CN105789574B - A kind of preparation method of high temperature modification graphite negative material of lithium ion battery - Google Patents
A kind of preparation method of high temperature modification graphite negative material of lithium ion battery Download PDFInfo
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- CN105789574B CN105789574B CN201610127132.XA CN201610127132A CN105789574B CN 105789574 B CN105789574 B CN 105789574B CN 201610127132 A CN201610127132 A CN 201610127132A CN 105789574 B CN105789574 B CN 105789574B
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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
- 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
- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
Abstract
The present invention discloses a kind of preparation method of high temperature modification graphite negative material of lithium ion battery and weighs graphite and solvent, ammonium hydroxide, its ratio be 1g first:0.5‑2L:2 10mL, are added in homogenizer, and carrying out 0.5~1h of dispersion using 500~2000r/min of rotating speed obtains mixing slurry；Then, titanate esters are added dropwise, the ratio between the mixing slurry and titanate esters are 1g:2‑5mL；Then; 5 10h are reacted in 40 80 DEG C of water-baths after adding titanate esters; it is cleaned repeatedly 45 times with water, ethyl alcohol after the completion of reaction; finally; it is dried in 80 100 DEG C of drying box; drying, which is placed in atmosphere protection stove, to be sintered, and is risen to 400~800 DEG C with the heating rate of 2~25 DEG C/min and is kept the temperature 4~18 hours, obtains high temperature modification graphite negative material of lithium ion battery.
Description
Technical field
The present invention relates to lithium ion battery negative material field technologies, are especially to provide a kind of high temperature modification lithium ion battery stone
The preparation method of black negative material.
Background technology
With the continuous intensification of global energy crisis, in increasingly exhausted and the atmosphere pollution, Global Temperature of petroleum resources
The harm aggravation risen, development clean energy resource are imperative.In new energy development, with operating voltage height, energy density is big, puts
Piezoelectric voltage is steady, have extended cycle life and the lithium ion battery of advantages of environment protection finds broad application.Negative material is to comment
One of the key factor of valence lithium ion battery comprehensive performance quality.It is mainly stone that the lithium cell cathode material used is commercialized at present
Ink, graphite have de-/embedding current potential (0~0.25V vs Li/Li+) of relatively low lithium, capacity high (372mAh/g), it is resourceful and
Lower-price characteristic.With the development of social productive forces and being constantly progressive for science and technology, research improves lithium ion battery
High-temperature behavior can necessitate suitable for exceedingly odious condition.The high-temperature behavior of battery refers to that lithium ion battery is being situated between
It is played in the electrical property in room temperature (25 DEG C) and safe handling temperature upper limit (90 DEG C) range, including cycle performance, storage performance,
High rate performance, security performance etc..In general, lithium ion battery is deposited when use environment temperature is up to 85 DEG C or more
Storage, battery will quickly flatulence and cannot use.
Invention content
In view of this, the present invention is in view of the existing deficiencies of the prior art, the purpose of the present invention is to provide provide it is a kind of at
The preparation method of this high temperature modification graphite negative material of lithium ion battery cheap, simple for process, obtained graphite cathode material tool
There is good solvent resistance, and remains excellent electric conductivity.Meanwhile the service life under battery high-temperature is increased, it improves
Battery high-temperature storage performance and security performance.
To achieve the above object, the present invention is using following technical solution：A kind of high temperature modification graphite negative electrode of lithium ion battery
The preparation method of material, including have the following steps：
First, graphite and solvent, ammonium hydroxide are weighed, its ratio be 1g:0.5-2L:2-10mL is added in homogenizer,
0.5~1h of dispersion, which is carried out, using 500~2000r/min of rotating speed obtains mixing slurry；Then, titanate esters are added dropwise, this is mixed
It is 1g to close the ratio between slurry and titanate esters:2-5mL；Then, 5-10h is reacted in 40-80 DEG C of water-bath after adding titanate esters, reaction is completed
It is cleaned 4-5 times with water, ethyl alcohol, finally, is dried in 80-100 DEG C of drying box repeatedly afterwards, drying is placed in atmosphere protection stove
Be sintered, with the heating rate of 2~25 DEG C/min rise to 400~800 DEG C and keep the temperature 4~18 hours, obtain high temperature modification lithium from
Sub- battery graphite cathode material.
As a preferred embodiment, the graphite is natural graphite, and purity is 99.999 or more, granularity d50=10-
20um。
As a preferred embodiment, the solvent is at least one of ethyl alcohol, propyl alcohol, butanol, purity 99.999
More than.
As a preferred embodiment, the ammoniacal liquor mass concentration is 25%.
As a preferred embodiment, the titanate esters are one in tetraethyl titanate, metatitanic acid orthocarbonate or butyl titanate
Kind.
As a preferred embodiment, the protective atmosphere used in the atmosphere protection stove is selected from helium, nitrogen, argon gas, two
At least one of carbonoxide.
The present invention has clear advantage and advantageous effect compared with prior art, specially：
1, one layer " shell " containing titanium dioxide is coated in graphite surface, titanium dioxide can subtract electrolyte solvent resistance
Few erosion of the electrolyte to " core "-graphite, reduces the stripping of graphite flake layer, effectively ensure that battery electrochemical stability and
Security performance is improved.Meanwhile can ensure " shell " thickness in 10nm by adjusting the addition of ammonium hydroxide, in this way in battery
High temperature cyclic performance and storage performance be improved, battery high rate performance can be unaffected.In addition, ultrathin nanometer coats
" shell " layer can ensure that electric conductivity is excellent, to reduce the battery polarization and internal resistance that " shell " layer is brought.
2, the method for the present invention is simple to operate, and production equipment is few, easy to utilize to further reduce the cost,
Suitable for large-scale production.
Specific implementation mode
Embodiment 1
A kind of preparation method of high temperature modification graphite negative material of lithium ion battery weighs graphite and solvent, ammonium hydroxide first,
Its ratio be 1g:0.5L:2mL is added in homogenizer, and carrying out dispersion 1h using rotating speed 500r/min obtains mixing slurry；
Then, titanate esters are added dropwise, the ratio between the mixing slurry and titanate esters are 1g:2mL；Then, it adds after titanate esters at 80 DEG C
5h is reacted in water-bath, is cleaned 4 times with water, ethyl alcohol after the completion of reaction, finally, is dried in 80 DEG C of drying box, after drying repeatedly
It is placed in atmosphere protection stove and is sintered, 400 DEG C are risen to the heating rate of 2 DEG C/min and keep the temperature 18 hours, obtain high temperature modification
Graphite negative material of lithium ion battery.
The graphite is natural graphite, and purity is 99.999 or more, granularity d50=10-20um.
The solvent is at least one of ethyl alcohol, propyl alcohol, butanol, and purity is 99.999 or more.
The ammoniacal liquor mass concentration is 25%.
The titanate esters are one kind in tetraethyl titanate, metatitanic acid orthocarbonate or butyl titanate.
The protective atmosphere used in the atmosphere protection stove in helium, nitrogen, argon gas, carbon dioxide at least one
Kind.
Embodiment 2
A kind of preparation method of high temperature modification graphite negative material of lithium ion battery weighs graphite and solvent, ammonium hydroxide first,
Its ratio be 1g:2L:10mL is added in homogenizer, and carrying out dispersion 0.5h using rotating speed 2000r/min is mixed
Slurry；Then, titanate esters are added dropwise, the ratio between the mixing slurry and titanate esters are 1g:5mL；Then, it adds after titanate esters 80
5h is reacted in DEG C water-bath, is cleaned 4 times with water, ethyl alcohol after the completion of reaction, finally, is dried in 100 DEG C of drying box repeatedly, is dried
It is placed in atmosphere protection stove and is sintered, 800 DEG C are risen to the heating rate of 25 DEG C/min and keep the temperature 4 hours, obtain high temperature
Type graphite negative material of lithium ion battery.
The graphite is natural graphite, and purity is 99.999 or more, granularity d50=10-20um.
The solvent is at least one of ethyl alcohol, propyl alcohol, butanol, and purity is 99.999 or more.
The ammoniacal liquor mass concentration is 25%.
The titanate esters are one kind in tetraethyl titanate, metatitanic acid orthocarbonate or butyl titanate.
The protective atmosphere used in the atmosphere protection stove in helium, nitrogen, argon gas, carbon dioxide at least one
Kind.
Embodiment 3
A kind of preparation method of high temperature modification graphite negative material of lithium ion battery weighs graphite and solvent, ammonium hydroxide first,
Its ratio be 1g:1L:6mL is added in homogenizer, and carrying out dispersion 0.7h using rotating speed 1000r/min obtains mixing slurry；
Then, titanate esters are added dropwise, the ratio between the mixing slurry and titanate esters are 1g:3mL；Then, it adds after titanate esters at 50 DEG C
60h is reacted in water-bath, is cleaned 4 times with water, ethyl alcohol after the completion of reaction, finally, is dried in 100 DEG C of drying box repeatedly, is dried
It is placed in atmosphere protection stove and is sintered, 600 DEG C are risen to the heating rate of 15 DEG C/min and keep the temperature 8 hours, obtain high temperature
Type graphite negative material of lithium ion battery.
The graphite is natural graphite, and purity is 99.999 or more, granularity d50=10-20um.
The solvent is at least one of ethyl alcohol, propyl alcohol, butanol, and purity is 99.999 or more.
The ammoniacal liquor mass concentration is 25%.
The titanate esters are one kind in tetraethyl titanate, metatitanic acid orthocarbonate or butyl titanate.
The protective atmosphere used in the atmosphere protection stove in helium, nitrogen, argon gas, carbon dioxide at least one
Kind.
Embodiment 4
A kind of preparation method of high temperature modification graphite negative material of lithium ion battery weighs graphite and solvent, ammonium hydroxide first,
Its ratio be 1g:1.5L:8mL is added in homogenizer, and carrying out dispersion 0.7h using rotating speed 1500r/min is mixed
Slurry；Then, titanate esters are added dropwise, the ratio between the mixing slurry and titanate esters are 1g:4mL；Then, it adds after titanate esters 70
7h is reacted in DEG C water-bath, is cleaned 4 times with water, ethyl alcohol after the completion of reaction, finally, is dried in 90 DEG C of drying box repeatedly, is dried
It is placed in atmosphere protection stove and is sintered, 700 DEG C are risen to the heating rate of 20 DEG C/min and keep the temperature 7 hours, obtain high temperature
Type graphite negative material of lithium ion battery.
The graphite is natural graphite, and purity is 99.999 or more, granularity d50=10-20um.
The solvent is at least one of ethyl alcohol, propyl alcohol, butanol, and purity is 99.999 or more.
The ammoniacal liquor mass concentration is 25%.
The titanate esters are one kind in tetraethyl titanate, metatitanic acid orthocarbonate or butyl titanate.
The protective atmosphere used in the atmosphere protection stove in helium, nitrogen, argon gas, carbon dioxide at least one
Kind.
Comparative example 1
The modified natural graphite material obtained using pitch as covering material.
Electrochemical property test is carried out to foregoing individual embodiments and comparative example below：
It is electric with half for the performance of the lithium ion battery negative material of detection ionic liquid coated graphite negative material of the present invention
Pond test method test, with the negative material of the above embodiment and comparative example: SBR (solid content 50%): CMC: Super-p=
95.5: 2: 1.5: 1 (weight ratio) adds appropriate amount of deionized water reconciliation pulp, is coated on copper foil and in dry in vacuum drying chamber
Negative plate is made within dry 12 hours, electrolyte is 1M LiPF6/EC+DEC+DMC=1: 1: 1, and microporous polypropylene membrane is diaphragm, to electricity
Extremely lithium piece is assembled into battery.Constant current charge-discharge experiment is carried out in LAND battery test systems, charging/discharging voltage is limited in 0.01
~3.0V, the charge and discharge electric cabinet computerizedd control carry out the acquisition and control of data, test temperature：25 DEG C and 60 DEG C.It obtains
Data are as shown in table 1 below.
The negative material performance that table 1 lists different embodiment and comparative examples compares.
As it can be seen from table 1 titanium dioxide " shell " layer be added greatly improved battery high temperature cyclic performance and
High-temperature storage performance.It can be seen that using using invention increases the service lifes under battery high-temperature, battery high-temperature storage is improved
Performance and security performance.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore every any trickle amendment, equivalent variations and modification made to the above embodiment according to the technical essence of the invention, still
Belong in the range of technical solution of the present invention.
Claims (6)
1. a kind of preparation method of high temperature modification graphite negative material of lithium ion battery, it is characterised in that：Including having the following steps：
First, graphite and solvent, ammonium hydroxide are weighed, its ratio be 1g:0.5-2L:2-10mL is added in homogenizer, is used
500~2000r/min of rotating speed carries out 0.5~1h of dispersion and obtains mixing slurry；Then, titanate esters are added dropwise, the mixing slurry
It is 1g with the ratio between titanate esters:2-5mL；Then, 5-10h is reacted in 40-80 DEG C of water-bath after adding titanate esters, is used after the completion of reaction
Water, ethyl alcohol clean 4-5 times repeatedly, finally, are dried in 80-100 DEG C of drying box, and drying, which is placed in atmosphere protection stove, to be carried out
Sintering rises to 400~800 DEG C with the heating rate of 2~25 DEG C/min and keeps the temperature 4~18 hours, obtains high temperature modification lithium-ion electric
Pond graphite cathode material.
2. a kind of preparation method of high temperature modification graphite negative material of lithium ion battery according to claim 1, it is characterised in that：
The graphite is natural graphite, and purity is 99.999% or more, d50=10-20 μm of granularity.
3. a kind of preparation method of high temperature modification graphite negative material of lithium ion battery according to claim 1, it is characterised in that：
The solvent is at least one of ethyl alcohol, propyl alcohol, butanol, and purity is 99.999% or more.
4. a kind of preparation method of high temperature modification graphite negative material of lithium ion battery according to claim 1, it is characterised in that：
The ammoniacal liquor mass concentration is 25%.
5. a kind of preparation method of high temperature modification graphite negative material of lithium ion battery according to claim 1, it is characterised in that：
The titanate esters are one kind in tetraethyl titanate, metatitanic acid orthocarbonate or butyl titanate.
6. a kind of preparation method of high temperature modification graphite negative material of lithium ion battery according to claim 1, it is characterised in that：
The protective atmosphere used in the atmosphere protection stove is selected from least one of helium, nitrogen, argon gas, carbon dioxide.
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Address after: 20 J unit, C building, 9 blocks, 1 Energy Science Park, Longhua Road, Longhua District, Shenzhen, Guangdong, 518131 Applicant after: Shenzhen City Cheung Polytron Technologies Inc. Fenghua Applicant after: DONGGUAN XFH BATTERY MATERIAL CO.,LTD. Applicant after: FUJIAN XFH NEW ENERGY MATERIALS Co.,Ltd. Address before: 518000 room 6, building 1, 30 District, 2 Science and Technology Park, 603 science Road, Nanshan District, Guangdong, Shenzhen Applicant before: Shenzhen Xiangfenghua Technology Co.,Ltd. Applicant before: DONGGUAN XFH BATTERY MATERIAL CO.,LTD. Applicant before: FUJIAN XFH NEW ENERGY MATERIALS Co.,Ltd. |
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