CN107871859A - A kind of preparation method of Hyperhemodynamics lithium ion battery negative material - Google Patents
A kind of preparation method of Hyperhemodynamics lithium ion battery negative material Download PDFInfo
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- CN107871859A CN107871859A CN201610857131.0A CN201610857131A CN107871859A CN 107871859 A CN107871859 A CN 107871859A CN 201610857131 A CN201610857131 A CN 201610857131A CN 107871859 A CN107871859 A CN 107871859A
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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
- H01M4/58—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
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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 relates to technical field of lithium ion battery negative, specifically a kind of preparation method of Hyperhemodynamics lithium ion battery negative material, it is characterised in that use following preparation process：(1), crush；(2), batch mixing；(3), Low Temperature Heat Treatment；(4), medium temperature or high-temperature process；(5), cooling classification.Compared with prior art, covering helps to realize uniform cladding the present invention using the composition of pitch and mink cell focus, while takes into account the higher energy density of material；Obtained negative material is also obviously improved on absorbent and peel strength, charge-discharge magnification is high and good cycle；Its technique is simple, mild condition, safe, not harsh to equipment requirement easily realizes industrialization.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, specifically a kind of Hyperhemodynamics lithium-ion electric
The preparation method of pond negative material.
Background technology
Lithium rechargeable battery is compared to conventional batteries such as ni-mh, plumbic acids, with energy density is big, output voltage is high, oneself
The advantages that discharge rate is low, environment-friendly, memory-less effect, long lifespan, it has also become portable type electronic product and consumer electronics production
Main flow battery in product, and realize extensive use in electric vehicle, solar energy and wind power plant etc..
The most ripe negative material of the graphite as lithium secondary battery, has higher energy density concurrently, less expansion,
The features such as longer discharge platform, the main flow negative pole still as EV fields uses at present.But because graphite layers are away from smaller, lithium
The relative deformation of ion intercalation/deintercalation is larger, and inside has certain defect, and after repeatedly circulation, surface texture easily occurs
Destroy, produce new SEI films and consume more electrolyte, cause cycle performance to decline, this phenomenon shows on native graphite
It is particularly evident.
Surface coating can improve the rate charge-discharge performance of graphite as a kind of method of common improvement circulation,
It has been widely used.Presently the most common method for coating is charing or graphite after uniformly being mixed with graphite using fix-bitumen
Change, one layer of amorphous carbon or low degree of graphitization graphite are formed on raw graphite surface.This surface structure is more stable, discharge and recharge
Deformation is smaller, and internal graphite is played a protective role.Even so, but this kind of technique is deficient in the uniformity of cladding
Lack, part material graphite is still directly in contact with electrolyte during discharge and recharge, and these regions are easily sent out under high rate cyclic
Generating layer forms new SEI films with Li+, causes capacity attenuation from end face, consumption electrolyte is exposed.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of to have good covering property to internal graphite
The preparation method of lithium ion battery negative material, and the materials'use prepared is safe, has Hyperhemodynamics.
To achieve the above object, a kind of preparation method of Hyperhemodynamics lithium ion battery negative material, its feature are designed
It is, using following preparation process：
(1), crush：Graphite is crushed respectively with pitch；The average grain diameter of graphite after crushing is respectively 5~20 μm, than
Surface area difference≤15m2/ g, compacted density difference >=1.0g/cm3；The average grain diameter of pitch after crushing is 2~6 μm；
(2), batch mixing: with pitch: graphite: mink cell focus=3~10: 100: 5~20 ratio carries out mixing to obtain compound, makes
Each component belongs to homogeneously dispersed state in other any components；Described mink cell focus be include alkane, cycloalkane and
The mixture of aromatic hydrocarbon；
(3), Low Temperature Heat Treatment：Compound is subjected to Low Temperature Heat Treatment, the temperature of Low Temperature Heat Treatment under inert gas shielding
Spend for 500 DEG C~700 DEG C, the time is 2~3 hours；
(4), medium temperature or high-temperature process：By the compound after Low Temperature Heat Treatment, carried out under inert gas shielding medium temperature or
High-temperature heat treatment 2~3 hours；Described medium temperature heat treatment temperature is 1100 DEG C~1300 DEG C；The high-temperature heat treatment temperature is
2500 DEG C~3000 DEG C；
(5), cooling classification：Sieve classification processing is carried out after cooling, produces lithium ion battery negative material.
After batch mixing, the compound of gained can also be first put into after mechanical fusion equipment carries out fusion treatment, then is carried out low
Temperature processing.The step not necessarily step, but can make abundant extrusion and collision occurs between particle, to obtain higher cohesive force,
Can further it enhance product performance.
The graphite is individual particle native graphite or individual particle Delanium.
The pitch is the one or both in coal-based pitch and oil-based asphalt with the mixture of arbitrary proportion.
The density of described mink cell focus is more than 0.85g/cm3。
Described compound forms soft charcoal after medium temperature heat treatment and accounts for the 3%~8% of graphite cathode material gross weight.
The run time of described mechanical fusion equipment is 0~30min.
The equipment of described Low Temperature Heat Treatment is to drive blade or the mixing plant of ribbon rotation using main shaft.
Inert gas in described Low Temperature Heat Treatment is nitrogen or argon gas.
Inert gas in described medium temperature or high-temperature process is nitrogen or argon gas.
Compared with prior art, covering helps to realize uniform bag the present invention using the composition of pitch and mink cell focus
Cover, while take into account the higher energy density of material；Obtained negative material also has on absorbent and peel strength substantially to be carried
Rise, charge-discharge magnification is high and good cycle；Its technique is simple, mild condition, easily reality safe, not harsh to equipment requirement
Now industrialize.
Embodiment
The present invention is further described in conjunction with embodiment.
Embodiment 1
(1), native graphite is ground into 9.5 μm of powder；The pitch of coking value 62% is ground into 3 μm of asphalt powder
End；
(2), the asphalt powder of 9.5 μm of natural graphite powder of 20kg particle diameters, 2kg mink cell focuses and 1kg coking values 62% is mixed
Close uniform compound；
(3) compound, is put into mechanical fusion equipment, equipment operation 5min；
(4) compound after fusion, is subjected to 550 DEG C of Low Temperature Heat Treatment 3h under High Purity Nitrogen protection；
(5), the compound after Low Temperature Heat Treatment is carried out to 1200 DEG C of heat treatment 3h under High Purity Nitrogen protection；
(6) sieve classification processing is carried out after, cooling down, that is, is prepared into negative material, amorphous carbon is calculated to obtain according to coking value
Mass fraction is about 5.10%.
Embodiment 2
(1), native graphite is ground into 9.5 μm of powder；The pitch of coking value 62% is ground into 3 μm of asphalt powder
End；
(2), by 9.5 μm of natural graphite powder of 20kg particle diameters, 3.8kg mink cell focuses and 0.6kg coking values be 62% pitch
It is well mixed to obtain compound；
(3) compound, is put into mechanical fusion equipment, equipment operation 5min；
(4) compound after fusion, is subjected to 550 DEG C of Low Temperature Heat Treatment 3h under High Purity Nitrogen protection；
(5), the compound after Low Temperature Heat Treatment is carried out to 1200 DEG C of heat treatment 3h under High Purity Nitrogen protection,
(6) classification processing is carried out after, cooling down, that is, is prepared into negative material, amorphous carbon quality is calculated to obtain according to coking value
Fraction is about 5.10%.
Embodiment 3
(1), native graphite is ground into 9.5 μm of powder；The pitch of coking value 62% is ground into 3 μm of asphalt powder
End；
(2), the asphalt powder of 9.5 μm of native graphites of 20kg particle diameters, 1kg mink cell focuses and 1.322kg coking values 62% is mixed
Close uniform compound；
(3) compound, is put into mechanical fusion equipment, equipment operation 5min；
(4) compound after fusion, is subjected to 550 DEG C of Low Temperature Heat Treatment 3h under High Purity Nitrogen protection；
(5), the compound after Low Temperature Heat Treatment is carried out to 1200 DEG C of heat treatment 3h under High Purity Nitrogen protection；
(6) sieve classification processing is carried out after, cooling down, that is, is prepared into negative material, amorphous carbon is calculated to obtain according to coking value
Mass fraction is about 5.10%.
Embodiment 4
(1), native graphite is ground into 9.5 μm of powder；The green grass or young crops for dripping coking value 75% is ground into 3 μm of asphalt powder
End；
(2), the asphalt powder of 9.5 μm of native graphites of 20kg particle diameters, 2kg mink cell focuses and 0.83kg coking values 75% is mixed
It is uniform to obtain compound；
(3) compound, is put into mechanical fusion equipment, equipment operation 5min；
(4) compound after fusion, is subjected to 550 DEG C of Low Temperature Heat Treatment 3h under High Purity Nitrogen protection；
(5), the compound after Low Temperature Heat Treatment is carried out to 1200 DEG C of heat treatment 3h under High Purity Nitrogen protection；
(6) sieve classification processing is carried out after, cooling down, that is, is prepared into negative material, amorphous carbon is calculated to obtain according to coking value
Mass fraction is about 5.10%.
Embodiment 5
(1), native graphite is ground into 9.5 μm of powder；The pitch of coking value 62% is ground into 3 μm of asphalt powder
End；
(2), the asphalt powder of 9.5 μm of native graphites of 20kg particle diameters, 2kg mink cell focuses and 1kg coking values 62% is mixed equal
It is even to obtain compound；
(3) compound, is subjected to 550 DEG C of Low Temperature Heat Treatment 3h under High Purity Nitrogen protection；
(4), the compound after fusion is carried out to 1200 DEG C of heat treatment 3h under High Purity Nitrogen protection；
(5) sieve classification processing is carried out after, cooling down, that is, is prepared into negative material, amorphous carbon is calculated to obtain according to coking value
Mass fraction is about 5.10%.
Embodiment 6
(1), native graphite is ground into 9.5 μm of powder；The pitch of coking value 62% is ground into 3 μm of asphalt powder
End；
(2), the asphalt powder of 16.0 μm of native graphites of 20kg particle diameters, 2kg mink cell focuses and 1kg coking values 62% is mixed equal
It is even to obtain compound；
(3) compound, is put into mechanical fusion equipment, equipment operation 5min；
(4) compound after fusion, is subjected to 550 DEG C of Low Temperature Heat Treatment 3h under High Purity Nitrogen protection；
(5), the compound after Low Temperature Heat Treatment is carried out to 1200 DEG C of heat treatment 3h under High Purity Nitrogen protection；
(6) sieve classification processing is carried out after, cooling down, that is, is prepared into negative material, amorphous carbon is calculated to obtain according to coking value
Mass fraction is about 5.10%.
Embodiment 7
(1), native graphite is ground into 9.5 μm of powder；The pitch of coking value 62% is ground into 3 μm of asphalt powder
End；
(2), the asphalt powder of 9.5 μm of native graphites of 20kg particle diameters, 3kg mink cell focuses and 1.5kg coking values 62% is mixed
It is uniform to obtain compound；
(3) compound, is put into mechanical fusion equipment, equipment operation 5min；
(4) compound after fusion, is subjected to 550 DEG C of Low Temperature Heat Treatment 3h under High Purity Nitrogen protection；
(5), the compound after Low Temperature Heat Treatment is carried out to 1200 DEG C of heat treatment 3h under High Purity Nitrogen protection；
(6) sieve classification processing is carried out after, cooling down, that is, is prepared into negative material, amorphous carbon is calculated to obtain according to coking value
Mass fraction is about 7.65%.
Above-described embodiment 1-7 physical and chemical index test is as shown in table 1, and electric performance test is as shown in table 2.
Table 1
Table 2
Based on embodiment 1 in each embodiment, embodiment 2 are coated with mink cell focus, it is comprehensive for specific surface area it is small, D.C. resistance
Greatly, high rate performance is poor；
For embodiment 3 based on pitch-coating, cyclicity is a bit weaker, and high rate performance is suitable；
Embodiment 4 is using the higher pitch of coking value, and specific surface area is somewhat larger, and D.C. resistance is smaller, and high rate performance is more
Good, this in 7 embodiments is most preferred embodiment；
Embodiment 5 eliminates mechanical fusion process, more lower than the tap density of embodiment 1, has one to be fixed to overall performance
Ring；
Embodiment 6 is using big particle diameter native graphite as raw material, and energy density is high but high rate performance is poor；
Embodiment 7 adds 50% covering amount on the premise of same ratio, and high rate performance significantly improves, but energy density
Equally also reduce obvious.
The invention has the characteristics that：Used covering is the composition of pitch and mink cell focus, this mixing cladding
Mode help to realize uniform cladding, while take into account the higher energy density of material.When using only pitch-coating, due to drip
The blue or green mobility under melting state is general, and the level of coverage on the surface of graphite does not reach perfect condition, and the high magnification of material follows
Ring limited performance system.When being coated using only mink cell focus, because coking value is very low, its carbonize or graphitization after in the structure that is formed
Abundant duct containing gas overflowing generation, short texture be not fine and close so that the real density of whole graphite particle reduces, and compacting is close
Degree declines to be become apparent compared with pitch cladding process, and the energy density of material is too low.Attempt to find by multiple, using pitch and
Two kinds of components of mink cell focus, and both relative amount and total content are adjusted, satisfactory negative material can effectively be prepared.
In addition, input mechanical fusion equipment, this procedure help to carry after raw material and covering are mixed together uniformly
High-tap density, it is helpful to the processing characteristics of product.It will enter in the equipment of graphite and cladding agent composition input good dispersion
Row Low Temperature Heat Treatment, be advantageous to covering and realize uniformly cladding in graphite surface.
With existing negative pole native graphite pitch-coating condition ratio, the material gram volume prepared using the present invention is reached
Compacted density reaches 1.65g/cm next time by more than 360mAh/g, 17MPa3, tap density reaches 1.10g/cm3, in identical amorphous carbon
On the premise of content, by 1C discharge and recharges and 500 weeks loop tests, capability retention can improve 2%~5%, up to more than 90%,
Applied to can also obtain similar effects on Delanium.Also, negative material made from the method also has substantially on absorbent
Lifting.
Present invention process is simple, mild condition, safe, not harsh to equipment requirement easily realizes industrialization, the present invention
The graphite negative material of lithium ion battery provided has potential application value in power vehicle, field of wind power generation.
Claims (10)
1. a kind of preparation method of Hyperhemodynamics lithium ion battery negative material, it is characterised in that use following preparation process：
(1), crush：Graphite is crushed respectively with pitch；The average grain diameter of graphite after crushing is respectively 5~20 μm, compares surface
Integrate not≤15m2/ g, compacted density difference >=1.0g/cm3；The average grain diameter of pitch after crushing is 2~6 μm；
(2), batch mixing：With pitch: graphite: mink cell focus=3~10: 100: 5~20 ratio carries out mixing to obtain compound, makes each
Kind component belongs to homogeneously dispersed state in other any components；Described mink cell focus is to include alkane, cycloalkane and fragrance
The mixture of hydrocarbon；
(3), Low Temperature Heat Treatment：Compound is subjected to Low Temperature Heat Treatment under inert gas shielding, the temperature of Low Temperature Heat Treatment is
500 DEG C~700 DEG C, the time is 2~3 hours；
(4), medium temperature or high-temperature process：By the compound after Low Temperature Heat Treatment, medium temperature or high temperature are carried out under inert gas shielding
Heat treatment 2~3 hours；Described medium temperature heat treatment temperature is 1100 DEG C~1300 DEG C；The high-temperature heat treatment temperature is 2500
DEG C~3000 DEG C；
(5), cooling classification：Sieve classification processing is carried out after cooling, produces lithium ion battery negative material.
A kind of 2. preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, it is characterised in that
After the compound input mechanical fusion equipment of gained carries out fusion treatment after described batch mixing, then carry out Low Temperature Heat Treatment.
A kind of 3. preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, it is characterised in that
The graphite is individual particle native graphite or individual particle Delanium.
A kind of 4. preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, it is characterised in that
The pitch is the one or both in coal-based pitch and oil-based asphalt with the mixture of arbitrary proportion.
A kind of 5. preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, it is characterised in that
The density of described mink cell focus is more than 0.85g/cm3。
A kind of 6. preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, it is characterised in that
Described compound forms soft charcoal after medium temperature heat treatment and accounts for the 3%~8% of graphite cathode material gross weight.
A kind of 7. preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, it is characterised in that
The run time of described mechanical fusion equipment is 0~30min.
A kind of 8. preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, it is characterised in that
The equipment of described Low Temperature Heat Treatment is to drive blade or the mixing plant of ribbon rotation using main shaft.
A kind of 9. preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, it is characterised in that
Inert gas in described Low Temperature Heat Treatment is nitrogen or argon gas.
10. a kind of preparation method of Hyperhemodynamics lithium ion battery negative material as claimed in claim 1, its feature exist
In the inert gas in described medium temperature or high-temperature process is nitrogen or argon gas.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112670461A (en) * | 2019-12-31 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Natural graphite carbon coated negative electrode material, preparation method thereof and lithium ion battery |
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|---|---|---|---|---|
| CN1278437C (en) * | 2004-12-02 | 2006-10-04 | 辽宁弘光科技集团有限公司 | Production method of carbon nagtive electrode material of lithium ion cell |
| CN103094536A (en) * | 2013-02-05 | 2013-05-08 | 新乡远东电子科技有限公司 | High-capacity lithium ion secondary battery cathode carbon material |
| CN103346326A (en) * | 2013-07-08 | 2013-10-09 | 辽宁弘光科技(集团)有限公司 | Preparation method for carbon cathode material of lithium ion battery |
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- 2016-09-27 CN CN201610857131.0A patent/CN107871859A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1278437C (en) * | 2004-12-02 | 2006-10-04 | 辽宁弘光科技集团有限公司 | Production method of carbon nagtive electrode material of lithium ion cell |
| CN103094536A (en) * | 2013-02-05 | 2013-05-08 | 新乡远东电子科技有限公司 | High-capacity lithium ion secondary battery cathode carbon material |
| CN103346326A (en) * | 2013-07-08 | 2013-10-09 | 辽宁弘光科技(集团)有限公司 | Preparation method for carbon cathode material of lithium ion battery |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112670461A (en) * | 2019-12-31 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Natural graphite carbon coated negative electrode material, preparation method thereof and lithium ion battery |
| CN112670461B (en) * | 2019-12-31 | 2022-11-29 | 宁波杉杉新材料科技有限公司 | Natural graphite carbon coated negative electrode material, preparation method thereof and lithium ion battery |
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Application publication date: 20180403 |