CN110518203A - Compound soft carbon negative electrode material and preparation method thereof, lithium ion battery - Google Patents
Compound soft carbon negative electrode material and preparation method thereof, lithium ion battery Download PDFInfo
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- CN110518203A CN110518203A CN201910722596.9A CN201910722596A CN110518203A CN 110518203 A CN110518203 A CN 110518203A CN 201910722596 A CN201910722596 A CN 201910722596A CN 110518203 A CN110518203 A CN 110518203A
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- H01—ELECTRIC ELEMENTS
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- 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
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H01M4/625—Carbon or graphite
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Abstract
The invention discloses a kind of preparation method of compound soft carbon negative electrode material, step: condensate is reacted to obtain by pitch is aggregated, polymerization temperature is 300~500 DEG C, and polymerization time is 2-4 hours；Polymer is solidified 2~6 hours in the environment that temperature is 200~500 DEG C；After the completion of curing process, polymer is crushed, is classified, and is carbonized in advance low-temperature treatment 8~24 hours at a temperature of 500 DEG C~650 DEG C and obtains carbon precursor；Carbon precursor is crushed again, is classified, and high temperature cabonization processing obtains carbonized particles in 12~24 hours at a temperature of 800 DEG C~1500 DEG C；Carbonized particles are uniformly mixed with the sub- silicon of oxidation with the ratio of certain mass ratio, and stands 1.5~3.0 hours and obtains finished product.Compound soft carbon negative electrode material is made in the preparation method, and for discharge capacity up to 400mAh/g or more, compacted density is high, and 85% or more first charge-discharge efficiency reduces the loss of irreversible capacity.
Description
Technical field
The present invention relates to the technical field of lithium battery, in particular to a kind of compound soft carbon negative electrode material and preparation method thereof,
Lithium ion battery.
Background technique
Lithium ion battery has many advantages, such as small in size, light weight, for efficiently use lithium ion battery these advantages, in recent years
Come, scientific research personnel is actively developing the lithium ion battery for electric car.Electric car generally comprises only using electronic
The electric car (EV) of machine driving and the hybrid electric automobile (HEV) driven by engine and motor combination,
In, the characteristics of HEV is economical and low oil consumption.
In this way, it is necessary to which HEV lithium ion battery has and the lithium ion battery institute not phase in existing small-sized Portable device
Same characteristic, needs better high rate during charging-discharging and greater security.Soft carbon negative electrode material has securely surely due to it
Fixed structure, it is preferably under high current charge-discharge using and be concerned, good security performance is expected in electric car
On be applied.
Chinese patent literature CN1947286A prepares amorphous with the oxidation of porosity pelletted pitch fluidized bed, charing method
Carbon, but this method there is discharge capacities low, the low defect of compacted density.
For this purpose, we have proposed a kind of compound soft carbon negative electrode materials and preparation method thereof, lithium ion battery.
Summary of the invention
The main purpose of the present invention is to provide a kind of compound soft carbon negative electrode materials and preparation method thereof, have discharge capacity
Greatly, the advantage that compacted density is high, first charge-discharge efficiency is big.
To achieve the above object, the present invention provides a kind of compound soft carbon negative electrode material and preparation method thereof, this is compound soft
The preparation method of carbon negative pole material includes the following steps:
Step (1) reacts to obtain condensate for pitch is aggregated, and polymerization temperature is 300~500 DEG C, and polymerization time is that 2-4 is small
When.Preferably, pitch is asphalt or coal tar pitch is one of or two kinds mix, and asphalt and coal tar pitch are medium temperature
Pitch.
Step (2) solidifies polymer 2~6 hours in the environment that temperature is 200~500 DEG C.Curing process is completed
Afterwards, polymer crushed, be classified, the revolving speed of pulverizer is 800~1000 revs/min in crushing process；Classification is using sieve
Divide hierarchical approaches, is screened using 60 meshes, and sieve extracting screen underflow.Further, pre- charcoal at a temperature of 500 DEG C~650 DEG C
Change low-temperature treatment 8~24 hours and obtains carbon precursor.Wherein, curing process, pre- carbonization low-temperature treatment carry out in inert gas.
Carbon precursor is crushed again, is classified by step (3), in crushing process the revolving speed of pulverizer be 2000~8000 turns/
Minute, using grader hierarchical approaches, the frequency of grader is 90-120HZ, and after being crushed, being classified, the volume of carbon precursor is average
Partial size D50 is 8~13 μm.Further, pyrocarbon at a temperature of 800 DEG C~1500 DEG C of the carbon precursor after crushing, being classified
Change processing and obtains carbonized particles in 12~24 hours；
Step (4), carbonized particles with aoxidize sub- silicon with mass ratio be uniformly mixed for the ratio of 90:10~99:1, and it is quiet
It sets 1.5~3.0 hours and obtains finished product.Preferably, aoxidizing sub- silicon is to aoxidize sub- silicon alloy material, and the volume for aoxidizing sub- silicon is averaged grain
Diameter D50 is 5~10 μm.
The volume of one kind compound soft carbon negative electrode material as made from above-mentioned preparation method, the compound soft carbon negative electrode material is flat
Equal partial size D50 is 10~35 μm, and specific surface area is 1~25m2/ g, real density are 1.2~2.5g/cm3, tap density be 0.7~
1.3g/cm3, discharge capacity is greater than 400mAh/g, and first charge-discharge efficiency is greater than 85%.
A kind of lithium ion battery, including using above-mentioned compound soft carbon negative electrode material as lithium ion battery negative material.
The prior art is compared, and the invention has the following beneficial effects: compound soft carbon is made using preparation method of the invention
Negative electrode material, for discharge capacity up to 400mAh/g or more, compacted density is high, and 85% or more first charge-discharge efficiency reduces not
The loss of reversible capacity reduces the dosage of anode.
Specific embodiment
To be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, below with reference to
Specific embodiment, the present invention is further explained.
Compound soft carbon negative electrode material is made using the preparation method of compound soft carbon negative electrode material in the present invention, obtained compound soft
Carbon negative pole material chemical property is good, and high rate during charging-discharging and good cycle, safety and stability is good, and to electricity
It solves liquid and other additive adaptability is preferable.And preparation method simple process of the invention is easy, raw material sources extensively and cost
It is low.
Embodiment 1
1. coal tar pitch carries out polymerization reaction 2 hours obtaining condensate at 320 DEG C；2. condensate is in inert gas in 300
DEG C curing process 4 hours, then crush through 1000 revs/min of revolving speeds of pulverizer, cross 60 meshes, extracting screen underflow in inert gas in
600 DEG C obtain carbon precursor in pre- charing process 16 hours；3. crushing through 2000 revs/min of revolving speeds of pulverizer, it is classified unit frequency 105Hz
Classification obtains the carbon precursor particle that volume average particle size D50 is 8.3 μm, in inert gas at 1100 DEG C of high temperature carbonization heat
Obtain carbonized particles within reason 18 hours；4. carbonized particles mix 1.5 hours by the mass ratio of 9:1 with the sub- silicon of oxidation to get compound soft carbon
Negative electrode material；Wherein, the volume volume average particle size D50 of the oxidation Asia silicon is 7 μm.
Embodiment 2
1. carrying out polymerization reaction 2 hours obtaining condensate at 420 DEG C of coal tar pitch；2. condensate is consolidated for 500 DEG C in inert gas
Change processing 2 hours, then crushed through 800 revs/min of revolving speeds of pulverizer, crosses 60 meshes, extracting screen underflow is in inert gas in 600 DEG C
Obtain carbon precursor within pre- charing process 20 hours；3. crushing through 5000 revs/min of revolving speeds of pulverizer, classification unit frequency 90Hz classification is obtained
The carbon precursor particle for being 12.9 μm to volume average particle size D50 is small in 1100 DEG C of high temperature carbonization heat treatments 24 in inert gas
When obtain carbonized particles；4. carbonized particles mix 3 hours by the mass ratio of 95:5 with the sub- silicon of oxidation to get compound soft carbon cathode material
Material；Wherein, the volume average particle size D50 of the oxidation Asia silicon is 10 μm.
Embodiment 3
1. asphalt carries out polymerization reaction 4 hours obtaining condensate at 300 DEG C；2. condensate is 500 in inert gas
DEG C curing process 2 hours, then crush through 1000 revs/min of revolving speeds of pulverizer, cross 60 meshes, extracting screen underflow in inert gas in
650 DEG C obtain carbon precursor in pre- charing process 8 hours；3. crushing through 8000 revs/min of revolving speeds of pulverizer, it is classified unit frequency 105Hz
Classification obtains the carbon precursor particle that volume average particle size D50 is 8.3 μm, is heat-treated in inert gas in 800 DEG C of high temperature carbonizations
24 hours；4. carbonized particles mix 2 hours by the mass ratio of 99:1 with the sub- silicon of oxidation to get compound soft carbon negative electrode material；Wherein,
The volume average particle size D50 of the oxidation Asia silicon is 6 μm.
Embodiment 4
1. asphalt carries out polymerization reaction 2 hours obtaining condensate at 500 DEG C；2. condensate is 200 in inert gas
DEG C curing process 6 hours, then crush through 900 revs/min of revolving speeds of pulverizer, cross 60 meshes, extracting screen underflow in inert gas in
550 DEG C obtain carbon precursor in pre- charing process 16 hours；3. crushing through 2000 revs/min of revolving speeds of pulverizer, it is classified unit frequency 105Hz
Classification obtains the carbon precursor particle that volume average particle size D50 is 13.8 μm, in inert gas at 1500 DEG C of high temperature carbonization heat
Reason 12 hours；4. carbonized particles mix 2.5 hours by the mass ratio of 95:5 with the sub- silicon of oxidation to get compound soft carbon negative electrode material；
Wherein, the volume average particle size D50 of the oxidation Asia silicon is 5 μm.
Embodiment 5
1. coal tar pitch carries out polymerization reaction 3 hours obtaining condensate at 420 DEG C；2. 300 DEG C in an inert atmosphere of condensate
Curing process 2 hours, then crushed through 800 revs/min of revolving speeds of pulverizer, 60 meshes are crossed, extracting screen underflow is in inert gas in 650
DEG C pre- charing process 24 hours carbon precursor；3. being crushed through 2000 revs/min of revolving speeds of pulverizer, unit frequency 90Hz points of classification
Grade obtains the carbon precursor particle that volume average particle size D50 is 11.2 μm, is heat-treated in inert gas in 1100 DEG C of high temperature carbonizations
18 hours；4. carbonized particles are mixed 2 hours with the sub- silicon of oxidation by the mass ratio of 95:5, the volume average particle size of the oxidation Asia silicon
D50 is 7 μm.
Comparative example 1
Coal tar pitch carries out polymerization reaction 2 hours obtaining condensate at 420 DEG C, after reaction 600 DEG C in inert gas
Pre- charing process 20 hours, obtained block material is crushed through 8000 revs/min of revolving speeds of pulverizer, classification unit frequency 90Hz is classified
The carbon precursor that volume average particle size D50 is 9.7 μm is obtained, 1100 DEG C of high temperature carbonizations are heat-treated 12 hours in inert gas,
Product is mixed 2.5 hours with the sub- silicon of oxidation by the mass ratio of 95:5, and the volume average particle size D50 of the oxidation Asia silicon is 6 μm.
Comparative example 2
Coal tar pitch carries out polymerization reaction 2 hours obtaining condensate at 420 DEG C, after reaction 300 DEG C in inert gas
Curing process 2 hours, the block material that curing process obtains crushed through 800 revs/min of revolving speeds of pulverizer, crosses 60 meshes, screenings
600 DEG C pre- charing process 16 hours in inert gas, obtained block material crush through 2000 revs/min of revolving speeds of pulverizer, divide
Grade unit frequency 105Hz is classified to obtain the carbon precursor that partial size D50 is 10.9 μm, 1100 DEG C of high temperature carbonization heat treatment in inert gas
18 hours, obtain soft carbon negative electrode material.
Compound soft carbon negative electrode material is made in preparation method by above-mentioned compound soft carbon negative electrode material, below by experiment
Data test to the performance that compound soft carbon negative electrode material is made:
Using the volume average particle size D50 of laser fineness gage MS2000 measurement sample in the present invention, using super perseverance
Warm water tank SC-15 measures the real density of sample, using the ash content of high-temperature electric resistance furnace SX2-2.5-12 measurement sample, using tap density
Tester FZS4-4B measures the tap density of sample, using the specific surface area of specific surface area measuring instrument NOVA2000 measurement sample.
Using half-cell test method electric discharge capacity and first charge-discharge efficiency, in half-cell test process are as follows: each
The negative electrode material sample of embodiment or comparative example, the N-Methyl pyrrolidone containing 6~7% Kynoar and 2% conduction
Carbon black is uniformly mixed, and is applied on copper foil, and it is to be dried in vacuo 4 hours in 110 DEG C of vacuum ovens that the pole piece coated, which is put into temperature,
It is spare.Simulated battery is assemblied in the German Braun glove box of applying argon gas and carries out, and electrolyte is 1M LiPF6+EC:DEC:DMC
=1:1:1 (volume ratio), metal lithium sheet are to electrode, and electrochemical property test is in U.S. ArbinBT2000 type cell tester
Upper progress, charging/discharging voltage range are 0.005 to 1.0V, charge-discharge velocity 0.1C.
Table 1 is the compound soft carbon negative electrode material volume average particle size D50, true that the embodiment of the present invention and comparative example obtain
Density, tap density, specific surface area, the data of discharge capacity and first charge-discharge efficiency compare:
The performance parameter of each embodiment of table 1 and comparative example
Table 1 is please referred to, the volume average particle size D50 of compound soft carbon negative electrode material of the invention is 10~35 μm, specific surface
Product is 1~25m2/ g, real density are 1.2~2.5g/cm3, tap density is 0.7~1.3g/cm3.According to upper table comparison it is found that
The first charge-discharge efficiency of comparative example 1 is low, is 80.8%；The discharge capacity and first charge-discharge efficiency of comparative example 2
It is all low；And compound soft carbon negative electrode material is made using preparation method of the invention, discharge capacity is up to 400mAh/g or more, for the first time
85% or more efficiency for charge-discharge, reduces the loss of irreversible capacity, reduces the dosage of anode.Compound soft carbon cathode of the invention
Material on electrolyte and other additive adaptability are good, and the negative electrode slurry good dispersion viscosity of modulation is normal, and sieving performance is good, pole
Piece caking property is good.
The present invention also provides a kind of lithium ion battery, by the production lithium of compound soft carbon negative electrode material made from embodiment 2 from
Sub- battery, and full battery test is carried out to the lithium ion battery.Full battery test method are as follows: compound soft carbon negative electrode material is born
Pole, cobalt acid lithium make anode, and 1M-LiPF6EC:DMC:EMC=1:1:1 (volume ratio) solution is assembled into full battery as electrolyte, survey
Examination 1C charge and discharge 600 times.
Lithium ion battery obtained by the compound soft carbon negative electrode material of the present invention has a safety feature, and over-charging is preferable, pole
Piece processability is good；Good cycle, recycling 600 capacity retention ratios can reach 95%；Compound soft carbon negative electrode material of the invention
Obtained lithium ion battery product property is stablized, almost without difference between batch: using compound soft carbon cathode of the invention
The half-cell (4/group) and full battery (20/group) of material assembling, the charging and discharging curve of every group of battery essentially coincides, consistency
Very good, the electrical property and physical and chemical index of the negative electrode material of the same terms preparation have reproducibility.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of preparation method of compound soft carbon negative electrode material, which comprises the steps of:
Step (1) reacts to obtain condensate for pitch is aggregated, and polymerization temperature is 300~500 DEG C, and polymerization time is 2-4 hours；
Step (2) solidifies the polymer 2~6 hours in the environment that temperature is 200~500 DEG C；Curing process is completed
Afterwards, polymer crushed, be classified, and carbonized in advance low-temperature treatment 8~24 hours at a temperature of 500 DEG C~650 DEG C and obtain carbon
Precursor；
Carbon precursor is crushed again, is classified by step (3), and the high temperature cabonization processing 12~24 at a temperature of 800 DEG C~1500 DEG C
Hour obtains carbonized particles；
The carbonized particles are uniformly mixed with the sub- silicon of oxidation with the ratio of certain mass ratio, and stand 1.5~3.0 by step (4)
Hour obtains finished product.
2. the preparation method of compound soft carbon negative electrode material according to claim 1, which is characterized in that the pitch is petroleum
Pitch or coal tar pitch one of which or two kinds of mixing.
3. the preparation method of compound soft carbon negative electrode material according to claim 1, which is characterized in that in the step (2)
The revolving speed of pulverizer is 800~1000 revs/min in crushing process.
4. the preparation method of compound soft carbon negative electrode material according to claim 1, which is characterized in that in the step (2)
Classification uses sieve classification mode, is screened using 60 meshes, and sieve extracting screen underflow.
5. the preparation method of compound soft carbon negative electrode material according to claim 1, which is characterized in that in the step (3)
The revolving speed of pulverizer is 2000~8000 revs/min in crushing process.
6. the preparation method of compound soft carbon negative electrode material according to claim 1, which is characterized in that in the step (3)
Classification uses grader hierarchical approaches, and the frequency of grader is 90-120HZ.
7. the preparation method of compound soft carbon negative electrode material according to claim 1, which is characterized in that the sub- silicon of the oxidation is
Sub- silicon alloy material is aoxidized, the volume average particle size D50 for aoxidizing sub- silicon is 5~10 μm.
8. the preparation method of compound soft carbon negative electrode material according to claim 1, which is characterized in that in the step (4)
Carbonized particles and the mass ratio for aoxidizing sub- silicon are 90:10~99:1.
9. a kind of soft carbon negative electrode material compound as made from preparation method according to any one of claims 1 to 8, feature exist
In the volume average particle size D50 of the compound soft carbon negative electrode material is 10~35 μm, and specific surface area is 1~25m2/ g, real density
For 1.2~2.5g/cm3, tap density is 0.7~1.3g/cm3, for discharge capacity greater than 400mAh/g, first charge-discharge efficiency is big
In 85%.
10. a kind of lithium ion battery, which is characterized in that including being made using compound soft carbon negative electrode material as claimed in claim 9
For lithium ion battery negative material.
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| TWI720805B (en) * | 2020-01-31 | 2021-03-01 | 台灣中油股份有限公司 | Soft carbon and its preparation method |
| CN112670465A (en) * | 2020-04-21 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Composite pyrolytic carbon material and preparation method and application thereof |
| CN114141993A (en) * | 2021-11-25 | 2022-03-04 | 广东凯金新能源科技股份有限公司 | Processing technology of composite modified graphite negative electrode with good cycling stability |
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Application publication date: 20191129 |