CN107959028A - A kind of carbon nanotubes/application of the spherical micro crystal graphite of Lauxite carbon coating as lithium ion battery negative material - Google Patents
A kind of carbon nanotubes/application of the spherical micro crystal graphite of Lauxite carbon coating as lithium ion battery negative material Download PDFInfo
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- CN107959028A CN107959028A CN201711412270.3A CN201711412270A CN107959028A CN 107959028 A CN107959028 A CN 107959028A CN 201711412270 A CN201711412270 A CN 201711412270A CN 107959028 A CN107959028 A CN 107959028A
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- graphite
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- crystal graphite
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 relates to a kind of carbon nanotubes/application of the spherical micro crystal graphite of Lauxite carbon coating as lithium ion battery negative material, lithium ion battery, negative material are prepared as ion cathode material lithium using spherical microcrystalline graphite material：SBR（Solid content 50%）：CMC：The weight ratio of Super ~ p is 97.5:1.5:2:1, then plus appropriate amount of deionized water reconciles into ginger shape, is coated on copper foil and negative plate is made when drying 12 is small in vacuum drying chamber, the electrolyte of lithium ion battery uses 1MLiPF6/EC+DEC+DMC=1:1:1, membrane is microporous polypropylene membrane, is lithium piece to electrode, battery is assembled into the glove box of closed argon atmosphere.For the lithium ion battery under 0.1C multiplying powers during discharge and recharge, first charge-discharge cycle charging capacity is 390 mAh/g, under 5C multiplying powers during discharge and recharge, after circulation 500 times, and capacity retention ratio 97.2%.
Description
Technical field
It is spherical more particularly, to a kind of carbon nanotubes/Lauxite carbon coating the present invention relates to field of lithium ion battery
Application of the micro crystal graphite as lithium ion battery negative material.
Background technology
Lithium ion battery is a kind of free of contamination green battery succeeded in developing at the end of the 20th century, compared with conventional batteries, tool
There is the advantages that high average discharge volt, volume capacity and quality capacity are all bigger, discharge time length, light weight.Lithium ion two
Primary cell rapid marketization in the case where Carbon Materials are used as the promotion of anode, but lithium ion battery is also deposited while the rapid marketization
In some problems, such as analyse lithium phenomenon in use, occurring in charge and discharge process under cryogenic and cause putting for battery
Decline drastically will occur for some important indicators such as capacitance, capacity retention ratio and cycle life.Current most of solutions
Method be to improve its cryogenic property by replacing low-temperature electrolyte, but while its cryogenic property is met, other performances
But it is difficult to be met, does not tackle the problem at its root.
The theoretical embedding lithium capacity of graphite is 372m Ah/g, it crystallizes complete and has a high orientation, Lithium-ion embeding with
During abjection, 10% or so expansion and contraction can be produced in d002 directions, its layer structure easy quilt in cyclic process
Destroy.In addition electrolyte solvent is inevitably had in cyclic process and is embedded in graphite layers altogether, due to the reduction of organic solvent, big
Gas expansion can be produced under electric current, causes graphite flake layer to peel off, causes active material irreversible loss and solid electrolyte circle
Facial mask (SEI films) constantly destroys and lives again, so as to cause cycle life not good enough.But there is also specific capacity is relatively low, first for graphite
The problems such as efficiency for charge-discharge is relatively low, diffusion velocity of the lithium ion in graphite is slower, in view of the above problems, researcher passes through pyrolysis
The means such as charcoal cladding and the mechanical compound, surface oxidation treatment of nano-carbon material (Carbon fibe or carbon nanotubes etc.) carry out modified graphite,
The chemical property of graphite is effectively improved, but its reversible specific capacity and cyclical stability under high magnification first
Deng still having much room for improvement.
Spherical graphite is that processing, the different fineness of production, likeness in form are modified to graphite surface using Advanced
Oval spherical graphite products.Spheroidal graphite materials are with good electric conductivity, crystallinity is high, cost is low, theoretical embedding lithium capacity
High, the features such as charge and discharge potential is low and flat, can be as the pith of lithium ion battery negative material.
The content of the invention
In order to solve the problems in the prior art, the purpose of the present invention is to, there is provided a kind of carbon nanotubes/Lauxite carbon coating
Application of the spherical micro crystal graphite as lithium ion battery negative material.
The present invention is achieved by the following technical solutions：
A kind of carbon nanotubes/application of the spherical micro crystal graphite of Lauxite carbon coating as lithium ion battery negative material,
Lithium ion battery, anode are prepared as ion cathode material lithium using carbon nanotubes/spherical micro crystal graphite of Lauxite carbon coating
Material：SBR (solid content 50%)：CMC：The weight ratio of Super~p is 97.5:1.5:2:1, then add appropriate amount of deionized water tune
With into ginger shape, it is coated on copper foil and negative plate, the electrolyte of lithium ion battery is made when drying 12 is small in vacuum drying chamber
Using 1MLiPF6/EC+DEC+DMC=1:1:1, membrane is microporous polypropylene membrane, is lithium piece to electrode, in closed argon atmosphere
Glove box in be assembled into battery；
Wherein, the carbon nanotubes/spherical microcrystalline graphite material of Lauxite carbon coating is prepared by following methods：
S1. using micro crystal graphite as raw material, by obtaining spherical crystallite by flotation, pretreatment, shaping, purification processes step
Graphite；
S2. spherical micro crystal graphite step S1 obtained is placed in ultrasonic response kettle, supersonic frequency 50KHz, power
It is 1 by the part by weight of product and Lauxite after 2h is stirred by ultrasonic for the ethanol solution of 2000W, then addition 50%:50,
Lauxite is added, is 1 by the part by weight of curing agent and Lauxite:12 add curing agent, are sufficiently stirred, in ball
Shape micro crystal graphite surface forms the first clad, reacts 4h under the conditions of 500 DEG C, is cooled to room temperature and crosses 300~400 mesh sieves；
S3. product step S2 obtained by weight proportion 1：20 mix with carbon nanotubes so that carbon nanotubes is uniformly wrapped
It is rolled in spherical micro crystal graphite surface；
S4. the product of step S3 is placed in carbide furnace and be carbonized, the temperature of carbide furnace is 1200 DEG C, and carbonization time is
8h, through crushing, sieving after cooling, that is, obtains the spherical micro crystal graphite negative material of carbon nanotubes/Lauxite carbon coating.
Wherein, micro crystal graphite is Chenzhou City Shandong pool graphite powder, its carbon content is 70~80%.
Preferably, the preparation method of the spherical microcrystalline graphite material is as follows：
Y1. pre-process：Using micro crystal graphite as raw material, its dry concentrate is obtained after flotation, is then carried out using cutter pre-
Processing, power 6KW, rotating speed 2000r/min, obtains coarse crushing micro crystal graphite；
Y2. shaping：The coarse crushing micro crystal graphite that step Y1 is obtained carries out processing in small, broken bits in first disintegrator, and first crushes
The rotating speed of machine is 2500r/min, then carries out first time classification, magnetic separation and is classified for second, the first grader and the second classification
The rotating speed of machine is respectively 2000r/min, 1800r/min, obtains spherical graphite initial product；
Y3. purify：The spherical graphite initial product that step Y2 is obtained, after dust removal process, using 40% hydrogen fluorine
Acid solution carries out 2 purified reactions with material in ultrasonic response kettle, and the frequency of ultrasonic response kettle is 50KHz, and power is
The liquid-solid ratio of 1800W, hydrofluoric acid and material is 3:1, reaction temperature is 50 DEG C, reaction time 2h, obtain spherical graphite half into
Product；
Y4. dry：Processing is dried in the spherical graphite semi-finished product that step Y3 is obtained, drying process temperature is 60 DEG C,
Up to spherical graphite final products.
The present invention pre-processes raw material using cutter, and preliminary powder is obtained before micro crystal graphite carries out reforming process
It is broken, be conducive to improve processing efficiency, while the technical process of follow-up shaping unit can also be simplified, so that reaching raising crushes precision
Purpose.
The present invention carries out purified reaction in ultrasonic response kettle, super by rationally controlling with the use of hydrofluoric acid aqueous solution
Acoustic frequency, power, are not only able to accelerate purified reaction, promote the cleaning of impurity in spherical graphite to remove, moreover it is possible to utilize ultrasonic wave
Cavitation cause the surface of spherical graphite to tend to be smooth, effectively reduce spherical graphite specific surface area, improve spherical graphite
Purity.
The present invention carries out coarse crushing using cutter to the dry concentrate of micro crystal graphite, while is purified in ultrasonic response kettle
Reaction, solve in a creative way crushed in spherical graphite preparation process be not thorough, the spherical graphite sphericity prepared it is not high, pure
Spend the problem of low so that micro crystal graphite not only forms Mechanical Crushing, moreover it is possible to produce physics collision process, micro crystal graphite raw material obtains
It is effective to crush and purification, and preparation process is simple, the spherical graphite specific surface area prepared is significantly reduced, tap density
It is improved.
Compared with prior art, the invention has the advantages that：
The present invention prepares spherical microcrystalline graphite material using micro crystal graphite, and Chinese micro crystal graphite large storage capacity is cheap,
It is mostly low value-added utilization, the present invention provides a kind of high value added utilization approach for micro crystal graphite.
The preparation side of the spherical micro crystal graphite negative material of the carbon nanotubes of offer provided by the invention/Lauxite carbon coating
Method is modified spherical micro crystal graphite surface using ultrasonic wave, while forms uniform clad in graphite surface, carbon is received
Mitron is wrapped in spherical graphite surface, and grid structure is formed on spherical micro crystal graphite surface, generates class bobbles shape, and enhancing surface is strong
Degree, and gives full play to the excellent performance of carbon nanotubes, improve the electric conductivity of negative material, discharge capacity, anti-decay property and
Excellent multiplying power property, discharge capacity is up to 390 mAh/g first.
The present invention's synthesizes a kind of novel anode material by secondary cladding process, lithium ion battery is filled under cryogenic
Analysis lithium phenomenon is reduced during electric discharge, thus reduce battery at low temperature in charge and discharge process Li+ irreversible loss, so as to fulfill low
The normal work of lithium ion battery under the conditions of temperature, while ensure that when lithium ion battery works at low temperature with higher electric discharge
Capacity.
Preparation process of the present invention is simple, and lithium storage content is high, and voltage platform is good, cheap, is followed repeatedly filling-discharging
It will not be collapsed after ring, good cycle.
Embodiment
The present invention is further illustrated with reference to specific embodiment.Unless stated otherwise, used in the embodiment of the present invention
Routinely raw material purchased in market and conventional use of method, used equipment routinely set for this area for this area for raw material and method
It is standby.
Embodiment 1
The present embodiment is a kind of spherical micro crystal graphite of carbon nanotubes Lauxite carbon coating as negative electrode of lithium ion battery material
The application of material, the present embodiment are used born using carbon nanotubes/spherical micro crystal graphite of Lauxite carbon coating as lithium ion first
Pole material prepares lithium ion battery, negative material：SBR (solid content 50%)：CMC：The weight ratio of Super~p is 97.5:
1.5:2:1, then plus appropriate amount of deionized water reconciles into ginger shape, is coated on copper foil and in dry 12 small when systems in vacuum drying chamber
Into negative plate, the electrolyte of lithium ion battery uses 1MLiPF6/EC+DEC+DMC=1:1:1, membrane is microporous polypropylene membrane,
It is lithium piece to electrode, battery is assembled into the glove box of closed argon atmosphere；
Wherein, carbon nanotubes/spherical microcrystalline graphite material of Lauxite carbon coating is prepared by following methods：
S1. using micro crystal graphite as raw material, by obtaining spherical crystallite by flotation, pretreatment, shaping, purification processes step
Graphite；Wherein, micro crystal graphite is Chenzhou City Shandong pool graphite powder, its carbon content is 70~80%；
S2. spherical micro crystal graphite step S1 obtained is placed in ultrasonic response kettle, supersonic frequency 50KHz, power
It is 1 by the part by weight of product and Lauxite after 2h is stirred by ultrasonic for the ethanol solution of 2000W, then addition 50%:50,
Lauxite is added, is 1 by the part by weight of curing agent and Lauxite:12 add curing agent, are sufficiently stirred, in ball
Shape micro crystal graphite surface forms the first clad, reacts 4h under the conditions of 500 DEG C, is cooled to room temperature and crosses 300~400 mesh sieves；
S3. product step S2 obtained by weight proportion 1：20 mix with carbon nanotubes so that carbon nanotubes is uniformly wrapped
It is rolled in spherical micro crystal graphite surface；
S4. the product of step S3 is placed in carbide furnace and be carbonized, the temperature of carbide furnace is 1200 DEG C, and carbonization time is
8h, through crushing, sieving after cooling, that is, obtains the spherical micro crystal graphite negative material of carbon nanotubes/Lauxite carbon coating.
Wherein, the spherical microcrystalline graphite material is prepared by following methods：
Y1. pre-process：Using micro crystal graphite as raw material, its dry concentrate is obtained after flotation, is then carried out using cutter pre-
Processing, power 6KW, rotating speed 2000r/min, obtains coarse crushing micro crystal graphite；
Y2. shaping：The coarse crushing micro crystal graphite that step Y1 is obtained carries out processing in small, broken bits in first disintegrator, and first crushes
The rotating speed of machine is 2500r/min, then carries out first time classification, magnetic separation and is classified for second, the first grader and the second classification
The rotating speed of machine is respectively 2000r/min, 1800r/min, obtains spherical graphite initial product；
Y3. purify：The spherical graphite initial product that step Y2 is obtained, after dust removal process, using 40% hydrogen fluorine
Acid solution carries out 2 purified reactions with material in ultrasonic response kettle, and the frequency of ultrasonic response kettle is 50KHz, and power is
The liquid-solid ratio of 1800W, hydrofluoric acid and material is 3:1, reaction temperature is 50 DEG C, reaction time 2h, obtain spherical graphite half into
Product；
Y4. dry：Processing is dried in the spherical graphite semi-finished product that step Y3 is obtained, drying process temperature is 60 DEG C,
Up to spherical graphite final products.
The specific surface area of the spherical microcrystalline graphite material obtained in the present embodiment is 2.6m2/g。
Circulation is carried out to battery using new prestige (Neware) charge-discharge test instrument to test with high rate performance, chemical property test
Voltage range is 1.7~2.8V, and current density 0.1C, test temperature is 25 DEG C.Electrochemical property test result is as follows：
The lithium ion battery carries out discharge and recharge under 0.1C multiplying powers and charge-discharge test is carried out under 5C multiplying powers, in 0.1C
Under multiplying power during discharge and recharge, first charge-discharge cycle charging capacity is 390mAh/g, under 5C multiplying powers during discharge and recharge, in circulation 500
After secondary, capacity retention ratio 97.2%.
Comparative example 1
Comparative example 1 is with 1 difference of embodiment：Carbon nanotubes/spherical crystallite of Lauxite carbon coating in comparative example 1
In the preparation method step S2 of graphite material, ultrasonic response kettle is not provided with.
The specific surface area of the spherical microcrystalline graphite material obtained in this comparative example is 2.6m2/g。
Circulation is carried out to battery using new prestige (Neware) charge-discharge test instrument to test with high rate performance, chemical property test
Voltage range is 1.7~2.8V, and current density 0.1C, test temperature is 25 DEG C.Electrochemical property test result is as follows：
Mixed expanded material made from comparative example 1 is assembled into lithium ion battery and discharge and recharge is carried out under 0.1C multiplying powers and in 5C
Charge-discharge test is carried out under multiplying power, under 0.1C multiplying powers during discharge and recharge, first charge-discharge cycle charging capacity is 300mAh/g,
Under 5C multiplying powers during discharge and recharge, after circulation 500 times, capacity retention ratio 90.8%.
The present invention illustrates the detailed process equipment of the present invention and processing step, people in the art by above-described embodiment
Member is it should be appreciated that the present invention limits from above-described embodiment, and the above embodiments and description only describe the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, this is to this area
It is it will be apparent that these changes and improvements all fall within the protetion scope of the claimed invention for technical staff.
Claims (2)
1. a kind of carbon nanotubes/application of the spherical micro crystal graphite of Lauxite carbon coating as lithium ion battery negative material, its
It is characterized in that, lithium ion is prepared as ion cathode material lithium using carbon nanotubes/spherical micro crystal graphite of Lauxite carbon coating
Battery, negative material：SBR（Solid content 50%）：CMC：The weight ratio of Super ~ p is 97.5:1.5:2:1, then plus it is appropriate go from
Sub- water reconciles into ginger shape, is coated on copper foil and negative plate is made when drying 12 is small in vacuum drying chamber, lithium ion battery
Electrolyte uses
1MLiPF6/EC+DEC+DMC=1:1:1, membrane is microporous polypropylene membrane, is lithium piece to electrode, in closed argon atmosphere
Battery is assembled into glove box；
Wherein, the carbon nanotubes/spherical microcrystalline graphite material of Lauxite carbon coating is prepared by following methods：
S1. using micro crystal graphite as raw material, by obtaining spherical microlite by flotation, pretreatment, shaping, purification processes step
Ink；
S2. spherical micro crystal graphite step S1 obtained is placed in ultrasonic response kettle, supersonic frequency 50KHz, and power is
2000 W, then add 50% ethanol solution, are 1 by the part by weight of product and Lauxite after 2 h are stirred by ultrasonic:50,
Lauxite is added, is 1 by the part by weight of curing agent and Lauxite:12 add curing agent, are sufficiently stirred, spherical
Micro crystal graphite surface forms the first clad, and 4 h are reacted under the conditions of 500 DEG C, is cooled to room temperature and crosses 300 ~ 400 mesh sieves；
S3. product step S2 obtained by weight proportion 1：20 mix with carbon nanotubes so that carbon nanotubes is uniformly wrapped in
Spherical micro crystal graphite surface；
S4. the product of step S3 being placed in carbide furnace and be carbonized, the temperature of carbide furnace is 1200 DEG C, and carbonization time is 8 h,
Through crushing, sieving after cooling, that is, obtain the spherical micro crystal graphite negative material of carbon nanotubes/Lauxite carbon coating；
Wherein, micro crystal graphite is Chenzhou City Shandong pool graphite powder, its carbon content is 70 ~ 80%.
2. carbon nanotubes/spherical micro crystal graphite of Lauxite carbon coating is as negative electrode of lithium ion battery according to claim 1
The application of material, it is characterised in that the preparation method of the spherical micro crystal graphite is as follows：
Y1. pre-process：Using micro crystal graphite as raw material, its dry concentrate is obtained after flotation, is then pre-processed using cutter,
Power is 6 KW, and rotating speed is 2000 r/min, obtains coarse crushing micro crystal graphite；
Y2. shaping：The coarse crushing micro crystal graphite that step Y1 is obtained carries out processing in small, broken bits in first disintegrator, first disintegrator
Rotating speed is 2500 r/min, then carries out first time classification, magnetic separation and second is classified, the first grader and the second grader
Rotating speed is respectively 2000 r/min, 1800 r/min, obtains spherical graphite initial product；
Y3. purify：The spherical graphite initial product that step S2 is obtained, after dust removal process, using 40% hydrofluoric acid solution
2 purified reactions are carried out in ultrasonic response kettle with material, the frequency of ultrasonic response kettle is 50KHz, and power is 1800 W,
The liquid-solid ratio of hydrofluoric acid and material is 3:1, reaction temperature is 50 DEG C, and the reaction time is 2 h, obtains spherical graphite semi-finished product；
Y4. dry：Processing is dried in the spherical graphite semi-finished product that step Y3 is obtained, drying process temperature is 60 DEG C, to obtain the final product
Spherical graphite final products.
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| CN110416497A (en) * | 2019-06-06 | 2019-11-05 | 湖南中科星城石墨有限公司 | A kind of high capacity fast charging type micro crystal graphite negative electrode material and preparation method thereof |
| CN112670463A (en) * | 2020-04-16 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Graphite negative electrode material and preparation method and application thereof |
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