CN109817952A - A kind of negative electrode of lithium ion battery and preparation method thereof - Google Patents
A kind of negative electrode of lithium ion battery and preparation method thereof Download PDFInfo
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- CN109817952A CN109817952A CN201910212332.9A CN201910212332A CN109817952A CN 109817952 A CN109817952 A CN 109817952A CN 201910212332 A CN201910212332 A CN 201910212332A CN 109817952 A CN109817952 A CN 109817952A
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Abstract
The invention discloses a kind of negative electrode of lithium ion battery and preparation method thereof, including silicon and frame material, the silicon is distributed in frame material with nano-scale, and the frame material is formed by by carbon nanotube or carbon black or charcoal-aero gel or the combination between them.The present invention is big for existing silicium cathode volume expansion, the low problem of conductivity, it devises and frame is combined by carbon nanotube or carbon black or charcoal-aero gel or the group between them, silicon particle is uniformly distributed in frame with nano-scale contains silicon composite cathode, this design improves material reactivity and shortens lithium ion diffusion path, the frame material of introducing has reserved the space for receiving silicon materials expansion, electronics and ionic conductance between material granule are improved simultaneously, and the reversible capacity and good cycling stability having containing silicon composite cathode material higher than 800mAh/g synthesized by the method for the invention, the method is simple and efficient, suitable for large-scale production.
Description
Technical field
The present invention relates to cell manufacturing techniques field, specially a kind of negative electrode of lithium ion battery and preparation method thereof.
Background technique
Electric car has gradually entered into people's lives in recent years, but following " mileage anxiety " also increasingly perplexs
People, the reason is that automobile-used lithium ion battery energy density need to be improved, and height ratio capacity negative electrode material is opened
Hair is to improve one aspect critically important in battery energy density.
The actual specific capacity of graphite cathode material is difficult again very close to its theoretical specific capacity (372mAh/g) at present
There is promotion.In all potential negative electrode of lithium ion battery, silicon is most potential negative electrode material.With graphite-phase ratio, silicon has super
Height ratio capacity (its theoretical specific capacity is about 4200mAh/g when forming Li4.4Si), potential inexpensive (Si element in the earth's crust
The second) and preferable safety (intercalation potential 0.4V vs.Li/Li+, be not likely to produce Li dendrite) content occupy.
But silicon volume expansion during removal lithium embedded is huge and self-conductance rate (2.52 × 10-4S cm) is lower, actually answers
Problems are brought to battery in.(1) coulombic efficiency is low for the first time, since volume expansion is huge in Si lithium intercalation
(up to 420%), Si particle and the separation of collector, graphite still unavoidably occur after compound with graphite leads to part lithium ion
It can not deviate from, actual coulombic efficiency for the first time is far below graphite；Compared with Si cathode, the volume expansion of SiO cathode has substantially
Improve but still be much higher than graphite, nonactive product Li2O and Li4SiO4 can be worse generated during its embedding lithium, manages
The coulombic efficiency for the first time of opinion is less than 70%.(2) pole piece thickness change is big, uniformity is poor.Silicium cathode volume change is greatly easily negative
The inside of pole pole piece generates stress and concentrates, and gently then generates local deformation weight during stress release and then pierce through diaphragm, then band
Carry out a series of safety problems.(3) cyclical stability is poor, and early period, decaying was especially significant.On the one hand particle expansion will lead to part
Particle shape can not receive electronics at " isolated island " to be chemically reacted, and the generation that another party will lead to new interface consumes free Li and generates
SEI.In addition, the low conductance of silicon materials itself adds the solid electrolyte membrane (SEI) thickened, inside battery polarization is caused to highlight, together
When anode take off lithium amount and increase oxidisability and become strong, also there is unstability therewith in electrolyte.Variety of problems eventually leads to battery collapse.
In summary situation, it is necessory to provide a kind of based on silicon, high capacity, low bulk and stable circulation answer
Close negative electrode material and its high efficiency preparation method.
Summary of the invention
The purpose of the present invention is to provide a kind of negative electrode of lithium ion battery and preparation method thereof, to solve above-mentioned background technique
The existing silicium cathode volume expansion of middle proposition is big, the low problem of conductivity.
To achieve the above object, the invention provides the following technical scheme: a kind of cathode material of lithium ion battery, including silicon
And frame material, the silicon are distributed in frame material with nano-scale, the frame material be by carbon nanotube or carbon black or
Charcoal-aero gel or the combination between them are formed by, and average primary particle diameter < 500nm of the silicon, the carbon nanotube is averaged
Diameter is 7-11nm, and average length is 5-20 μm, and the average primary particle diameter of the carbon black is 15-70nm, and DBP absorption value is 180-
350ml/100g, the porosity 80-98% of the charcoal-aero gel, typical pore size < 50nm, network colloidal particle diameter 3-
20nm, specific surface area 600-1100m2/g。
The preparation method of above-mentioned cathode material of lithium ion battery, comprising the following steps:
Step 1: frame material is mixed with micron silicon particle, by frame material (carbon nanotube or carbon black or charcoal-aero gel
Or the combination between them) be mixed in a certain ratio with silicon particle, 15- is mixed at revolving speed 10-20 turns/min in dry powder form
60min, is then added decentralized medium appropriate, decentralized medium be water, alcohol, N-Methyl pyrrolidone one kind or they between
Combination, stirring 10-20 turn/min, and dispersion 1500-2000 turns/min mixing 15-60min, then turns/min, dispersion to stir 30-40
3500-4500 turns/min mixing 3-8h.
Step 2, micron silicon particle nanosizing, after the mixture in step 1 is dried under vacuum or protective atmosphere
Temperature is heated to higher than 1410 DEG C, keep the temperature 0.5-5h and applies 5-30 turns/min of stirring；Then under vacuum or protective atmosphere with
Mixture is cooled to room temperature by certain cooling velocity, and protective atmosphere is nitrogen or argon gas.
The obtained mixture of step 2 is carried out mechanical ball mill, that is, needed for obtaining by step 3, nodularization containing silicon composite cathode
Partial size contains silicon composite cathode.
Preferably, which is fabricated to pole piece and lithium piece is assembled into button cell, at 25 DEG C,
0.1C charge and discharge between 0-2.5V use.
Preferably, cathode material of lithium ion battery is fabricated to pole piece and Li (Ni1/3Co1/3Mn1/3)O2Made anode
Piece is assembled into full battery, and at 25 DEG C, 1/3C charge and discharge between 2.4-3.9V are used.
Compared with prior art, the beneficial effects of the present invention are: improving material reaction by by silicon materials nanosizing and living
Property, lithium ion diffusion path is shortened, by introducing the combination institute shape by carbon nanotube or carbon black or charcoal-aero gel or between them
At frame material, the space for receiving silicon materials expansion has been reserved, to reduce the expansion of battery cathode, by utilizing frame
Material itself has good electron conduction, is conducive to the deficiency for making up silicon materials own electronic poorly conductive, passes through utilization
The characteristic of frame material high-specific surface area can adsorb more electrolyte, help to improve the ion-conductance between composite material granular
It leads, and this method high production efficiency, can be mass produced.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in the embodiment of the present invention
Technical solution is clearly and completely described, it is clear that and described embodiments are only a part of the embodiments of the present invention, without
It is whole embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not before making creative work
Every other embodiment obtained is put, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of cathode material of lithium ion battery, including silicon and frame material, silicon are distributed in frame material with nano-scale
In, frame material is formed by by carbon nanotube or carbon black or charcoal-aero gel or the combination between them, the average primary grain of silicon
Diameter is 400nm, and the average diameter of carbon nanotube is 7nm, and average length is 5 μm, and the average primary particle diameter of carbon black is 15nm, DBP
Absorption value is 180ml/100g, the porosity 80% of charcoal-aero gel, typical pore size 40nm, network colloidal particle diameter 3nm,
Specific surface area 600m2/g。
The preparation method of above-mentioned cathode material of lithium ion battery, comprising the following steps:
Step 1: frame material is mixed with micron silicon particle, and carbon nanotube (CNT), Li435 and silicon particle are pressed quality
It is mixed than 2:1:1, mixes 30min (15 revs/min of stirring) in dry powder form, 1.5 times of solid gross mass of N- methyl is then added
Pyrrolidones (NMP) disperses 1800 revs/min of mixing 30min to stir 15 revs/min, then with 35 revs/min of stirring, disperse 400 turns/
Divide mixing 4h.
Step 2, micron silicon particle nanosizing will be heated under an argon atmosphere after the mixture drying in step 1
It 1500 DEG C of temperature, keeps the temperature 4h and applies stirring (15 revs/min)；Then mixture is cooled to the furnace room temperature under an argon atmosphere.
The obtained mixture of step 2 is carried out mechanical ball mill 4h, obtains D50 by step 3, nodularization containing silicon composite cathode
For 10 μm containing silicon composite cathode.
The negative electrode material is fabricated to pole piece and lithium piece is assembled into button cell, 25 DEG C, 0.1C charge and discharge between 0-2.5V,
Reversible capacity is 1025mAh/g, which is fabricated to pole piece and Li (Ni1/3Co1/3Mn1/3)O2Made positive plate
It is assembled into full battery, 25 DEG C, 1/3C charge and discharge between 2.4-3.9V, the capacity retention ratio after 10 circle of circulation, 100 circles, 300 are enclosed divides
It Wei 98.6%, 93.4%, 89.5%.
Embodiment 2
A kind of cathode material of lithium ion battery, including silicon and frame material, silicon are distributed in frame material with nano-scale
In, frame material is formed by by carbon nanotube or carbon black or charcoal-aero gel or the combination between them, the average primary grain of silicon
Diameter 450nm, the average diameter of carbon nanotube are 9nm, and average length is 10 μm, and the average primary particle diameter of carbon black is 35nm, and DBP inhales
Receipts value be 260ml/100g, the porosity 90% of charcoal-aero gel, typical pore size 45nm, network colloidal particle diameter 14nm,
Specific surface area 800m2/g。
The preparation method of above-mentioned cathode material of lithium ion battery, includes the following steps:
Step 1, frame material are mixed with micron silicon particle, and CNT, charcoal-aero gel and silicon particle 1:1:1 in mass ratio are mixed
Close, mix in dry powder form 30min (stirring 15 revs/min), 1.5 times of solid gross mass of NMP is then added with stir 15 turns/
Point, disperse 1800 revs/min of mixing 30min, then with 35 revs/min of stirring, disperse 400 revs/min of mixing 4h.
Step 2, micron silicon particle nanosizing, by the mixture in step 1 it is dry after heat treated under argon is extremely again
It 1600 DEG C of temperature, keeps the temperature 3h and applies stirring (15 revs/min)；Then under an argon atmosphere by mixture with the speed of 200 DEG C/h
It is cooled to room temperature.
The obtained mixture of step 2 is carried out mechanical ball mill 7h, obtains D50 by step 3, nodularization containing silicon composite cathode
For 7 μm containing silicon composite cathode.
The negative electrode material is fabricated to pole piece and lithium piece is assembled into button cell, 25 DEG C, 0.1C charge and discharge between 0-2.5V,
Reversible capacity is 1465mAh/g, which is fabricated to pole piece and Li (Ni1/3Co1/3Mn1/3)O2Made positive plate
It is assembled into full battery, 25 DEG C, 1/3C charge and discharge between 2.4-3.9V, the capacity retention ratio after 10 circle of circulation, 100 circles, 300 are enclosed divides
It Wei 97.4%, 92.1%, 88.7%.
Embodiment 3
A kind of cathode material of lithium ion battery, including silicon and frame material, silicon are distributed in frame material with nano-scale
In, frame material is formed by by carbon nanotube or carbon black or charcoal-aero gel or the combination between them, the average primary grain of silicon
Diameter 490nm, the average diameter of carbon nanotube are 11nm, and average length is 20 μm, and the average primary particle diameter of carbon black is 70nm, DBP
Absorption value is 350ml/100g, the porosity 98% of charcoal-aero gel, typical pore size 49nm, network colloidal particle diameter
20nm, specific surface area 1100m2/g
The preparation method of above-mentioned lithium ion battery negative material, includes the following steps:
Step 1, frame material are mixed with micron silicon particle, Li435, charcoal-aero gel and silicon particle 1:1:1 in mass ratio
Mixing mixes 30min (15 revs/min of stirring) in dry powder form, 1.5 times of solid gross mass of alcohol is added then to stir 15
Rev/min, disperse 1800 revs/min of mixing 30min, then with 35 revs/min of stirring, disperse 400 revs/min of mixing 4h.
Step 2, micron silicon particle nanosizing, by the mixture in step 1 it is dry after heat treated under argon is extremely again
It 1650 DEG C of temperature, keeps the temperature 2.5h and applies stirring (15 revs/min)；Then under an argon atmosphere by mixture with the speed of 300 DEG C/h
Degree is cooled to room temperature.
The obtained mixture of step 2 is carried out mechanical ball mill 3h, obtains D50 by step 3, nodularization containing silicon composite cathode
For 12 μm containing silicon composite cathode.
The negative electrode material is fabricated to pole piece and lithium piece is assembled into button cell, 25 DEG C, 0.1C charge and discharge between 0-2.5V,
Reversible capacity is 1374mAh/g, which is fabricated to pole piece and Li (Ni1/3Co1/3Mn1/3)O2Made positive plate
It is assembled into full battery, 25 DEG C, 1/3C charge and discharge between 2.4-3.9V, the capacity retention ratio after 10 circle of circulation, 100 circles, 300 are enclosed divides
It Wei 97.7%, 92.8%, 89.0%.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
Claims (6)
1. a kind of cathode material of lithium ion battery, it is characterised in that: including silicon and frame material, the silicon is with nano-scale point
It is distributed in frame material, the frame material is formed by carbon nanotube or carbon black or charcoal-aero gel or the combination between them
, average primary particle diameter < 500nm of the silicon, the average diameter of the carbon nanotube is 7-11nm, and average length is 5-20 μ
M, the average primary particle diameter of the carbon black are 15-70nm, and DBP absorption value is 180-350ml/100g, the hole of the charcoal-aero gel
Gap rate 80-98%, typical pore size < 50nm, network colloidal particle diameter 3-20nm, specific surface area 600-1100m2/g。
2. a kind of preparation method of cathode material of lithium ion battery described in claim 1, which is characterized in that including following step
It is rapid:
Step 1: frame material is mixed with micron silicon particle, by frame material (carbon nanotube or carbon black or charcoal-aero gel or it
Between combination) be mixed in a certain ratio with silicon particle, in dry powder form revolving speed 10-20 turn/min under mix 15-60min,
Then it is added decentralized medium appropriate, decentralized medium is water, alcohol, one kind of N-Methyl pyrrolidone or the combination between them,
It stirs 10-20 and turns/min, dispersion 1500-2000 turns/min mixing 15-60min, then turns/min to stir 30-40, disperses 3500-
4500 turns/min mixing 3-8h.
Step 2, micron silicon particle nanosizing will heat under vacuum or protective atmosphere after the mixture drying in step 1
It is higher than 1410 DEG C to temperature, keep the temperature 0.5-5h and applies 5-30 turns/min of stirring；Then with certain under vacuum or protective atmosphere
Cooling velocity mixture is cooled to room temperature, protective atmosphere be nitrogen or argon gas.
The obtained mixture of step 2 is carried out mechanical ball mill, that is, partial size needed for obtaining by step 3, nodularization containing silicon composite cathode
Contain silicon composite cathode.
3. application of a kind of cathode material of lithium ion battery in terms of button cell according to claim 1.
4. a kind of application of cathode material of lithium ion battery according to claim 3, which is characterized in that the lithium-ion electric
Pond is fabricated to pole piece with negative electrode material and lithium piece is assembled into button cell, and at 25 DEG C, 0.1C charge and discharge between 0-2.5V are used.
5. application of a kind of cathode material of lithium ion battery in terms of full battery according to claim 1.
6. a kind of application of cathode material of lithium ion battery according to claim 5, which is characterized in that the lithium-ion electric
Pond is fabricated to pole piece and Li (Ni with negative electrode material1/3Co1/3Mn1/3)O2Made positive plate is assembled into full battery, at 25 DEG C
Under, 1/3C charge and discharge between 2.4-3.9V use.
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| CN111540896A (en) * | 2020-05-07 | 2020-08-14 | 七台河万锂泰电材有限公司 | Preparation method of silicon-carbon composite negative electrode material |
| CN112072093A (en) * | 2020-09-18 | 2020-12-11 | 天科新能源有限责任公司 | Lithium battery negative electrode slurry with good dispersion effect and preparation method thereof |
| CN113644246A (en) * | 2021-08-15 | 2021-11-12 | 江西理工大学 | Self-breaking silicon electrode based on continuous electric contact network and preparation method thereof |
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