CN105938906B - A kind of lithium ion battery artificial composite cathode material of silicon/carbon/graphite and preparation method thereof - Google Patents
A kind of lithium ion battery artificial composite cathode material of silicon/carbon/graphite and preparation method thereof Download PDFInfo
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- CN105938906B CN105938906B CN201610434287.8A CN201610434287A CN105938906B CN 105938906 B CN105938906 B CN 105938906B CN 201610434287 A CN201610434287 A CN 201610434287A CN 105938906 B CN105938906 B CN 105938906B
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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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- 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
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Abstract
The present invention provides a kind of lithium ion battery artificial composite cathode material of silicon/carbon/graphite and preparation method thereof, the material is the second particle compound of pure artificial graphite, it is using needle coke as raw material, using pitch as binder, through broken, classification, spheroidization, ion beam bombardment, mixing, high temperature is compound, classification, graphitization, sieves, except the techniques such as magnetic are made.The compacted density of the composite negative pole material of the method for the present invention preparation is up to 1.80g/cc, and reversible capacity is higher than 355mAh/g, and first charge discharge efficiency about 94% recycles 200 weeks electrode expansions and is lower than 8%.The present invention is conventional powder processing or carbon technique, Yi Shixian industrialization using technique.
Description
Technical field
The present invention relates to negative electrode material of a kind of lithium ion battery and preparation method thereof, in particular to a kind of lithium-ion electric
Pond cathode high capacity, high-pressure solid, low circulation rebound artificial graphite composite material and preparation method.
Background technique
With the functionalization of electronic equipment, intelligent continuous renewal, people are to the power supply of electronic equipment it is also proposed that higher
It is required that.High capacity, high-pressure solid, long circulation life are the development trends of current IT Li-like ions battery.
However, the negative electrode material of high capacity, high-pressure solid, generally will appear biggish swelling in cyclic process, follows
Electrode expansion is generally more than 10% after ring 200 weeks, and battery cycle life is caused to decline, and is difficult to break through 800 weeks.Therefore, how to reduce
The circulation of negative electrode material expands, and is a most critical issue for guaranteeing IT Li-like ions battery cycle life.
In order to solve the circulation expansion issues of high capacity, high-pressure solid negative electrode material, it is compound that we use second particle
Mode reserves some spaces by changing the average crystalline orientation value of graphite particle, and between particle and particle to buffer
Electrochemical expansion prepares high capacity, high-pressure solid, low circulation rebound artificial graphite composite material.
Summary of the invention
The present invention is intended to provide the artificial graphite of a kind of lithium ion battery high capacity, high-pressure solid, low circulation rebound is compound
Material and preparation method thereof.Wherein, D50=14-21 μm of artificial graphite composite material, tap density 1.0-1.2g/cc, than
Surface area is 0.5-1.6m2/g；Reversible specific capacity is 355-363mAh/g；Practical compacted density 1.8g/cc, room temperature 1C circulation
2000 weeks capacity retention ratios are higher than 80%, and electrode expansion is lower than 8% after 200 weeks circulations.
Composite material of the present invention, sharpest edges are: on the good basis of guaranteed capacity compaction capacity, room
Warm 1C recycles 2000 weeks capacity retention ratios and is higher than 80%, and electrode expansion is lower than 8% after 200 weeks circulations.
The present invention passes through the compound realization of following second particle: the following steps are included:
A kind of preparation method of the artificial composite cathode material of silicon/carbon/graphite of lithium ion battery, which is characterized in that it includes following
Step:
S1. commercially available needle coke is subjected to broken classification；
S2. the needle coke particles after above-mentioned broken classification are subjected to spheroidization processing, obtain primary particle；
S3. the primary particle that S2 is walked is uniformly mixed with pitch, under the conditions of protective atmosphere, it is multiple carries out high temperature
Conjunction processing, gained compound are classified to remove bulky grain；
S4. the S3 compound walked is put into graphitizing furnace and carries out graphitization processing；
S5. the compound Jing Guo graphitization processing is sieved, except magnetic, packaging.
Further, the needle coke in the S1 step, range includes petroleum needle green coke, the needle-shaped green coke of coal measures, petroleum
Needle-shaped calcined coke and the needle-shaped calcined coke of coal measures, the volatile matter range of needle coke are 0.1-10%.
As a preferred solution of the present invention, in the S3 step, the S2 primary particle walked is banged with ion beam
It hits, obtains the composite precursor that surface is cheated with micropore or irregular dimple, be then uniformly mixed composite precursor with pitch,
Under the conditions of protective atmosphere, high temperature combined processing is carried out, gained compound is classified to remove bulky grain.
Further, in the S3 step, the primary particle that S2 is walked first is heated under the conditions of protective atmosphere
It 1600-2000 DEG C, is then bombarded with the ion beam that energy is 600-800eV, beam current density is 0.1-0.3mA/cm2, from
The distance of beamlet to primary particle is 1-10mm, and bombardment angle is 30-150 °, and bombardment while, which is stirred primary particle, to be turned over
Dynamic, bombardment time 5-30min obtains the composite precursor that surface is cheated with micropore or irregular dimple.
Further, the asphalt softening point in S3 step is 150-280 DEG C, it is experience airflow milling treated powder
Material, D50 are 3-5 μm；The ratio of needle coke and pitch is 100:10-20.
Further, it is the artificial graphite composite negative pole material of preparation method production according to claim 1 to 3.
Further, D50=14-21 μm of the artificial graphite composite negative pole material, tap density 1.0-1.2g/cc,
Specific surface area is 0.5-1.6m2/g；Reversible specific capacity is 355-363mAh/g；Practical compacted density 1.8g/cc, room temperature 1C circulation
2000 weeks capacity retention ratios are higher than 80%, and electrode expansion is lower than 8% after 200 weeks circulations.
Compared with prior art, the present invention is had the advantage that
1. the primary particle that S2 is walked first is heated to 1600-2000 DEG C by the present invention under the conditions of protective atmosphere, so
It is bombarded afterwards with the ion beam that energy is 600-800eV, beam current density is 0.1-0.3mA/cm2, ion beam to primary particle
Distance be 1-10mm, bombardment angle is 30-150 °, and bombardment while, which is stirred primary particle, to be stirred, and bombardment time is
5-30min obtains the composite precursor that surface is cheated with micropore or irregular dimple, then again mixes composite precursor and pitch
It closes uniformly, under the conditions of protective atmosphere, carries out high temperature combined processing.By this secondary granulation technology, the crystalline substance of material is improved
To index, a large amount of micropore or irregular dimple hole are formed between particle surface, particle, this can not only enhance composite precursor
Binding force between pitch is allowed into the entirety of a firm connection, during charge and discharge cycles, composite precursor and drip
Blueness is not easy loose and disintegrates, and can effectively improve the service life of negative electrode material and entire battery, and facilitates reduction electrode and exist
Expansion in electrochemistry cyclic process provides and receives each other with space between particle and particle, improves circulating battery number
15%-30%。
2. spheroidization processing helps to improve the pattern of primary particle, and the pole piece compacting for providing composite material in turn is close
Degree, in addition, spheroidization can also enhance the binding force of active material and collector, enhance the electrode machining performance of composite material.
3. entire technical process is easily achieved industrialization.
Specific embodiment
Embodiment 1
Lithium ion battery high capacity, high-pressure solid, low circulation rebound artificial graphite composite material, the specific steps are as follows:
S1. the petroleum needle green coke that commercially available volatilization is divided into 7% be crushed and be classified to D50=7 μm；
S2. spheroidization processing is carried out using petroleum needle green coke of the balling machine to broken classification, balling machine revolving speed is
2600rpm, time 3min；
S3. it is in mass ratio with D50 is 3 μm, softening point is 150 DEG C pitch by primary particle that S2 is walked
100:10 is uniformly mixed, and under the conditions of protective atmosphere, 500 DEG C of high temperature combined processings, gained compound is classified big to remove
Particle；
S4. the S3 compound walked is put into acheson furnace and carries out graphitization processing, graphitization temperature
It is 2800 DEG C；
S5. the compound Jing Guo graphitization processing is sieved, except magnetic, packaging.
Embodiment 2
Lithium ion battery high capacity, high-pressure solid, low circulation rebound artificial graphite composite material, the specific steps are as follows:
S1. coke after the forging of commercially available petroleum needle be crushed and be classified to D50=10 μm；
S2. the petroleum needle green coke progress spheroidization processing using balling machine to broken classification, revolving speed 3000rpm, when
Between 5min；
S3. the primary particle that S2 is walked first is heated under the conditions of protective atmosphere 1600 DEG C, is then with energy
600-800eV, the ion beam that beam current density is 0.1mA/cm2 are bombarded, and the distance of ion beam to primary particle is 1mm, Hong
Hitting angle is 30 °, and bombardment while, which is stirred primary particle, to be stirred, bombardment time 5min, obtains surface with micropore
Or the composite precursor in irregular dimple hole；Then by the composite precursor and D50 is 3 μm, softening point is 220 DEG C pitch
It is uniformly mixed in mass ratio for 100:15, under the conditions of protective atmosphere, 600 DEG C of high temperature combined processings, gained compound is divided
Grade is to remove bulky grain；
S4. be graphitized: acheson furnace, graphitization temperature are 3000 DEG C；
S5. it sieves, except magnetic, packaging.
Embodiment 3
Lithium ion battery high capacity, high-pressure solid, low circulation rebound artificial graphite composite material, the specific steps are as follows:
S1. coke after the needle-shaped forging of commercially available coal measures be crushed and be classified to D50=13 μm；
S2. spheroidization is handled: revolving speed 3600rpm, time 10min；
S3. the primary particle that S2 is walked first is heated under the conditions of protective atmosphere 2000 DEG C, is then with energy
600-800eV, the ion beam that beam current density is 0.3mA/cm2 are bombarded, and the distance of ion beam to primary particle is 10mm,
Bombarding angle is 150 °, and bombardment while, which is stirred primary particle, to be stirred, and bombardment time 30min, obtaining surface has
Micropore or the composite precursor in irregular dimple hole；Then by the composite precursor and 5 μm, the pitch that softening point is 280 DEG C
It is uniformly mixed in mass ratio for 100:20, under the conditions of protective atmosphere, 700 DEG C of high temperature combined processings, gained compound is divided
Grade is to remove bulky grain；
S4. be graphitized: acheson furnace, graphitization temperature are 3200 DEG C；
S5. it sieves, except magnetic, packaging.
Embodiment 4
Lithium ion battery high capacity, high-pressure solid, low circulation rebound artificial graphite composite material, the specific steps are as follows:
S1. the needle-shaped green coke of coal measures of commercially available volatile matter 5% be crushed and be classified to D50=10 μm；
S2. spheroidization is handled: revolving speed 3000rpm, time 10min；
It S3. is in mass ratio 100:12 by the S2. primary particle walked and 4 μm, the pitch that softening point is 250 DEG C
It is uniformly mixed, under the conditions of protective atmosphere, 600 DEG C of high temperature combined processings, gained compound is classified to remove bulky grain；
S4. be graphitized: acheson furnace, graphitization temperature are 3200 DEG C；
S5. it sieves, except magnetic, packaging.
Comparative example
Oil system needle coke is crushed and is classified to D50=14 μm, the graphitization processing at 3000 DEG C, products therefrom is comparative sample.
The comparison from table is it is found that product of the present invention is shown on the basis of guaranteeing that specific capacity * compacted density is increased
The circulation expansion for reducing pole piece is write, and effectively extends the cycle life of battery.
Claims (5)
1. a kind of lithium ion battery preparation method of artificial composite cathode material of silicon/carbon/graphite, comprising the following steps:
S1. commercially available needle coke is subjected to broken classification；
S2. the needle coke particles after above-mentioned broken classification are subjected to spheroidization processing, obtain primary particle；
S3. the primary particle that S2 is walked is uniformly mixed with pitch, under the conditions of protective atmosphere, carries out the compound place of high temperature
Reason, gained compound are classified to remove bulky grain；
S4. the S3 compound walked is put into graphitizing furnace and carries out graphitization processing；
S5. the compound Jing Guo graphitization processing is sieved, except magnetic, packaging；
Needle coke in the S1 step, range includes petroleum needle green coke, the needle-shaped green coke of coal measures, petroleum needle calcined coke and coal
It is needle-shaped calcined coke, the volatile matter range of needle coke is 0.1-10%；
It is characterized by: the primary particle that S2 is walked is bombarded with ion beam, obtaining surface has in the S3 step
Composite precursor, is then uniformly mixed, in protective atmosphere condition by micropore or the composite precursor in irregular dimple hole with pitch
Under, high temperature combined processing is carried out, gained compound is classified to remove bulky grain.
2. a kind of preparation method of the lithium ion battery as described in claim 1 with artificial composite cathode material of silicon/carbon/graphite, feature
It is: in the S3 step, the primary particle that S2 is walked first is heated to 1600-2000 DEG C under the conditions of protective atmosphere, so
It is afterwards 600-800eV with energy, beam current density 0.1-0.3mA/cm2Ion beam bombarded, ion beam to primary particle
Distance be 1-10mm, bombardment angle is 30-150 °, and bombardment while, which is stirred primary particle, to be stirred, and bombardment time is
5-30min obtains the composite precursor that surface is cheated with micropore or irregular dimple.
3. a kind of preparation method of the lithium ion battery as described in claim 1 with artificial composite cathode material of silicon/carbon/graphite, feature
Be: the asphalt softening point in S3 step is 150-280 DEG C, it is experience airflow milling treated powder body material, D50 3-
5μm；The ratio of needle coke and pitch is 100:10-20.
4. a kind of artificial composite cathode material of silicon/carbon/graphite of lithium ion battery, it is characterised in that: it is -3 any according to claim 1
The artificial graphite composite negative pole material of preparation method production described in.
5. a kind of artificial composite cathode material of silicon/carbon/graphite of lithium ion battery as claimed in claim 4, it is characterised in that: the people
D50=14-21 μm for making composite cathode material of silicon/carbon/graphite, tap density 1.0-1.2g/cc, specific surface area 0.5-1.6m2/g；
Reversible specific capacity is 355-363mAh/g；Practical compacted density 1.8g/cc, room temperature 1C recycle 2000 weeks capacity retention ratios and are higher than
80%, electrode expansion is lower than 8% after recycling within 200 weeks.
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| CN115924905A (en) * | 2022-12-28 | 2023-04-07 | 广东众大智能科技有限公司 | Asphalt-coated needle coke granularity stabilizing method |
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Address after: 410600 Quanzhou North Road, Jinzhou District, Changsha, Hunan, China (Ningxiang Town, Jinzhou town) Applicant after: Hunan Branch Star graphite Co. Address before: 410645 Quanzhou New District, Jinzhou new district, Ningxiang, Changsha, Hunan Applicant before: HUNAN SHINZOOM TECHNOLOGY CO., LTD. |
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