CN108666556A - A kind of technique preparing ion cathode material lithium using Nano carbon balls - Google Patents
A kind of technique preparing ion cathode material lithium using Nano carbon balls Download PDFInfo
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- CN108666556A CN108666556A CN201810527220.8A CN201810527220A CN108666556A CN 108666556 A CN108666556 A CN 108666556A CN 201810527220 A CN201810527220 A CN 201810527220A CN 108666556 A CN108666556 A CN 108666556A
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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
- H01M4/364—Composites as mixtures
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 techniques preparing ion cathode material lithium using Nano carbon balls, which is characterized in that includes the following steps：Silica flour and glass putty are added in n-hexane and mix by ball milling, and the weight ratio of the n-hexane, silica flour and glass putty is 26.4:5:1, it is added in ball-grinding machine and is uniformly mixed after mixing, add nano carbon microsphere and carry out secondary ball milling until silica flour, glass putty and nano carbon microsphere are uniformly mixed, the weight ratio of nano carbon microsphere and glass putty is 15:1；The mixture of silica flour, glass putty, nano carbon microsphere and n-hexane is pyrolyzed by high temperature pyrolysis under inert gas protection, and pyrolysis temperature is 200 205 DEG C, and pyrolysis time is 12 hours, obtained negative material.Preparation method of the present invention is simple, and raw material is easy to get, and conductivity is high, lithium ion diffusion coefficient is larger, service life is longer and of low cost, good cycle, is conducive to mass produce.
Description
Technical field
The present invention relates to battery material technical fields, and in particular to a kind of to prepare ion cathode material lithium using Nano carbon balls
Technique.
Background technology
Negative material is one of core component of lithium ion battery, close to the safety of lithium battery, cycle life and energy
Degree has a major impact.Graphite is the main Types of current commercial lithium cell negative pole material, collection conductivity height, lithium ion diffusion coefficient
The advantages such as larger, service life is longer and of low cost are in one, global market share nearly 90%.But the lower theory of graphite
Embedding lithium capacity（372 mAh/g）It has become and restricts the bottleneck that capacity of lithium ion battery greatly improves, and stability also needs to be carried
It is high.Such as silicon substrate and Zr-based materials non-carbon negative material theoretical capacity that new development goes out can reach 1000mAh/g, but there is cycle
The shortcomings of poor performance, need to be used in mixed way with carbon material.
In recent years, the experimental results show to carry out nanosizing and porous to carbon material, can effectively improve carbon material
Embedding lithium capacity.Nanosizing can provide the specific surface area of bigger for carbonaceous material and be touched to increase the knot between electrode and electrolyte,
So that reaction active site increases, promote the generation of electrode reaction, the polarization loss in charge and discharge process is reduced, to improve battery
Capacity.Nano carbon balls, carbon nanotube, carbon nano-fiber and nano-graphene etc. can all make battery capacity super as cathode of lithium battery
Cross the embedding lithium Capacity Theory value of graphite.Such as the graphene that laboratory is prepared can make battery charging and discharging capacity reach 700-900
mAg/g.Form a large amount of mesoporous nanos in carbon material, lithium ion will be not only embedded between carbon-coating when charging, while be also embedded in
In nano grade pore, charge/discharge capacity is made to be far above theoretical specific capacity.For example, to interphase carbon ball（MCMB）Carry out special thermal treatment
After pore-creating, reversible charge/discharge capacity can be made to be improved to 750 mAg/g by 200 mAg/g.
There are many method that porous and nanosizing are carried out to carbon material, such as template and explosion method are used equally for pore-creating,
The nanosizing of carbon material then may be implemented in arc discharge method, hydro-thermal method, chemical vapour deposition technique and template etc..Although passing through this
A little methods have prepared the carbon negative pole material of the embedding lithium capacity of serial height in laboratory, but are deposited when pushing extensive industrialization to
In certain problem.First, the above method needs the harsh conditions such as high temperature, high pressure, vacuum, product cost higher mostly.Secondly,
These synthetic methods often relate to using and discharging for acid, alkali, organic matter and heavy metal ion, are unsatisfactory for wanting for pollution-free industry
It asks.
By carbon material structure spheroidization, porous, the stability of carbon negative pole material can be effectively improved：Graphite anisotropy is very
Height is also easy to produce graphite flake swelling during embedding and removing, collapses, thus stability is very in rapid large-current charge and discharge
Low, there are great security risks.This makes graphite cathode be difficult to obtain large-scale application on lithium-ion-power cell.By carbon
After material structure ball-typeization reduces anisotropy, this can be effectively solved the problems, such as.Such as MCMB is that overall appearance is spherical in shape
Micron order carbon material is conducive to lithium ion from all directions of ball are embedded and deintercalation since bead has laminar structured, can be with
It solves the problems, such as that graphite anisotropy is higher, obtains application on lithium-ion-power cell.But the embedding lithium capacity of MCMB is relatively low, about
For 200 mAg/g.Its capacity is further increased, need to be graphitized, the after-treatment that pore-creating etc. is complicated, it is with high costs.Carbon
Its stability can also be improved after material porous.The presence of hole can provide buffering section for carbon volume change, play " gas
The effect of pad protection ", therefore be also the effective means for effectively improving carbon in high current charge-discharge condition stability inferior.
In conclusion as can carrying out nanosizing, porous and ball-type to carbon material simultaneously, being expected to develop has height embedding
The lithium ion battery negative material of lithium capacity and high stability.But have the new carbon of above structure since technique is numerous at present
Again, cost is high, rests on laboratory pilot stage mostly.This develops out one kind there is an urgent need to us and is easily achieved on a large scale
Low-cost industrial produces, and environmentally protective method has the lithium-ion negative pole of high embedding lithium capacity and high stability novel to prepare
Carbon material.
Invention content
To solve the above problems, the present invention provides, a kind of preparation method is simple, and raw material is easy to get, and conductivity is high, lithium ion expands
Scattered coefficient is larger, service life is longer and of low cost, good cycle, is conducive to a kind of of large-scale production and utilizes carbon nanometer
The technique that ball prepares ion cathode material lithium.
Technical scheme of the present invention：
A kind of technique being prepared ion cathode material lithium using Nano carbon balls, is included the following steps：
Ball milling：Silica flour and glass putty are added in n-hexane and mixed, the weight ratio of the n-hexane, silica flour and glass putty is 26.4:5:
1, it is added in ball-grinding machine and is uniformly mixed after mixing, add nano carbon microsphere and carry out secondary ball milling until silica flour, glass putty
It is uniformly mixed with nano carbon microsphere, the weight ratio of nano carbon microsphere and glass putty is 15:1；
High temperature pyrolysis：The mixture of silica flour, glass putty, nano carbon microsphere and n-hexane is pyrolyzed under inert gas protection, pyrolysis temperature
Degree is 200-205 DEG C, and pyrolysis time is 1-2 hours, obtained negative material.
Preferably, the preparation process of the nano carbon microsphere includes the following steps：
（1）Electrochemical treatments：Using graphite cake as anode electrode plate, using inert metal plate as cathode electrode plate, with the aqueous solution of salt
For electrolyte, commutated direct current electrolysis is added；
（2）Adjust pH：The pH value of active nano carbon ball colloidal sol is adjusted with 50% dilute sulfuric acid or ammonium hydroxide, it is 7 to adjust pH；
（3）Washing：Through high-purity water washing, the high purity water of washing and the mass ratio of electrolyte are 12:1, the high purity water is average
It is divided into three parts to be washed, carbon ball is obtained after washing, the carbon ball is dried through ultrasonic echography after ultrasonic,
60 DEG C of vacuum dryings obtain drying carbon ball；
（4）Surface treatment：Drying carbon ball impregnated with glacial acetic acid, then use ultrasonic echography, ultrasound after with 99.5% ethyl alcohol
It is washed, average to wash in three times, glacial acetic acid：99.5% ethyl alcohol：The mass ratio for drying carbon ball is 210:158:1,60 after washing
DEG C vacuum drying is to get nano carbon microsphere.
Preferably, step（1）Decomposition voltage is 36V, and electric current 10A, electrolysis time is 24-28 hours, obtains activity and receives
The mass ratio of rice carbon ball colloidal sol, the anode electrode plate and electrolyte is 1:2.
Preferably, the step（1）The aqueous solution of the salt is sodium-chloride water solution, potassium chloride solution, potassium sulfate water
Solution or aqueous sodium persulfate solution, the mass concentration of salt is 1% in the aqueous solution of the salt.
Preferably, the inert gas is argon gas.
Preferably, step（3）With（4）Ultrasonic echography, ultrasonic activation power density are 0.35w/cm2, vibration frequency
20000Hz, ultrasonic time are 1-2 hours.
Preferably, the purity of the n-hexane is 99%.
Preferably, a diameter of 200-500nm of the nano carbon microsphere.
Preferably, the specification of the silica flour is not more than 25 μm, and the specification of the glass putty is not more than 25 μm.
Beneficial effects of the present invention：
Preparation method of the present invention is simple, and raw material is easy to get, conductivity is high, lithium ion diffusion coefficient is larger, service life is longer and at
This cheap, good cycle, is conducive to mass produce.The raw materials used in the present invention is easy, obtains and utilizes abrasive body by first ball milling
It is impacted and abrasive action makes silica flour and glass putty are uniformly mixed in n-hexane, it is secondary to add active material nano carbon microsphere
Ball milling is conducive to prepare ion cathode material lithium in next step finally so that silica flour, glass putty and nano carbon microsphere are uniformly mixed；By silicon
Powder, glass putty, nano carbon microsphere and n-hexane lead to argon gas protection, and pyrolysis temperature is 200-205 DEG C, and pyrolysis time is 1-2 hours, high temperature
Pyrolysis makes wherein solvent volatilization, obtained blocky negative material.
Nano carbon balls impurity prepared by the nano carbon microsphere of the present invention is few, using the power characteristic and cavitation of ultrasonic wave,
The physicochemical characteristic for changing nano carbon microsphere, also can further remove the micro impurity being wherein mingled with, realize that its purity further carries
High and active humidification.In order to increase the activity and dispersibility of nano carbon microsphere, carried out at surface using glacial acetic acid and ethyl alcohol
Reason and modification, control its pattern, crystal form and size, realize its controllable preparation and the raising of stability.It will be for surface treatment
Glacial acetic acid and ethyl alcohol make its volatilization by way of drying, obtain pure active nano carbon ball, are received using produced by the invention
Rice carbon ball prepares that ion cathode material lithium conductivity is high, lithium ion diffusion coefficient is larger, service life is longer and of low cost, follows
Ring performance is good.
Specific implementation mode
One, nano carbon microsphere is prepared to include the following steps：
（1）Electrochemical treatments：Using graphite cake as anode electrode plate, using inert metal plate as cathode electrode plate, with the aqueous solution of salt
For electrolyte, commutated direct current electrolysis is added；Decomposition voltage is 36V, and electric current 10A, electrolysis time is 26 hours, obtains activity
The quality of nano carbon microsphere colloidal sol, the anode electrode plate is 1500g, and electrolyte is the sodium-chloride water solution that mass concentration is 1%
3000g；Anode electrode plate length 500mm, width 500mm；Cathode electrode plate length 500mm, 500 mm of width；
（2）Adjust pH：The pH value of active nano carbon ball colloidal sol is adjusted with ammonium hydroxide, it is 7 to adjust pH；
（3）Washing：Through high-purity water washing, the high purity water 37800g of washing is equally divided into three parts and is washed, and washing every time is used
12600g obtains carbon ball after washing, the carbon ball is dried through ultrasonic echography after ultrasonic, and 60 DEG C of vacuum are dried
It is dry, obtain drying carbon ball；Ultrasonic activation power density is 0.35w/cm2, vibration frequency 20000Hz, the ultrasonic time is 2 small
When；
（4）Surface treatment：It dries carbon ball to be impregnated with 1575g glacial acetic acid, then uses ultrasonic echography, 1185g is used after ultrasound
The ethyl alcohol that purity is 99.5% is washed, and is washed in three times, 99.5% ethyl alcohol of each washing is 395g, 60 DEG C after washing
Vacuum drying is to get nano carbon microsphere 7.5g, a diameter of 200-500nm of nano carbon microsphere；Ultrasonic activation power density is
0.35w/cm2, vibration frequency 20000Hz, the ultrasonic time is 1 hour.
Two, it utilizes（One）Middle Nano carbon balls prepare the technique of ion cathode material lithium, include the following steps：
Ball milling：2.5g silica flours and 0.5g glass puttys are added in 13.2g n-hexanes and mixed, is added in ball-grinding machine after mixing
It is uniformly mixed, adds 7.5g nano carbon microspheres and carry out secondary ball milling until silica flour, glass putty and nano carbon microsphere are uniformly mixed；The silicon
The specification of powder is not more than 25 μm, and the specification of the glass putty is not more than 25 μm.
High temperature pyrolysis：The mixture of silica flour, glass putty, nano carbon microsphere and n-hexane is pyrolyzed under protection of argon gas, pyrolysis temperature
Degree is 200-205 DEG C, and pyrolysis time is 2 hours, obtained negative material.
The purity of the n-hexane is 99%.
Three, negative material is crushed through pulverizer, bulk is crushed to powder, powder granularity control is at 50 μm hereinafter, so
It is sieved afterwards with 400 mesh standard sieves, extracting screen underflow；
0.5g carbon blacks, 1.0gCMC sodium carboxymethylcelluloses, 1.0gSBR butadiene-styrene rubber is added in screenings less than 400 mesh, is used
10.0g high purity waters and cream, it is uniform with cream to make, it need to be put into ultrasonic equipment and disperse, be uniformly mixed；
Coating is that above-mentioned lotion is applied on the copper foil of 1g, and coating procedure should be noted control coating layer thickness（1-2mm）, uniformly
It is covered with copper foil, is then placed in vacuum drying oven, temperature is controlled at 110-120 DEG C, is baked to；
By the copper foil prepared and lithium piece, diaphragm, electrolyte（Lithium hexafluoro phosphate）Battery is assembled into glove box with battery case,
Using electrochemical workstation, battery performance test is carried out using cyclic voltammetry, detects the performance of negative material, obtained nano-sized carbon
Ball material is 560 mAh/g as cathode, after testing specific capacity, opposite commercial product（370 mAh/g）There is better specific volume
Amount.
Description and application of the invention herein are illustrative, is not wishing to limit the scope of the invention to above-described embodiment
In.The deformation and change of embodiments disclosed herein are possible, real for those skilled in the art
The replacement and equivalent various parts for applying example are well known.It will be apparent to those skilled in the art do not departing from this hair
In the case of bright spirit or essential characteristics, the present invention can otherwise, structure, arrangement, ratio, and with other elements,
Material and component are realized.Without departing from the scope and spirit of the present invention, can to embodiments disclosed herein into
Other deformations of row and change.
Claims (9)
1. a kind of technique preparing ion cathode material lithium using Nano carbon balls, which is characterized in that include the following steps：
Ball milling：Silica flour and glass putty are added in n-hexane and mixed, the weight ratio of the n-hexane, silica flour and glass putty is 26.4:5:
1, it is added in ball-grinding machine and is uniformly mixed after mixing, add nano carbon microsphere and carry out secondary ball milling until silica flour, glass putty
It is uniformly mixed with nano carbon microsphere, the weight ratio of nano carbon microsphere and glass putty is 15:1；
High temperature pyrolysis：The mixture of silica flour, glass putty, nano carbon microsphere and n-hexane is pyrolyzed under inert gas protection, pyrolysis temperature
Degree is 200-205 DEG C, and pyrolysis time is 1-2 hours, obtained negative material.
2. a kind of technique preparing ion cathode material lithium using Nano carbon balls according to claim 1, which is characterized in that
The preparation process of the nano carbon microsphere includes the following steps：
（1）Electrochemical treatments：Using graphite cake as anode electrode plate, using inert metal plate as cathode electrode plate, with the aqueous solution of salt
For electrolyte, commutated direct current electrolysis is added；
（2）Adjust pH：The pH value of active nano carbon ball colloidal sol is adjusted with 50% dilute sulfuric acid or ammonium hydroxide, it is 7 to adjust pH；
（3）Washing：Through high-purity water washing, the high purity water of washing and the mass ratio of electrolyte are 12:1, the high purity water is average
It is divided into three parts to be washed, carbon ball is obtained after washing, the carbon ball is dried through ultrasonic echography after ultrasonic,
60 DEG C of vacuum dryings obtain drying carbon ball；
（4）Surface treatment：Drying carbon ball impregnated with glacial acetic acid, then use ultrasonic echography, ultrasound after with 99.5% ethyl alcohol
It is washed, average to wash in three times, glacial acetic acid：99.5% ethyl alcohol：The mass ratio for drying carbon ball is 210:158:1,60 after washing
DEG C vacuum drying is to get nano carbon microsphere.
3. a kind of technique preparing ion cathode material lithium using Nano carbon balls according to claim 2, which is characterized in that
Step（1）Decomposition voltage is 36V, and electric current 10A, electrolysis time is 24-28 hours, obtains active nano carbon ball colloidal sol, described
The mass ratio of anode electrode plate and electrolyte is 1:2.
4. the step（1）The aqueous solution of the salt is sodium-chloride water solution, potassium chloride solution, potassium sulfate solution or sulfuric acid
Sodium water solution, the mass concentration of salt is 1% in the aqueous solution of the salt.
5. a kind of technique preparing ion cathode material lithium using Nano carbon balls according to claim 2, which is characterized in that
The inert gas is argon gas.
6. a kind of technique preparing ion cathode material lithium using Nano carbon balls according to claim 2, which is characterized in that
Step（3）With（4）Ultrasonic echography, ultrasonic activation power density are 0.35w/cm2, vibration frequency 20000Hz, when ultrasonic
Between be 1-2 hours.
7. a kind of technique preparing ion cathode material lithium using Nano carbon balls according to claim 1, which is characterized in that
The purity of the n-hexane is 99%.
8. a kind of technique preparing ion cathode material lithium using Nano carbon balls according to claim 1, which is characterized in that
A diameter of 200-500nm of the nano carbon microsphere.
9. a kind of technique preparing ion cathode material lithium using Nano carbon balls according to claim 1, which is characterized in that
The specification of the silica flour is not more than 25 μm, and the specification of the glass putty is not more than 25 μm.
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