lithium ion battery |
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Application publication date: 20190830 |