CN103236517A - Lithium ion battery silicon-based negative material and preparation method thereof - Google Patents
Lithium ion battery silicon-based negative material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a lithium ion battery silicon-based negative material and a preparation method thereof, which belong to the technical field of lithium ion battery negative materials. The lithium ion battery silicon-based negative material is prepared from silicon monoxide; the macroscopic particle diameter of the negative material is 10-25 micrometers; according to a microstructure, the negative material is composed of nanometer silicon particles covered with silica; the internal silicon particle diameter of the negative material is 20-30 nanometers; and at 0.1C discharge rate, the first discharge capacity of the negative material reaches 2010-2640 mAh/g, and is 420-790 mAh/g after 50 cycles. The negative materials with the structure characteristic combines the dispersion and the reduction of silicon particles; and on one hand, the silicon particles can be dispersed by a pore channel structure of silica so as to provide a space for the expansion of silicon in charge and discharge processes, on the other hand, the particle diameter of silicon can be reduced, and therefore, a volume effect of silicon in the charge and discharge processes can be weakened.
Description
Technical field
The present invention relates to a kind of lithium ion battery cathode material and its preparation method, more particularly, the present invention relates to silica-based negative material of a kind of lithium ion battery and preparation method thereof, belong to the lithium ion battery negative material technical field.
Background technology
Along with petering out and problems such as global warming that it brings of fossil fuel, the new forms of energy industry is subjected to numerous researchers gradually and pays close attention to.Lithium ion battery has advantages such as high-energy-density, low self-discharge rate and green environmental protection, thereby is widely used as in the battery of digital product and electric automobile, is the research focus of new energy field.
Graphite is the lithium ion battery negative material of extensive use, it has good cycle, advantages such as wide material sources, but its theoretical capacity lower (372mAh/g), further limited the raising of lithium ion battery energy density, also allowed the negative material of seeking high-energy-density density become numerous researchers' common recognition.
Silicon is done negative pole and is had very high theoretical capacity (4200 mAh/g), be the ideal material that substitutes graphite electrode, but because its volumetric expansion that exists in charge and discharge process causes capacity attenuation, cyclicity is relatively poor.How overcoming the volumetric expansion problem of silicon materials, improve its cyclical stability, is the emphasis of silicon materials research.The main mode of the modification of silicon materials has that silicon grain is dispersed in porous material neutralization and other materials is compound etc.
It is CN101740747A that State Intellectual Property Office discloses a publication number in 2010.6.16, name is called the patent of invention of " a kind of silicium cathode and the lithium ion battery that contains this silicium cathode ", this patent provides a kind of silicium cathode material, comprise collector and the silicium cathode material that loads on this collector, the silicium cathode material comprises silicium cathode active material and adhesive.Effect by adhesive, improve the microstructure of silica-base material system, increase the porosity between the silica-base material, big pore structure is conducive to battery and partially absorbs the volumetric expansion that removal lithium embedded produces in the charge and discharge cycles process, improves the cyclicity of lithium ion battery.But limited in one's ability because of adhesive pore-creating, only depend on the binding agent effect can not well improve the performance of silicon materials.
It is CN101850959A that State Intellectual Property Office discloses a publication number in 2010.10. 6; name is called the patent of invention of " a kind of preparation method of lithium ion battery silicon-carbon cathode material "; this patent provides a kind of preparation method of lithium ion battery silicon-carbon cathode material; at first phenol monomer and aldehyde monomer being put into solvent is hydrolyzed; synthetic high specific area porous presoma; put into nano silica fume again; utilize hyperacoustic special cavitation concussion effect; nano silica fume is dispersed in the synthetic high specific area porous presoma uniformly; the presoma of final synthesizing high specific surface area porous polymer resin-coating silicon; make bulk effect weaken greatly; then with gained presoma drying; and under protective atmosphere and under the specific temperature, carry out roasting, finally obtain silicon-carbon cathode material.The silicon-carbon recombination energy is improved the cycle performance of silicon materials preferably, but also exists the processing step complexity, is difficult for shortcomings such as popularization.
It is CN101740747B that State Intellectual Property Office discloses a publication number in 2012.6. 13, name is called the patent of invention of " a kind of preparation method of silicon nanoparticle and contain negative material and the lithium ion battery of this silicon nanoparticle ", this patent provides a kind of preparation method of silicon nanoparticle and contains the preparation method of negative material and the lithium ion battery of this silicon nanoparticle, it comprises that the high temperature disproportionated reaction of silicon monoxide and corrosion remove two steps of silicon dioxide, under protective atmosphere, silicon monoxide is heated, generate the silicon dioxide coated nano silicon grain; The silicon dioxide coated nano silicon grain mixed with corrosive liquid carries out corrosion treatment, with silicon dioxide etching fall again through separate silicon nanoparticle.The subject matter that this technology exists is, on the one hand, owing to use severe toxicity and the strong hydrofluoric acid of corrosivity, do not meet the principle of environmental protection, is unfavorable for that industrialization promotion uses; It is unsatisfactory to erode behind the silicon dioxide cyclical stability of material on the other hand.
Summary of the invention
The present invention is intended to solve in the existing lithium ion battery silicon negative material charge and discharge process because the very big capacity attenuation that causes of change in volume problem rapidly, provides that a kind of specific capacity is big, the silica-based negative material of lithium ion battery of stable circulation.
Another object of the present invention is for providing above-mentioned lithium ion battery silica-based negative material preferred manufacturing procedure, and this preparation method's process route is simple, production cost is low.
In order to realize the foregoing invention purpose, its concrete technical scheme is as follows:
The silica-based negative material of a kind of lithium ion battery, it is characterized in that: the silica-based negative material of described lithium ion battery is made by silicon monoxide, the macroscopic particles particle diameter is 10-25 μ m, and microstructure is the silicon nanoparticle of coated with silica, and inner silicon grain particle diameter is 20-30nm.
Above-mentioned negative material is under the 0.1C multiplying power, and discharge capacity reaches 2010-2640mAh/g first, is 420-790mAh/g through 50 circulation backs.
Preferably, the preparation method of the silica-based negative material of a kind of lithium ion battery is characterized in that: comprise following processing step:
A, take by weighing the silicon monoxide particle that particle diameter is 2-30mm, place heating furnace, under Buchholz protection, be warming up to 800-1300 ℃ with the heating rate of 1-50 ℃/min, roasting 1-10h obtains solid;
B, the solid that steps A is obtained are put into ball grinder, add abrading-ball;
C, elder generation vacuumize ball grinder, charge into gas then;
D, ball grinder is placed ball mill, obtain powder behind the ball milling;
E, the powder that step D is obtained sieve, and namely obtain the silica-based negative material of lithium ion battery of the present invention.
Preferably, the present invention is in steps A, and described heating furnace is tube furnace, box type furnace or rotary furnace.
Preferably, the present invention is in steps A and step C, and described gas is nitrogen, helium, argon gas, perhaps the gaseous mixture of argon gas and hydrogen.
Further, when described gas was the gaseous mixture of argon gas and hydrogen, the volume of described hydrogen was the 5-10% of gaseous mixture.
Preferably, the present invention is in step B, and the mass ratio of abrading-ball and solid is 10:1-15:1.
Preferably, the present invention is in step C, and described vacuumizing refers to be evacuated to vacuum degree and be not less than 0.08MPa.
Preferably, the present invention is in step C, and the described gas that charges into need be replaced 3-5 time repeatedly.
Preferably, the present invention is in step D, and the rotating speed of described ball mill is 300-800rpm.
Preferably, the present invention is in step D, and the described ball milling time is 6-12h.
Preferably, the present invention is in step e, and described sieving referred to that fineness was the sieve of 26-30 μ m.
The useful technique effect that the present invention brings:
1, the silica-based negative material of lithium ion battery of the present invention is the silicon nanoparticle of coated with silica, and integral particle is of a size of 10-25 μ m, and inner silicon grain is of a size of 20-30nm.This architectural feature is with the dispersion of silicon nanoparticle and dwindle and unite two into one, and can utilize the pore passage structure of silicon dioxide to come the dispersing nanometer silicon grain on the one hand, for the expansion of silicon in the charge and discharge process provides the space; Can dwindle the particle diameter of silicon on the other hand, thereby weaken the bulk effect of silicon in the charge and discharge process;
2, the lithium ion battery silicon negative material prepared of the present invention, it is big to have specific capacity, repeatable high, advantages such as good stability, under the 0.1C multiplying power, this material capacity first reaches 2010-2640mAh/g, be stabilized in 420-790 mAh/g through 50 circulation volumes, have good stable;
3, the silica-based negative material of lithium ion battery of the present invention adopts the silicon monoxide preparation, and silicon monoxide is a kind of silicon materials that application potential is arranged very much, and it has unique pore structure, and the mixture that disproportionated reaction generates silicon and silicon dioxide can take place at a certain temperature.Silicon grain is less in mixture, has weakened the bulk effect in the charge and discharge process, and the pore structure of silicon monoxide itself also makes its more stable and unlikely efflorescence in charge and discharge process cave in simultaneously.The present invention utilizes the property of silicon monoxide to prepare the silicon-based anode material, has the simple environmental protection of process route, repeatable high, advantages such as specific capacity is big, good cycling stability;
4, the preparation method of the silica-based negative material of lithium ion battery of the present invention compares with traditional nano silicon material synthetic method, technology and equipment that the present invention adopts are very simple, only just can make the silicon materials of required Nano grade by high-temperature roasting and ball milling, production cost is low, is easy to industrialization promotion;
5, the present invention is preferred, gas among steps A and the step C is chosen as the gaseous mixture of argon gas and hydrogen, because the silicon grain particle diameter behind the ball milling is little, active higher, may be by little air oxidation residual in the jar, utilize the reducing power of hydrogen, adopt the hydrogen-argon-mixed oxidation that can prevent silicon grain, further the hydrogen ratio of Xuan Zeing uses safer; Preferred vacuum degree is not less than 0.08MPa, and easy to operate, cost is low, and the conventional vacuum pump can be realized; Preferably, charging into gas need replace 3-5 time repeatedly, can fully get rid of the air in the ball grinder, guarantees that atmosphere is pure; Preferably, the rotating speed of ball mill is 300-800rpm, and rotating speed has maximum effect of impact and good abrasive action in this scope the time; Preferably, the ball milling time is 6-12h, and this ball milling is in the time, and material is fully pulverized, and reaches optimal effectiveness.
Description of drawings
Fig. 1 is the silicon grain schematic diagram of lithium battery silicon-based anode material coated with silica of the present invention;
First charge-discharge curve when Fig. 2 uses for lithium battery silicon-based anode material of the present invention.
Embodiment
Embodiment 1
The silica-based negative material of a kind of lithium ion battery is characterized in that: the silica-based negative material of described lithium ion battery is made by silicon monoxide, and the macroscopic particles particle diameter is 10 μ m, and microstructure is the silicon nanoparticle of coated with silica, and inner silicon grain particle diameter is 20nm.
Above-mentioned negative material is under the 0.1C multiplying power, and discharge capacity reaches 2010mAh/g first, is 420mAh/g through 50 circulation backs.
Embodiment 2
The silica-based negative material of a kind of lithium ion battery is characterized in that: the silica-based negative material of described lithium ion battery is made by silicon monoxide, and the macroscopic particles particle diameter is 25 μ m, and microstructure is the silicon nanoparticle of coated with silica, and inner silicon grain particle diameter is 30nm.
Above-mentioned negative material is under the 0.1C multiplying power, and discharge capacity reaches 2640mAh/g first, is 790mAh/g through 50 circulation backs.
Embodiment 3
The silica-based negative material of a kind of lithium ion battery is characterized in that: the silica-based negative material of described lithium ion battery is made by silicon monoxide, and the macroscopic particles particle diameter is 18 μ m, and microstructure is the silicon nanoparticle of coated with silica, and inner silicon grain particle diameter is 25nm.
Above-mentioned negative material is under the 0.1C multiplying power, and discharge capacity reaches 2325mAh/g first, is 605mAh/g through 50 circulation backs.
Embodiment 4
The silica-based negative material of a kind of lithium ion battery is characterized in that: the silica-based negative material of described lithium ion battery is made by silicon monoxide, and the macroscopic particles particle diameter is 21 μ m, and microstructure is the silicon nanoparticle of coated with silica, and inner silicon grain particle diameter is 22nm.
Above-mentioned negative material is under the 0.1C multiplying power, and discharge capacity reaches 2500mAh/g first, is 700mAh/g through 50 circulation backs.
Embodiment 5
The optimization preparation method of the silica-based negative material of a kind of lithium ion battery of the present invention:
A, take by weighing the silicon monoxide particle that particle diameter is 2mm, place heating furnace, under Buchholz protection, be warming up to 800 ℃ with the heating rate of 1 ℃/min, roasting 1h obtains solid;
B, the solid that steps A is obtained are put into ball grinder, add abrading-ball;
C, elder generation vacuumize ball grinder, charge into gas then;
D, ball grinder is placed ball mill, obtain powder behind the ball milling;
E, the powder that step D is obtained sieve, and namely obtain the silica-based negative material of lithium ion battery of the present invention.
Embodiment 6
The optimization preparation method of the silica-based negative material of a kind of lithium ion battery of the present invention:
A, take by weighing the silicon monoxide particle that particle diameter is 30mm, place heating furnace, under Buchholz protection, be warming up to 1300 ℃ with the heating rate of 50 ℃/min, roasting 10h obtains solid;
B, the solid that steps A is obtained are put into ball grinder, add abrading-ball;
C, elder generation vacuumize ball grinder, charge into gas then;
D, ball grinder is placed ball mill, obtain powder behind the ball milling;
E, the powder that step D is obtained sieve, and namely obtain the silica-based negative material of lithium ion battery of the present invention.
Embodiment 7
The optimization preparation method of the silica-based negative material of a kind of lithium ion battery of the present invention:
A, take by weighing the silicon monoxide particle that particle diameter is 16mm, place heating furnace, under Buchholz protection, be warming up to 1050 ℃ with the heating rate of 26 ℃/min, roasting 5.5h obtains solid;
B, the solid that steps A is obtained are put into ball grinder, add abrading-ball;
C, elder generation vacuumize ball grinder, charge into gas then;
D, ball grinder is placed ball mill, obtain powder behind the ball milling;
E, the powder that step D is obtained sieve, and namely obtain the silica-based negative material of lithium ion battery of the present invention.
Embodiment 8
The optimization preparation method of the silica-based negative material of a kind of lithium ion battery of the present invention:
A, take by weighing the silicon monoxide particle that particle diameter is 5mm, place heating furnace, under Buchholz protection, be warming up to 1000 ℃ with the heating rate of 40 ℃/min, roasting 8h obtains solid;
B, the solid that steps A is obtained are put into ball grinder, add abrading-ball;
C, elder generation vacuumize ball grinder, charge into gas then;
D, ball grinder is placed ball mill, obtain powder behind the ball milling;
E, the powder that step D is obtained sieve, and namely obtain the silica-based negative material of lithium ion battery of the present invention.
Embodiment 9
On the basis of embodiment 5-8, preferred:
In steps A and step C, described gas is nitrogen, helium, argon gas, perhaps the gaseous mixture of argon gas and hydrogen.
When described gas was the gaseous mixture of argon gas and hydrogen, the volume of described hydrogen was the 5-10% of gaseous mixture.
In step B, the mass ratio of abrading-ball and solid is 10:1.
In step C, described vacuumizing refers to be evacuated to vacuum degree and is not less than 0.08MPa.
In step C, the described gas that charges into need be replaced 3 times repeatedly.
In step D, the rotating speed of described ball mill is 300rpm.
In step D, the described ball milling time is 6h.
In step e, described sieving referred to that fineness was the sieve of 26 μ m.
Embodiment 10
On the basis of embodiment 5-8, preferred:
In steps A and step C, described gas is nitrogen, helium, argon gas, perhaps the gaseous mixture of argon gas and hydrogen.
When described gas was the gaseous mixture of argon gas and hydrogen, the volume of described hydrogen was the 5-10% of gaseous mixture.
In step B, the mass ratio of abrading-ball and solid is 15:1.
In step C, described vacuumizing refers to be evacuated to vacuum degree and is not less than 0.08MPa.
In step C, the described gas that charges into need be replaced 5 times repeatedly.
In step D, the rotating speed of described ball mill is 800rpm.
In step D, the described ball milling time is 12h.
In step e, described sieving referred to that fineness was the sieve of 30 μ m.
Embodiment 11
On the basis of embodiment 5-8, preferred:
In steps A and step C, described gas is nitrogen, helium, argon gas, perhaps the gaseous mixture of argon gas and hydrogen.
When described gas was the gaseous mixture of argon gas and hydrogen, the volume of described hydrogen was the 5-10% of gaseous mixture.
In step B, the mass ratio of abrading-ball and solid is 12.5:1.
In step C, described vacuumizing refers to be evacuated to vacuum degree and is not less than 0.08MPa.
In step C, the described gas that charges into need be replaced 4 times repeatedly.
In step D, the rotating speed of described ball mill is 550rpm.
In step D, the described ball milling time is 9h.
In step e, described sieving referred to that fineness was the sieve of 28 μ m.
Embodiment 12
On the basis of embodiment 5-8, preferred:
In steps A and step C, described gas is nitrogen, helium, argon gas, perhaps the gaseous mixture of argon gas and hydrogen.
When described gas was the gaseous mixture of argon gas and hydrogen, the volume of described hydrogen was the 5-10% of gaseous mixture.
In step B, the mass ratio of abrading-ball and solid is 14:1.
In step C, described vacuumizing refers to be evacuated to vacuum degree and is not less than 0.08MPa.
In step C, the described gas that charges into need be replaced 4 times repeatedly.
In step D, the rotating speed of described ball mill is 500rpm.
In step D, the described ball milling time is 11h.
In step e, described sieving referred to that fineness was the sieve of 27 μ m.
Claims (10)
1. silica-based negative material of lithium ion battery, it is characterized in that: the silica-based negative material of described lithium ion battery is made by silicon monoxide, the macroscopic particles particle diameter is 10-25 μ m, and microstructure is the silicon nanoparticle of coated with silica, and inner silicon grain particle diameter is 20-30nm.
2. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 1 is characterized in that: comprise following processing step:
A, take by weighing the silicon monoxide particle that particle diameter is 2-30mm, place heating furnace, under Buchholz protection, be warming up to 800-1300 ℃ with the heating rate of 1-50 ℃/min, roasting 1-10h obtains solid;
B, the solid that steps A is obtained are put into ball grinder, add abrading-ball;
C, elder generation vacuumize ball grinder, charge into gas then;
D, ball grinder is placed ball mill, obtain powder behind the ball milling;
E, the powder that step D is obtained sieve, and namely obtain the silica-based negative material of lithium ion battery of the present invention.
3. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 2, it is characterized in that: in steps A and step C, described gas is nitrogen, helium, argon gas, perhaps the gaseous mixture of argon gas and hydrogen.
4. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 4, it is characterized in that: when described gas was the gaseous mixture of argon gas and hydrogen, the volume of described hydrogen was the 5-10% of gaseous mixture.
5. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 2, it is characterized in that: in step B, the mass ratio of abrading-ball and solid is 10:1-15:1.
6. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 2 is characterized in that: in step C, described vacuumizing refers to be evacuated to vacuum degree and is not less than 0.08MPa.
7. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 2, it is characterized in that: in step C, the described gas that charges into need be replaced 3-5 time repeatedly.
8. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 2, it is characterized in that: in step D, the rotating speed of described ball mill is 300-800rpm.
9. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 2, it is characterized in that: in step D, the described ball milling time is 6-12h.
10. the preparation method of the silica-based negative material of a kind of lithium ion battery according to claim 2, it is characterized in that: in step e, described sieving referred to that fineness was the sieve of 26-30 μ m.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103626187A (en) * | 2013-12-03 | 2014-03-12 | 山东玉皇化工有限公司 | High specific capacity porous silica compound preparation method |
| CN105826560A (en) * | 2016-06-02 | 2016-08-03 | 中国科学院半导体研究所 | A kind of preparation method of SiOx-based lithium ion battery composite negative electrode material |
| CN108376781A (en) * | 2018-04-17 | 2018-08-07 | 天津巴莫科技股份有限公司 | A kind of lithium-ion-power cell silicon-carbon cathode material and preparation method thereof |
| CN109046618A (en) * | 2018-08-13 | 2018-12-21 | 昆明海创兴科技有限公司 | The method that one-step method prepares lithium ion battery negative material nano-silicon powder |
| CN109524626A (en) * | 2017-09-18 | 2019-03-26 | 浙江工业大学 | A kind of Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method thereof |
| CN109585802A (en) * | 2018-10-16 | 2019-04-05 | 湖南宸宇富基新能源科技有限公司 | A kind of high compacted density lithium ion battery silicon-carbon cathode material and preparation method thereof |
| CN110191861A (en) * | 2017-01-11 | 2019-08-30 | 捷恩智株式会社 | Polysilsesquioxane-coated silicon nanoparticle or sintered body thereof, production method thereof, negative electrode active material for lithium ion battery, negative electrode for lithium ion battery, and lithium ion battery |
| CN110660989A (en) * | 2019-09-27 | 2020-01-07 | 东北大学 | Silicon-based Si-B-C negative electrode material prepared from calcium carbide co-reduction silicon oxide and boron-containing oxide and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626187A (en) * | 2013-12-03 | 2014-03-12 | 山东玉皇化工有限公司 | High specific capacity porous silica compound preparation method |
| CN103626187B (en) * | 2013-12-03 | 2016-03-30 | 山东玉皇盛世化工股份有限公司 | A kind of preparation method of height ratio capacity porous silicon oxide compound |
| CN105826560A (en) * | 2016-06-02 | 2016-08-03 | 中国科学院半导体研究所 | A kind of preparation method of SiOx-based lithium ion battery composite negative electrode material |
| CN110191861A (en) * | 2017-01-11 | 2019-08-30 | 捷恩智株式会社 | Polysilsesquioxane-coated silicon nanoparticle or sintered body thereof, production method thereof, negative electrode active material for lithium ion battery, negative electrode for lithium ion battery, and lithium ion battery |
| CN109524626A (en) * | 2017-09-18 | 2019-03-26 | 浙江工业大学 | A kind of Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method thereof |
| CN108376781A (en) * | 2018-04-17 | 2018-08-07 | 天津巴莫科技股份有限公司 | A kind of lithium-ion-power cell silicon-carbon cathode material and preparation method thereof |
| CN109046618A (en) * | 2018-08-13 | 2018-12-21 | 昆明海创兴科技有限公司 | The method that one-step method prepares lithium ion battery negative material nano-silicon powder |
| CN109585802A (en) * | 2018-10-16 | 2019-04-05 | 湖南宸宇富基新能源科技有限公司 | A kind of high compacted density lithium ion battery silicon-carbon cathode material and preparation method thereof |
| CN110660989A (en) * | 2019-09-27 | 2020-01-07 | 东北大学 | Silicon-based Si-B-C negative electrode material prepared from calcium carbide co-reduction silicon oxide and boron-containing oxide and preparation method and application thereof |
| CN110660989B (en) * | 2019-09-27 | 2020-09-22 | 东北大学 | Silicon-based Si-B-C negative electrode material prepared from calcium carbide co-reduction silicon oxide and boron-containing oxide and preparation method and application thereof |
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Application publication date: 20130807 |