CN109768245A - A kind of lithium ion battery high power density negative electrode material and preparation method - Google Patents
A kind of lithium ion battery high power density negative electrode material and preparation method Download PDFInfo
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- CN109768245A CN109768245A CN201811642656.8A CN201811642656A CN109768245A CN 109768245 A CN109768245 A CN 109768245A CN 201811642656 A CN201811642656 A CN 201811642656A CN 109768245 A CN109768245 A CN 109768245A
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- 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
Abstract
The present invention provides a kind of lithium ion battery high power density negative electrode materials, including soft carbon matrix, the amorphous conductive carbon coating layer being uniformly wrapped on soft carbon matrix, preparation method are as follows: pre-oxidize amorphous carbon material, then pre-oxidation amorphous carbon material is put into carbide furnace and heats pre- carbonization, pre- carbonization soft carbon particle is subjected to broken classification again, it is then placed in rotary furnace and carries out CVD cladding with organic carbon source gas, obtain presoma, presoma is finally subjected to carbonization treatment, screening, obtains soft carbon finished product.The negative electrode material of the method for the present invention preparation has reversible capacity, for the first time coulombic efficiency and the high rate performance for being apparently higher than existing negative electrode material.
Description
Technical field
The present invention relates to a kind of lithium ion battery negative material and preparation method thereof, especially a kind of lithium ion battery is compound
Negative electrode material and preparation method thereof.
Background technique
With the continuous deterioration in short supply with climatic environment of global petroleum resources, develop the new-energy automobile of clean energy-saving by
To the great attention of countries in the world.The development of new-energy automobile, key is in its electrical source of power.Currently, commercialized lithium-ion electric
Pond mainly uses graphite negative electrodes material, but power density is lower, is unable to satisfy the following lithium ion battery to high power density
Demand.So exploitation high-performance novel electrode material becomes research emphasis, soft carbon class negative electrode material is because having irregular random layer knot
Structure, therefore its fast charging and discharging performance, cycle performance and security performance are excellent, but soft carbon first charge discharge efficiency is lower, and voltage platform
It is higher, matched with positive electrode in need to increase positive usage amount, be difficult to meet business application.CN101916856A discloses one kind
Lithium ion power and energy-storage battery negative electrode material and preparation method thereof, using the pitch that catalyst is added, through 500 ~ 1300 DEG C
Carbonization treatment obtains, and preparation method includes: increasing temperature and pressure, and heat of carbonization polycondensation reaction occurs, is washed out, extracts, washs again, dries
It is dry to obtain mesophase ball presoma, using carbonization treatment, obtain lithium ion power and energy-storage battery negative electrode material, but its
Head effect is too low, limits its application.
Summary of the invention
It is close the purpose of the invention is to overcome the deficiencies of the prior art and provide a kind of new lithium ion battery high power
Spend negative electrode material and preparation method.
The present invention is achieved by the following technical programs:
A kind of lithium ion battery high power density negative electrode material, which is characterized in that including soft carbon matrix, be uniformly wrapped on soft carbon
Amorphous conductive carbon coating layer on matrix.
A kind of preparation method of lithium ion battery high power density negative electrode material, which comprises the following steps:
A1, amorphous carbon material pre-oxidation: amorphous carbon material and hydrogen peroxide are pre-oxidized in stirring in water bath pot, pre-oxidized
Temperature be 70-100 DEG C, preoxidation time be 2-10 h；
A2, amorphous carbon material are carbonized in advance: the pre-oxidation amorphous carbon material obtained after step A1 processing being put into carbide furnace and is heated
Pre- carbonization, using atmosphere protection, 2-10 DEG C of heating rate/min is warming up to 500-1000 DEG C, and soaking time 1-5h obtains pre- carbon
Change soft carbon particle；
A3, it is crushed, classification: the pre- carbonization soft carbon particle that step A2 is obtained is crushed, and is classified to D50It is 5-10 μm, obtains
Soft carbon particle；
A4, gas phase cladding: carrying out CVD cladding with organic carbon source gas in rotary furnace for soft carbon particle obtained in step A3,
It is coated under atmosphere protection and carries out, heating rate is 2-10 DEG C/min, and temperature of plate is 600-1000 DEG C, and the cladding time is 2-
8h obtains presoma；
A5, carbonization, sieving: the presoma progress carbonization treatment that step A4 is obtained, atmosphere protection, 2-10 DEG C of heating rate/
Min, carburizing temperature are 1000-1300 DEG C, carbonization time 2-6h；It is sieved with screening machine, obtains soft carbon finished product.
It preferably, according to mass ratio is 1:1-5:1 in stirring in water bath pot by amorphous carbon material and hydrogen peroxide in step A1
In pre-oxidized, wherein hydrogen peroxide mass fraction be 5%-20%；
Preferably, in step A1, the amorphous carbon material is 2500 DEG C or more graphitizable carbon, and the amorphous carbon material is
One of petroleum coke, needle coke, carbon fiber and non-graphitized carbonaceous mesophase spherules or a variety of combinations.
Preferably, in step A2 and A5, the carbide furnace can be pushed bat kiln, roller kilns, rotary kiln；
Preferably, for non-oxidizing atmosphere protection, gas used by the non-oxidizing atmosphere is protected is the atmosphere protection
Any one in nitrogen, helium, argon gas or hydrogen or a variety of combinations.
Preferably, in step A3, the pre- carbonization soft carbon particle obtained after step A2 processing is crushed, described be crushed is adopted
Mode is mechanical mill, airflow milling, ball milling；
Preferably, in step A4, the organic carbon source gas that the gas phase carbon coating treatment process is selected is hydro carbons, the organic carbon
Source gas is any one or at least two in methane, ethylene, acetylene, propane, benzene,toluene,xylene, styrene or phenol
The combination of kind.
Preferably, in step A4, it is 3-15% that the gas phase, which coats carbon source covering amount used,.
Compared with prior art, the present invention is had the advantages that
(1) present invention removes defect by pre-oxidation process, improves surface texture, forms passivation layer, introduces nano-pore and nanometer
Channel is conducive to improve the reversible gram volume of soft carbon material, first effect and high rate performance.
(2) present invention is uniformly coated amorphous carbon layer by way of gas phase cladding to soft carbon particle surface, improves soft carbon
Surface nonactive site improves interface, advantageously forms stable SEI film, improves coulombic efficiency for the first time.
(3) present invention solves in the prior art directly when using soft carbon as cathode material of lithium ion battery, is deposited
First charge discharge efficiency it is lower, voltage platform is higher, matched with positive electrode in need the problem of increasing positive usage amount.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of soft carbon composite negative pole material prepared by embodiment 1.
Fig. 2 is the XRD diagram of soft carbon composite negative pole material prepared by embodiment 1.
Fig. 3 is the TEM figure of soft carbon composite negative pole material prepared by embodiment 1.
Specific embodiment
Embodiment 1
By needle coke and hydrogen peroxide, hydrogen peroxide mass fraction is 5%, and the mass ratio of needle coke and hydrogen peroxide is 1:1 in water
It is pre-oxidized in bath agitated kettle, temperature is 70 DEG C, preoxidation time 2h.Needle coke is put into carbide furnace, nitrogen atmosphere
Protection, 2 DEG C/min of heating rate are warming up to 500 DEG C, soaking time 1h.Soft carbon particle after pre- carbonization is subjected to broken be classified to
D50It is 5 μm.Obtained soft carbon particle is subjected to CVD cladding with methane in rotary furnace, heating rate is 2 DEG C/min, cladding temperature
Degree is 600 DEG C, and the cladding time is 2h, obtains presoma.Presoma is subjected to carbonization treatment, nitrogen atmosphere protection, heating rate 2
DEG C/min, carburizing temperature is 1000 DEG C, carbonization time 2h.It is sieved with screening machine, obtains soft carbon finished product, is i.e. soft carbon is compound
Negative electrode material, SEM figure, XRD diagram and the TEM of the soft carbon composite negative pole material distinguish as shown in Figure 1, Figure 2, Figure 3 shows.
Embodiment 2
By petroleum coke and hydrogen peroxide, hydrogen peroxide mass fraction is 10%, and the mass ratio of petroleum coke and hydrogen peroxide is 2:1,
It is pre-oxidized in stirring in water bath pot, temperature is 80 DEG C, and preoxidation time is 6 h.Petroleum coke is put into carbide furnace, helium gas
Atmosphere protection, 5 DEG C/min of heating rate are warming up to 650 DEG C, soaking time 3h.Soft carbon particle after pre- carbonization is subjected to broken classification
To D50It is 6 μm.Obtained soft carbon particle is subjected to CVD cladding with ethylene in rotary furnace, heating rate is 4 DEG C/min, cladding
Temperature is 700 DEG C, and the cladding time is 3h, obtains presoma.Presoma is subjected to carbonization treatment, helium atmosphere protection, heating speed
4 DEG C/min is spent, carburizing temperature is 1100 DEG C, carbonization time 4h.It is sieved with screening machine, obtains soft carbon finished product.
Embodiment 3
By carbon fiber and hydrogen peroxide, hydrogen peroxide mass fraction is 15%, and the mass ratio of carbon fiber and hydrogen peroxide is that 4:1 exists
It is pre-oxidized in stirring in water bath pot, temperature is 90 DEG C, and preoxidation time is 8 h.Carbon fiber is put into carbide furnace, argon gas gas
Atmosphere protection, 7 DEG C/min of heating rate are warming up to 800 DEG C, soaking time 4h.Soft carbon particle after pre- carbonization is subjected to broken classification
To D50It is 9 μm.Obtained soft carbon particle is subjected to CVD cladding with acetylene in rotary furnace, heating rate is 7 DEG C/min, cladding
Temperature is 900 DEG C, and the cladding time is 5h, obtains presoma.Presoma is subjected to carbonization treatment, argon atmosphere protection, heating speed
8 DEG C/min is spent, carburizing temperature is 1200 DEG C, carbonization time 5h；It is sieved with screening machine, obtains soft carbon finished product.
Embodiment 4
By non-graphitized carbonaceous mesophase spherules and hydrogen peroxide, hydrogen peroxide mass fraction is 20%, and non-graphitized mesocarbon is micro-
The mass ratio of ball and hydrogen peroxide is that 5:1 is pre-oxidized in stirring in water bath pot, and temperature is 100 DEG C, preoxidation time 10
h.Non-graphitized carbonaceous mesophase spherules are put into carbide furnace, hydrogen atmosphere protection, 10 DEG C/min of heating rate is warming up to 1000
DEG C, soaking time 5h.Soft carbon particle after pre- carbonization be crushed and is classified to D50It is 10 μm.Obtained soft carbon particle is being turned round
CVD cladding is carried out with propane in furnace, heating rate is 10 DEG C/min, and temperature of plate is 1000 DEG C, and the cladding time is 8h, before obtaining
Drive body.Presoma is subjected to carbonization treatment, hydrogen atmosphere protection, 10 DEG C/min of heating rate, carburizing temperature is 1300 DEG C, carbonization
Time is 6h；It is sieved with screening machine, obtains soft carbon finished product.
Comparative example 1
By needle coke and hydrogen peroxide, hydrogen peroxide mass fraction is 5%, and the mass ratio of needle coke and hydrogen peroxide is 1:1 in water
It is pre-oxidized in bath agitated kettle, temperature is 70 DEG C, preoxidation time 2h.Needle coke is put into carbide furnace, nitrogen atmosphere
Protection, 2 DEG C/min of heating rate are warming up to 500 DEG C, soaking time 1h.Soft carbon particle after pre- carbonization is subjected to broken be classified to
D50It is 5 μm.Obtained soft carbon particle is subjected to carbonization treatment, nitrogen atmosphere is protected, 2 DEG C/min of heating rate, and carburizing temperature is
800 DEG C, carbonization time 2h.It is sieved with screening machine, obtains soft carbon finished product.
Comparative example 2
Needle coke is put into carbide furnace, nitrogen atmosphere protection, 2 DEG C/min of heating rate is warming up to 500 DEG C, soaking time 1h,
It is carbonized in advance.Soft carbon particle after pre- carbonization be crushed and is classified to D50It is 5 μm.By obtained soft carbon particle in rotary furnace
CVD cladding is carried out with methane, heating rate is 2 DEG C/min, and temperature of plate is 600 DEG C, and the cladding time is 2h, obtains presoma.
Presoma is subjected to carbonization treatment, nitrogen atmosphere protection, 2 DEG C/min of heating rate, carburizing temperature is 800 DEG C, and carbonization time is
2h.It is sieved with screening machine, obtains soft carbon finished product.
Performance test；The negative electrode material that embodiment and comparative example provide is prepared into battery, specific steps are as follows:
In a solvent by negative electrode material, conductive agent and binder 94:2:4 mixed dissolution in mass ratio, control solid content is 50%,
Coated in copper foil current collector, the LiPF6/EC+DMC+EMC (v/v=1:1:1) of cathode pole piece, 1mol/L is made in vacuum drying
Electrolyte, SK diaphragm, lithium piece, shell use the button cell of conventional production process assembly；In Shenzhen Xin Wei Co., Ltd battery
In test macro, test condition are as follows: under room temperature, 1C constant current charge-discharge, charge and discharge blanking voltage 0.01V-1.5V.Test result is shown in
Table 1:
As it can be seen from table 1 the lithium ion battery high power density negative electrode material of the method for the present invention preparation, hence it is evident that improve soft carbon material
Reversible gram volume, for the first time coulombic efficiency and the high rate performance of material.
Claims (6)
1. a kind of lithium ion battery high power density negative electrode material, which is characterized in that including soft carbon matrix, be uniformly wrapped on it is soft
Amorphous conductive carbon coating layer on carbon base body.
2. a kind of lithium ion battery preparation method of high power density negative electrode material, which comprises the following steps:
A1, amorphous carbon material pre-oxidation: amorphous carbon material and hydrogen peroxide are pre-oxidized in stirring in water bath pot, pre-oxidized
Temperature be 70-100 DEG C, preoxidation time be 2-10 h；
A2, amorphous carbon material are carbonized in advance: the pre-oxidation amorphous carbon material obtained after step A1 processing being put into carbide furnace and is heated
Pre- carbonization, using atmosphere protection, 2-10 DEG C of heating rate/min is warming up to 500-1000 DEG C, and soaking time 1-5h obtains pre- carbon
Change soft carbon particle；
A3, it is crushed, classification: the pre- carbonization soft carbon particle that step A2 is obtained is crushed, and is classified to D50It is 5-10 μm, obtains soft
Carbon particle；
A4, gas phase cladding: carrying out CVD cladding with organic carbon source gas in rotary furnace for soft carbon particle obtained in step A3,
It is coated under atmosphere protection and carries out, heating rate is 2-10 DEG C/min, and temperature of plate is 600-1000 DEG C, and the cladding time is 2-
8h obtains presoma；
A5, carbonization, sieving: the presoma progress carbonization treatment that step A4 is obtained, atmosphere protection, 2-10 DEG C of heating rate/
Min, carburizing temperature are 1000-1300 DEG C, carbonization time 2-6h；It is sieved with screening machine, obtains soft carbon finished product.
3. a kind of preparation method of the lithium ion battery according to claim 2 with high power density negative electrode material, feature
It is: in step A1, amorphous carbon material and hydrogen peroxide is subjected to pre- oxygen according to mass ratio for 1:1-5:1 in stirring in water bath pot
Change, wherein hydrogen peroxide mass fraction is 5%-20%；
A kind of preparation method of lithium ion battery high power density negative electrode material according to claim 2, feature exist
In: in step A1, the amorphous carbon material be 2500 DEG C or more graphitizable carbon, the amorphous carbon material be petroleum coke,
One of needle coke, carbon fiber and non-graphitized carbonaceous mesophase spherules or a variety of combinations.
4. a kind of preparation method of the lithium ion battery according to claim 2 with high power density negative electrode material, feature
Be: in step A2 and A5, the carbide furnace can be pushed bat kiln, roller kilns, rotary kiln；
A kind of preparation method of lithium ion battery high power density negative electrode material according to claim 2, feature exist
In: for the atmosphere protection for non-oxidizing atmosphere protection, gas used by the non-oxidizing atmosphere is protected is nitrogen, helium
Any one in gas, argon gas or hydrogen or a variety of combinations.
5. a kind of preparation method of the lithium ion battery according to claim 2 with high power density negative electrode material, feature
Be: in step A3, obtained pre- carbonization soft carbon particle after step A2 processing being crushed, the broken mode used for
Mechanical mill, airflow milling, ball milling；
A kind of preparation method of lithium ion battery high power density negative electrode material according to claim 2, feature exist
In: in step A4, the organic carbon source gas that the gas phase carbon coating treatment process is selected is hydro carbons, and the organic carbon source gas is
In methane, ethylene, acetylene, propane, benzene,toluene,xylene, styrene or phenol any one or at least two group
It closes.
6. a kind of preparation method of lithium ion battery high power density negative electrode material according to claim 2 or 3, special
Sign is: in step A4, it is 3-15% that the gas phase, which coats carbon source covering amount used,.
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| CN114122393A (en) * | 2021-11-11 | 2022-03-01 | 深圳市翔丰华科技股份有限公司 | Preparation method of high-power-density negative electrode material for lithium ion battery |
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