CN109935793A - A kind of preparation method of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material - Google Patents
A kind of preparation method of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material, using graphene temper carbon particle as made from cladding, bonding, graphitization, since kernel is graphene, capacity height, good rate capability, after external composite artificial graphite, so that capacity is high, charge-discharge performance is good, and particle surface one way or another is arranged, has the characteristics that high isotropism, while second particle structure can increase graphite internal void；Lithium ion is moved to several directions, is conducive to electrolyte and infiltrates, form more lithium ion mobility channels, migration path is shorter, improves the large current density performance performance of graphite, circulation, cryogenic property are more preferably.
Description
Technical field
The present invention relates to field of lithium ion battery technologies, and it is compound to refer in particular to a kind of lithium ion cell high-capacity high magnification
The preparation method of graphene negative electrode material.
Background technique
Lithium ion battery have voltage height, specific energy height, memory-less effect, have extended cycle life it is special with non-environmental-pollution etc.
Point is widely used in mobile phone, laptop and other portable electronic devices.The cathode material of lithium ion battery
Material plays a key effect for the performance of entire battery, therefore negative electrode material becomes research hotspot in recent years.
The negative electrode material of commercial Li-ion batteries is mostly graphite material.Graphite have crystallization layer structure, be easy to lithium from
Son forms interlayer compound L iC in intercalation/deintercalation wherein6, it is a kind of negative electrode material that performance is stable.But graphite cathode is managed
It is only 372mAh/g by specific capacity, therefore realizes that lithium ion battery high specific energy quantifies, it is necessary to researchs and develops the cathode of high capacity
Material graphene (graphene) is a kind of Novel Carbon Nanomaterials, tightly packed at bi-dimensional cellular shape knot by single layer s carbon atom
Structure.It has recently been demonstrated that graphene has excellent electricity, calorifics, optics and mechanical property, high theoretical specific surface area
A series of and special natures such as conductivity never to disappear.The big specific surface area of graphene and its good electric property are determined
It has been determined in the great potential of field of lithium ion battery, has been had at present using graphene as lithium ion battery negative material a small amount of
Report.Because graphene is made of single layer of carbon atom close-packed arrays, lithium ion may be stored not only in the two of graphene sheet layer
Side can also store in the edge and hole of graphene sheet layer, and theoretical capacity is 740~780mAh/g, about traditional stone
More than 2 times of ink material.It uses graphene that battery lithium storage content will be greatly improved as lithium ion battery negative material, and then improves
Energy density.In addition, using graphene as lithium ion battery negative material when, diffusion of the lithium ion in grapheme material
Path is shorter, and conductivity is higher, can largely improve its high rate performance.Therefore, graphene is as lithium ion battery
Negative electrode material has a good application prospect.But graphene is used as merely cathode, because its granularity is small, jolt ramming is low, large specific surface area
Etc. factors, there are many problems in terms of processing.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide a kind of lithium ion batteries
The preparation method of high capacity high magnification composite graphite alkene negative electrode material, cladding is bonded one layer of artificial graphite on the surface of graphene,
It is high with capacity, compaction capacity is good, the characteristics of good rate capability, improve the large current density performance of battery cathode.
To achieve the above object, the present invention is using following technical solution:
A kind of preparation method of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material, includes the following steps
Step (1), by reduced graphene and pore creating material 1:(10-30 in mass ratio) after mixing, it is soaked in aqueous solvent
Stain after drying is under an inert atmosphere activated 0.1-0.4 hours, then cleaned under conditions of 1000-3000 DEG C, and weldering is dry
Obtain porous graphene；
Step (2), feeds intake: porous graphene, bonding agent and graphitization catalyst thrown to roller microwave oven,
When feeding intake, it is desirable that the roller in roller microwave oven feeds in rotation, and drum rotation speed control turns/min. in 10-20, should
It is auxiliary in roller microwave oven to give oscillator, vibration frequency 80-100Hz；Wherein, each material to feed intake is in mass ratio are as follows: more
Graphene 30-94 parts of hole, 5-30 parts of bonding agent, 1-5 parts of graphitization catalyst；
Step (3), low temperature cladding, bonding, charing: roller microwave oven revolving speed 90-120 turns of adjusting/
Min., so that heating in furnace is carried out level-one heating, temperature is made to rise to 200 DEG C from room temperature, constant temperature is kept for 1.5-2 hours, realizes low temperature
Then cladding and bonding make heating in furnace carry out second level heating, so that temperature is risen to 400 DEG C, constant temperature is kept for 1-1.5 hours, then is made
Heating carries out three-level heating in furnace, and temperature is made to rise to 600 DEG C, and constant temperature is kept for 1-1.5 hours, and heating in furnace is finally made to carry out four
Grade heating, makes temperature rise to 800 DEG C, and constant temperature is kept for 1-1.5 hours, make graphitization catalyst successively from outer layer to internal layer step by step
Charing；
Step (4), it is cooling: Dry Quenching to be used, with cold inert gas N2Heat is carried out in coke oven with red-hot coke
Exchange, the cooling in coke dry quenching furnace of inertia recyclegas is red defocused, absorbs the high temperature circulation gas of red burnt heat through primary dedusting
Device enters boiler after removing coarse granule coke powder, and boiler heat absorption generates steam, and cooled inertia recyclegas is through secondary filter
Fine grain coke powder is removed, then coke dry quenching furnace is blasted by circulating fan and continues cycling through cooling red coke, until coke is down to room temperature；
Step (5) purifies graphitization processing: using catalyst made from platonic carbon electrode bar for anode, be with high-purity carbon electrode bar
Cathode realizes the arc discharge between two electrode of positive and negative in the helium that air pressure is 900~1500Torr, and discharge current is
300~350A；The distance between anode and cathode is 1~1.5mm when electric discharge, and composite graphite alkene negative electrode material crude product is made；
The crude product of above-mentioned preparation is subjected to high-temperature heat treatment in air, the temperature of air atmosphere controls the processing at 300~500 DEG C
Time is 0.5~1.0 hour, to remove most impurity；
Step (6) finally obtains using graphene as kernel through finely ground, sieving, is coated with artificial graphite, is bonded shape
At core-shell structure second particle.
As a preferred embodiment, in step (1), the specific surface area of the porous graphene is 3.5-5m2/ g, jolt ramming
Density is 0.8-1.0g/cm3, aperture 2-10nm, particle size is 5-15 μm.
As a preferred embodiment, in step (2), the bonding agent is one kind of pitch prill, coal tar, macromolecule resin
Or mixtures thereof.
As a preferred embodiment, in step (2), the bonding agent is macromolecule resin, includes fourth in parts by weight
60~90 parts of diene, 5~15 parts of Rn-CH=C-CN, 1~5 part of CH3-C=CH-COORm, the monomer emulsion polymerization of three and
At product obtains the lotion containing glue 35%~55% after purification.
As a preferred embodiment, in step (2), the graphitization catalyst be containing silicon, iron, tin oxide or
Carbide.
As a preferred embodiment, in step (2), the graphitization catalyst is SiO2、SiC、 Fe2O3、SnO2One
Or mixtures thereof kind.
As a preferred embodiment, in step (5), the anode and cathode arc discharge is that be passed through to two end electrodes can
The pulse direct current of tune, adjusting current density are 5~15mA/cm2, 20~30min of residence time.
As a preferred embodiment, in step (6), the outer artificial graphite coated of the graphene kernel is in dirt spar
Structure, each dirt spar mutually closely cut arrangement and form conductive network.
As a preferred embodiment, in step (2), organic carbon source substance can be further increased when feeding intake.
As a preferred embodiment, the organic carbon source is selected from glucose, sucrose, ascorbic acid, polyvinyl alcohol, lemon
One of acid, starch, agarose, polyethylene glycol, beta-cyclodextrin or two or more mixtures.
The present invention has obvious advantages and beneficial effects compared with the existing technology, specifically, by above-mentioned technical proposal
It is found that the present invention uses graphene temper carbon particle as made from cladding, bonding, graphitization, since kernel is graphite
Alkene, capacity is high, good rate capability, after external composite artificial graphite, so that capacity is high, charge-discharge performance is good, and particle surface
One way or another arrangement, has the characteristics that high isotropism, while second particle structure can increase graphite internal void；Make
Obtaining lithium ion can move to several directions, be conducive to electrolyte and infiltrate, form more lithium ion mobility channels, migration path is more
It is short, the large current density performance performance of graphite is improved, circulation, cryogenic property are more preferably.
In order to explain the structural features and functions of the invention more clearly, come combined with specific embodiments below to the present invention into
Row is described in detail.
Specific embodiment
The present invention provides a kind of negative electrode material, the lithium ion two especially suitable for high capacity high current fast charging and discharging demand
Primary cell, be it is a kind of by relative low temperature it is integrated cladding, bonding, charring process prepare the two of graphene core-shell structure
Schungite particle, makes it have the graphite material that capacity is high, multiplying power property is good, and specific production stage is as follows.
Step (1), by reduced graphene and pore creating material 1:(10-30 in mass ratio) after mixing, it is soaked in aqueous solvent
Stain after drying is under an inert atmosphere activated 0.1-0.4 hours, then cleaned under conditions of 1000-3000 DEG C, and weldering is dry
Obtain porous graphene.After this technique, the specific surface area of the porous graphene is 3.5-5m2/ g, tap density are
0.8-1.0g/cm3, aperture 2-10nm, particle size is 5-15 μm.
Step (2), feeds intake: porous graphene, bonding agent and graphitization catalyst thrown to roller microwave oven,
When feeding intake, it is desirable that the roller in roller microwave oven feeds in rotation, and drum rotation speed control turns/min. in 10-20, should
It is auxiliary in roller microwave oven to give oscillator, vibration frequency 80-100Hz；Wherein, each material to feed intake is in mass ratio are as follows: more
Graphene 30-94 parts of hole, 5-30 parts of bonding agent, 1-5 parts of graphitization catalyst.By the roller side in roller microwave oven
Side charging is rotated, the mixed effect of graphene, bonding agent and graphitization catalyst can be improved, makes three's mixing abundant, benefit
In bonding agent and graphitization catalyst to the cladding of graphene, coat bonding agent and graphitization catalyst more evenly effective.
Wherein, the bonding agent is or mixtures thereof pitch prill, coal tar, one kind of macromolecule resin.The grain of the bonding agent
Diameter can be 100um hereinafter, preferably 15um or less.In the present embodiment, the bonding agent is macromolecule resin, in parts by weight,
Include 60~90 parts of butadiene, 5~15 parts of Rn-CH=C-CN, 1~5 part of CH3-C=CH-COORm, the monomer emulsions of three
It is polymerized, product obtains the lotion containing glue 35%~55% after purification.The graphitization catalyst be containing silicon, iron,
The oxide or carbide of tin.In the present embodiment, the graphitization catalyst is SiO2、SiC、Fe2O3、 SnO2One kind or
Its mixture.
In addition to this, organic carbon source substance can also be further increased when feeding intake, such as such each material to feed intake is by matter
Measure ratio are as follows: 82 parts of porous graphene, 29 parts of bonding agent, 5 parts of graphitization catalyst, 8 parts of organic carbon source.It is described in the present embodiment
Organic carbon source is selected from glucose, sucrose, ascorbic acid, polyvinyl alcohol, citric acid, starch, agarose, polyethylene glycol, β-ring paste
One of essence or two or more mixtures.
Step (3), low temperature cladding, bonding, charing: roller microwave oven revolving speed 90-120 turns of adjusting/
Min., so that heating in furnace is carried out level-one heating, temperature is made to rise to 200 DEG C from room temperature, constant temperature is kept for 1.5-2 hours, realizes low temperature
Then cladding and bonding make heating in furnace carry out second level heating, so that temperature is risen to 400 DEG C, constant temperature is kept for 1-1.5 hours, then is made
Heating carries out three-level heating in furnace, and temperature is made to rise to 600 DEG C, and constant temperature is kept for 1-1.5 hours, and heating in furnace is finally made to carry out four
Grade heating, makes temperature rise to 800 DEG C, and constant temperature is kept for 1-1.5 hours, make graphitization catalyst successively from outer layer to internal layer step by step
Charing.Due to using roller microwave oven this device, microwave special envoy obtain heating temperature do not need it is very high, relatively
In 2000 DEG C of traditional heating furnace or more of carbonization temperature, highest carbonization temperature of the invention only needs to be adjusted to 800 DEG C, because
This is referred to as low-temperature carbonization.After the cladding of low temperature, bonding, charring process, make the lesser core-shell structure one of partial size
Secondary particle has the characteristics that high isotropism, increases simultaneously in the composite graphite particles surface one way or another arrangement being bonded
Graphite internal void is added；Lithium ion is moved to several directions, is conducive to electrolyte and infiltrates, form more lithium ions
Migrating channels, migration path is shorter, improves graphite large current density, cryogenic property.
Step (4), it is cooling: Dry Quenching to be used, with cold inert gas N2Heat is carried out in coke oven with red-hot coke
Exchange, the cooling in coke dry quenching furnace of inertia recyclegas is red defocused, absorbs the high temperature circulation gas of red burnt heat through primary dedusting
Device enters boiler after removing coarse granule coke powder, and boiler heat absorption generates steam, and cooled inertia recyclegas is through secondary filter
Fine grain coke powder is removed, then coke dry quenching furnace is blasted by circulating fan and continues cycling through cooling red coke, until coke is down to room temperature.This
The kind type of cooling, shortens 50 times or more than the natural cooling time.
Step (5) purifies graphitization processing: using catalyst made from platonic carbon electrode bar for anode, be with high-purity carbon electrode bar
Cathode realizes the arc discharge between two electrode of positive and negative in the helium that air pressure is 900~1500Torr, and discharge current is
300~350A；The distance between anode and cathode is 1~1.5mm when electric discharge, and composite graphite alkene negative electrode material crude product is made；
The crude product of above-mentioned preparation is subjected to high-temperature heat treatment in air, the temperature of air atmosphere controls the processing at 300~500 DEG C
Time is 0.5~1.0 hour, to remove most impurity.In the present embodiment, the anode and cathode arc discharge is to two
Termination electrode is passed through adjustable pulse direct current, and adjusting current density is 5~15mA/cm2, 20~30min of residence time.By
After purification graphitization processing, impurity can be more sufficiently removed, the graphite purity of preparation is higher.
Step (6) finally obtains using graphene as kernel through finely ground, sieving, is coated with artificial graphite, is bonded shape
At core-shell structure second particle.Wherein, the outer artificial graphite coated of the graphene kernel is in dirt spinel structure, respectively
Dirt spar mutually closely cuts arrangement and forms conductive network.This second particle being combined, the specific surface area of artificial graphite
For 1000-3000m2/ g, tap density 3-5g/cm3, aperture 30-38nm, particle size is 7-11 μm, and capacity is greater than
350mAh/g。
In conclusion design focal point of the invention is, use using graphene as kernel, coated with artificial graphite,
The second particle of core-shell structure made of bonding has the characteristics that capacity is high, compaction capacity is good, good rate capability.Process
Include: mixing in specific proportions, bonding agent is added is coated, be bonded, is carbonized finally by temperature programming, and then be made
Composite graphite material.It is suitble to high capacity fast charge or high capacity high current with high capacity, high-pressure solid, high-rate characteristics
The lithium ion secondary battery of electric discharge demand.
The above described is only a preferred embodiment of the present invention, not making any limit to technical scope of the invention
System, therefore any subtle modifications, equivalent variations and modifications to the above embodiments according to the technical essence of the invention,
All of which are still within the scope of the technical scheme of the invention.
Claims (10)
1. a kind of preparation method of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material, it is characterised in that: including
Following steps
Step (1), by reduced graphene and pore creating material 1:(10-30 in mass ratio) after mixing, it impregnates, dries in aqueous solvent
After dry under an inert atmosphere, is activated 0.1-0.4 hours under conditions of 1000-3000 DEG C, then cleaned, weldering is dry obtain it is more
Hole graphene；
Step (2), feeds intake: porous graphene, bonding agent and graphitization catalyst being thrown to roller microwave oven, fed intake
When, it is desirable that the roller in roller microwave oven feeds in rotation, and drum rotation speed control turns/min. in 10-20, and the roller is micro-
It is auxiliary in Wave heating furnace to give oscillator, vibration frequency 80-100Hz；Wherein, each material to feed intake is in mass ratio are as follows: porous graphite
30-94 parts of alkene, 5-30 parts of bonding agent, 1-5 parts of graphitization catalyst；
Step (3) low temperature cladding, bonding, charing: adjusts roller microwave oven revolving speed 90-120 and turns/min., make furnace
Interior heating carries out level-one heating, and temperature is made to rise to 200 DEG C from room temperature, and constant temperature is kept for 1.5-2 hours, realizes low temperature cladding and glues
It connects, heating in furnace is then made to carry out second level heating, temperature is made to rise to 400 DEG C, constant temperature is kept for 1-1.5 hours, then makes heating in furnace
Three-level heating is carried out, temperature is made to rise to 600 DEG C, constant temperature is kept for 1-1.5 hours, so that heating in furnace is carried out level Four heating, is made
Temperature rises to 800 DEG C, and constant temperature is kept for 1-1.5 hours, carbonizes graphitization catalyst successively step by step from outer layer to internal layer；
Step (4), it is cooling: Dry Quenching to be used, with cold inert gas N2Heat exchange is carried out in coke oven with red-hot coke,
The cooling in coke dry quenching furnace of inertia recyclegas is red defocused, and the high temperature circulation gas for absorbing red burnt heat is removed through disposable dust remover
Enter boiler after coarse granule coke powder, boiler heat absorption generates steam, and cooled inertia recyclegas removes thin through secondary filter
The coke powder of particle, then coke dry quenching furnace is blasted by circulating fan and continues cycling through cooling red coke, until coke is down to room temperature；
Step (5) purifies graphitization processing: using catalyst made from platonic carbon electrode bar for anode, using high-purity carbon electrode bar as cathode,
Air pressure be 900~1500Torr helium in, realize two electrode of positive and negative between arc discharge, discharge current be 300~
350A；The distance between anode and cathode is 1~1.5mm when electric discharge, and composite graphite alkene negative electrode material crude product is made；It will be above-mentioned
The crude product of preparation carries out high-temperature heat treatment in air, and the temperature of air atmosphere is controlled at 300~500 DEG C, and the processing time is
0.5~1.0 hour, to remove most impurity；
Step (6) finally obtains using graphene as kernel through finely ground, sieving, is coated with artificial graphite, is bonded formation
The second particle of core-shell structure.
2. a kind of preparation side of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 1
Method, it is characterised in that: in step (1), the specific surface area of the porous graphene is 3.5-5m2/ g, tap density 0.8-
1.0g/cm3, aperture 2-10nm, particle size is 5-15 μm.
3. a kind of preparation side of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 1
Method, it is characterised in that: in step (2), the bonding agent is or mixtures thereof pitch prill, coal tar, one kind of macromolecule resin.
4. a kind of preparation side of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 2
Method, it is characterised in that: in step (2), the bonding agent be macromolecule resin, in parts by weight, comprising 60~90 parts of butadiene,
5~15 parts of Rn-CH=C-CN, 1~5 part of CH3-C=CH-COORm, the monomer emulsion polymerization of three forms, and product is by mentioning
The lotion containing glue 35%~55% is obtained after pure.
5. a kind of preparation side of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 1
Method, it is characterised in that: in step (2), the graphitization catalyst be containing silicon, iron, tin oxide or carbide.
6. a kind of preparation side of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 5
Method, it is characterised in that: in step (2), the graphitization catalyst is SiO2、SiC、Fe2O3、SnO2Or mixtures thereof one kind.
7. a kind of preparation side of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 1
Method, it is characterised in that: in step (5), the anode and cathode arc discharge is that two end electrodes are passed through with adjustable pulse direct current
Electricity, adjusting current density are 5~15mA/cm2, 20~30min of residence time.
8. a kind of preparation side of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 1
Method, it is characterised in that: in step (6), the outer artificial graphite coated of the graphene kernel is in dirt spinel structure, each dirt spar
Mutually closely cutting arrangement forms conductive network.
9. a kind of preparation side of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 1
Method, it is characterised in that: in step (2), organic carbon source substance can be further increased when feeding intake.
10. a kind of preparation of lithium ion cell high-capacity high magnification composite graphite alkene negative electrode material according to claim 8
Method, it is characterised in that: the organic carbon source is selected from glucose, sucrose, ascorbic acid, polyvinyl alcohol, citric acid, starch, fine jade
One of lipolysaccharide, polyethylene glycol, beta-cyclodextrin or two or more mixtures.
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| CN114556629A (en) * | 2021-06-21 | 2022-05-27 | 宁德新能源科技有限公司 | Negative electrode material, electrochemical device, and electronic device |
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