CN109888244A - A kind of graphene coated graphitization coal negative electrode material, battery and preparation method thereof - Google Patents
A kind of graphene coated graphitization coal negative electrode material, battery and preparation method thereof Download PDFInfo
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- CN109888244A CN109888244A CN201910198387.9A CN201910198387A CN109888244A CN 109888244 A CN109888244 A CN 109888244A CN 201910198387 A CN201910198387 A CN 201910198387A CN 109888244 A CN109888244 A CN 109888244A
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Abstract
The invention discloses a kind of graphene coated graphitization coal negative electrode materials, battery and preparation method thereof, wherein, the method includes the steps: coal powder is mixed with graphene precursor solution according to predetermined ratio, is ground, graphene presoma cladding coal powdery pulp is obtained；The slurry is spray-dried, presoma powder is obtained；The presoma powder is calcined in an inert atmosphere, obtains the negative electrode material of graphene coated coated graphite coal.The present invention solves the problems, such as that carbon negative pole material manufacturing cost is excessively high in the prior art, stability is bad.
Description
Technical field
The present invention relates to new material technology fields, more particularly to plant a kind of graphene coated graphitization coal negative electrode material,
Battery and preparation method thereof.
Background technique
Lithium ion battery, a kind of effective energy storage tankage based on structural material He intercalation chemistry.With
The consumption of the portable electronic devices such as mobile phone, laptop increases and hybrid power and pure electric automobile are increasingly popularized,
Caused people to of new generation low cost, high security, high-energy density, high power, have the lithium of new generation of fast charge characteristic from
Sub- battery is paid close attention to, and to meet ever-increasing market demand, the research and development for being badly in need of accelerating lithium ion battery material are improved.
Carbonaceous Negative Materials for Li-Ion Battery is one of core material of lithium ion battery, including natural graphite, graphene,
Soft or hard carbon and be the artificial graphite etc. of raw material with petroleum coke etc., the lamellar structure of graphite makes it have high theoretical capacity (372
MAh/g), and graphene have up to 744 mAh/g theoretical capacity, but use CVD (vapor deposition), oxidation-reduction method etc. just
The graphene low output of method preparation, it is at high cost, it is difficult to sizable application.Meanwhile being changed using graphene coated prepared by conventional method
Property negative electrode material, specific surface is high, and cyclical stability is poor, it is difficult to practical application.
Rich coal resources in China, and use anthracite as carbon source after deliming is handled, using coating modification system
Standby lithium ion battery negative material causes the extensive concern of researcher.Currently, the surface coating modification of coal-based carbon cathode
Agent is asphalt or coal tar asphalt, and high temperature sintering forms after pitch-coating, and wherein pitch has toxicity, can be caused
Cancer, Pintsch process can release toxic gas, pollute environment and harm health.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of graphene coated graphitization coal is negative
Pole material, battery and preparation method thereof, it is intended to it is excessively high with carbon negative pole material manufacturing cost, stable to solve lithium battery in the prior art
The bad problem of property.
Technical scheme is as follows:
A kind of preparation method of graphene coated graphitization coal negative electrode material, wherein comprising steps of
Coal powder is mixed with graphene precursor solution according to predetermined ratio, is ground, graphene presoma cladding is obtained
Coal powdery pulp；
The slurry is spray-dried, presoma powder is obtained；
The presoma powder is calcined in an inert atmosphere, obtains the cathode material of graphene coated coated graphite coal
Material.
The preparation method of the graphene coated graphitization coal negative electrode material, wherein described to be incited somebody to action according to predetermined ratio
The step of coal powder, graphene precursor solution mix, wherein the mass ratio of coal powder and graphene presoma is 1:
0.05~0. 5。
The preparation method of the described graphene coated graphitization coal negative electrode material, wherein the graphene presoma is
Oligomerisation of propene nitrile.
The preparation method of the graphene coated graphitization coal negative electrode material, wherein the coal powder passes through in advance
Deliming processing.
The preparation method of the graphene coated graphitization coal negative electrode material, wherein sprayed by the slurry
Before the dry step of mist, further includes: above-mentioned slurry is placed at a temperature of 80 ~ 350 DEG C and is heat-treated, before obtaining precrosslink
Drive somaplasm material.
The preparation method of the described graphene coated graphitization coal negative electrode material, wherein by the presoma powder
Before the step of being calcined in an inert atmosphere, further comprise the steps of: the presoma powder at a temperature of 180 ~ 250 DEG C into
Row pre-oxidation, and carry out shaping.
The preparation method of the described graphene coated graphitization coal negative electrode material, wherein the calcination temperature is 500 ~
3000 DEG C, calcination time is 2 ~ 24 h.
The preparation method of the graphene coated graphitization coal negative electrode material, wherein further comprise the steps of: to the stone
The negative electrode material of black alkene cladding coal is doped modification, and the doping vario-property includes that metal-doped modification and nonmetal doping change
Property.
A kind of graphene coated graphitization coal negative electrode material, wherein the graphene coated is graphitized coal cathode material
Material is prepared by preparation method as described above.
A kind of battery, wherein including negative electrode, the negative electrode includes negative electrode material, binder and acetylene black, described
Negative electrode material is the negative electrode material that graphene coated as described above is graphitized coal.
The utility model has the advantages that negative electrode material provided by the present invention is graphitized coal by graphene coated using coal as substrate
It obtains, the preparation method simple process, raw material sources are extensive, and low in cost, negative electrode material has stable structure, easy processing
Property, good electrolyte compatibility is excellent simultaneously with high gram volume, high security, high circulation stability, high rate capability etc.
Point.
Detailed description of the invention
Fig. 1 is the preparation method preferred embodiment process signal that graphene coated of the present invention is graphitized coal negative electrode material
Figure；
Fig. 2 ~ 5 are respectively X-ray diffractogram, scanning electron microscope (SEM) photograph, the half-cell cycle performance of negative electrode material obtained in embodiment 1
Figure and cycle charge-discharge curve graph.
Specific embodiment
The present invention provides a kind of graphene coated graphitization coal negative electrode material, battery and preparation method thereof, to make this hair
Bright purpose, technical solution and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that herein
Described specific embodiment is only used to explain the present invention, is not intended to limit the present invention.
The preparation method of graphene coated graphitization coal negative electrode material of the present invention, as shown in Figure 1, including step
It is rapid:
S1, coal powder and graphene precursor solution are mixed according to predetermined ratio, ground, obtaining graphene presoma packet
Cover toner body slurry；
S2, the slurry is spray-dried, obtains presoma powder；
S3, the presoma powder is calcined in an inert atmosphere, obtains the negative of graphene coated coated graphite coal
Pole material.
Coal powder is first mixed with graphene precursor solution, is ground by the present invention, by coal powder and graphene
Precursor is sufficiently mixed uniformly, and the slurry after then grinding is spray-dried, then is calcined in an inert atmosphere, by graphene
Precursor and coal powder are graphitized, and the graphene that is graphitized of graphene precursor is by graphited coal powder body surface
Bread wraps, and forms stable crystalline structure, the fault of construction that coal powder can be overcome intrinsic, and good electrolyte is compatible
Property, the advantages that simultaneously with high gram volume, high security, high circulation stability, high rate capability.
The coal is anthracite, lean coal, meager coal, coking coal, rich coal, bottle coal, jet coal, lignite, non-caking coal, weak bonding
One of coal or two or more combinations.
Preferably, before step S1, coal pieces are crushed to D50=1 ~ 50 μm, the breaking method be smash, crush,
Split it is broken, one of grind or two or more combinations.Instrument equipment is beater disintegrating machine, disk mill, right
Roller pulverizer, roller pulverizer, medicinal herb grinder, sand mill, airflow mill, tumbling ball mill, planetary ball mill etc..
More preferably, before step S1, coal powder is handled through deliming, removes sulphur therein, metal impurities, obtains
Fixed carbon content reaches high-purity coal powder of national standard.And the method that the deliming processing uses roasts for floatation, chlorination
One of burning method, high temperature method, acid-base method, hydrogen fluoride or two or more combinations.Wherein, the temperature of high temperature method deliming processing
Degree be 1500 ~ 3000 DEG C, the processing time be 2 ~ 10h.
It specifically, is 1:0.05's ~ 0. 5 according to the mass ratio of coal powder and graphene presoma in the step S1
Predetermined ratio mixes coal powder, graphene precursor solution, and be stirred using mechanically or magnetically power, ball milling mixing,
One of ultrasonic mixing, the mixing of roller mill, heating mixing or two or more combined mode mixed processing 8 ~ for 24 hours, to fill
Divide and be uniformly mixed, obtains graphene presoma carbon coated powdery pulp.Wherein, the mixed temperature of the heating is 80 ~ 150 DEG C,
The processing time is 5 ~ 20h.Preferably, the relative molecular weight of the graphene presoma is 100 ~ 100000, before graphene
Driving the mass fraction in liquid solution is 1% ~ 90%.The graphene presoma concretely oligomerisation of propene nitrile comprising acrylonitrile
Any one in monomer-polymer, acrylonitrile and other alkene monomer polymers, and the solvent of solution be ethyl alcohol, water, methanol,
One of ethyl acetate, acetone or two or more combinations.
Preferably, it before the step S2, is carried out at a temperature of step S1 slurry obtained is first placed in 80 ~ 350 DEG C
Heat treatment, specifically can be and carries out in the convection oven of 80 ~ 350 DEG C of temperature, obtain the forerunner of graphene precursor precrosslink
Somaplasm material, precrosslink are convenient for more uniformly enveloping graphited coal using the graphene of generation when subsequent calcination.It is more excellent
The time on ground, heat treatment controls in 6 ~ 12h, can achieve the effect that precrosslink, and do not waste more energy consumptions.
In the step S2, using spray drying device such as atomizer is dry, press spray is dry etc. by step
Solvent removal in the obtained graphene presoma carbon coated powdery pulp of S1, can access graphene presoma and coal
The presoma powder that powder mixes well.Preferably, the inlet air temperature temperature of the spray drying is 180 ~ 250 DEG C, charging speed
Degree is 10 ~ 50 mL/min, and spray drying has better effect.
Preferably, between step S3, i.e., the step of the presoma powder is calcined in an inert atmosphere it
Before, first the presoma powder is pre-oxidized at a temperature of 180 ~ 250 DEG C, and carry out shaping, to form target material
Blank, is specifically shaped as particle of the particle size between 100 nm ~ 100 μm, and pattern is ellipsoid dress, blocky, cotton-shaped, silk
In shape, strip, sheet, honeycomb, cellular, diamond shaped, one of a combination of one or more without specific shape
Or it is a variety of.Wherein, the Training system is one or more of airflow milling, ball milling, sand milling, and equipment can use flat gas
Flow grinding machine, circulating airflow mill, to spray formula airflow mill, target formula airflow mill, fluidization to spray formula airflow mill, roller ball
One or two kinds of combination of the above such as grinding machine, planetary ball mill, vertical grinding machine, horizontal sand mill.
In the step S3, by precursor powder obtained in step S2 be placed in the inert gases such as nitrogen, argon gas into
Row calcining, it is preferable that calcination temperature is 500 ~ 3000 DEG C, calcination time is 2 ~ 24 h, under calcining effect, graphene presoma
Such as oligomerisation of propene nitrile graphite turns to graphene, and coal powder is also graphitized, and because of abovementioned steps by graphene
Precursor be well dispersed in around coal powder (in more preferably scheme, the precrosslink of graphene precursor enlist the services of in coal
Powder periphery), thus the graphene formed can be firmly coated on coal powder, or even be penetrated into coal surface micropore, shape
At stable crystalline structure, thus overcome existing coal porous surface, loose fault of construction, it will not be in charging and discharging easily
Deformation occurs.Too low can not be successfully of the calcination temperature is graphitized, and temperature is excessively high, can form other by-products too much.
Wherein, inert gas flow control is in 50 ~ 1000 mL/min.
The fixation carbon content of the negative electrode material of the graphene coated coated graphite coal obtained by above-mentioned preparation method
>=99.9%, average grain diameter D50It is 1 ~ 50 μm, specific surface is 1 ~ 100 m2/ g, tap density are 0.30 ~ 1.6 g/cm3.It is preferred that
Ground, reversible gram volume >=350.0 mAh/g of the negative electrode material of the graphene coated coated graphite coal, coulomb is imitated for the first time
500 circle retention rate >=85.0% of rate >=95.0%, 1C circulation.
Preferably, the preparation method of graphene coated graphitization coal negative electrode material is further comprised the steps of: to described
The negative electrode material of graphene coated coal is doped modification, and the doping vario-property includes metal-doped modification and nonmetal doping
It is modified.The substance of the metal-doped modification is metal simple-substances and its chemical combination such as tin, copper, silver, aluminium, iron, chromium, nickel, cobalt, titanium, manganese
Object, metal oxide, metal nitride, metal boride, metal fluoride, metal bromide, metal sulfide or metal
One of organic compound or two or more combinations；The non-metallic inclusion is silicon, phosphorus, boron, nitrogen, carbon, sulphur simple substance
And its one of compound or two or more combinations.
Based on the above method, the present patent application additionally provides a kind of graphene coated graphitization coal negative electrode material, wherein
The graphene coated graphitization coal negative electrode material is obtained by preparation method as described above.
Based on the above method, the present patent application additionally provides a kind of battery, wherein including negative electrode, the negative electrode packet
Negative electrode material, binder and acetylene black are included, the negative electrode material is that graphene coated as described above is graphitized coal
Negative electrode material.
Below by embodiment, the present invention is described in detail.
Embodiment 1
100 g anthracites are taken, ball mill grinding obtains D50=16 μm of thick anthracite powder carries out coarse powder material using alkali acid system
High-purity anthracite powder is obtained after deliming processing.It is according to mass ratio with oligomeric propylene liguid nitrile solution by high-purity anthracite powder
Deionized water is added according to the proportion that high-purity coal powder and solvent quality proportion are 1:3, using drum-type in the proportion of 1:0.10
Ball milling mixing 8h, obtains precursor pulp.Precursor pulp is placed in 50 DEG C of heat treatment 6h in convection oven, obtains micro- crosslinking
Precursor pulp.The precursor pulp of micro- crosslinking is dry using atomizer, and inlet air temperature is 180 DEG C, and feeding speed is
25 mL/min obtain dry presoma powder.Dry presoma powder is placed in low-level oxidation 8h in 150 DEG C of convection oven,
Obtain low-level oxidation presoma powder.By lower 2600 DEG C of low-level oxidation presoma powder inert atmosphere, 6h is kept the temperature, graphene coated is obtained
Coal negative electrode material.
According to negative electrode material active material: binder (SBR, SA, CMC or PVDF etc.): acetylene black=93:6:1 ratio
(mass percent) stirs slurry and electrode slice is made, and lithium piece makees anode assembling button cell, electricity is carried out on the indigo plant electrical measurement test system of Wuhan
Chemical property test.The characterization test of the negative electrode material of graphene coated coated graphite coal is as shown in Fig. 2 ~ 5, the cathode material
The X-ray diffractogram (XRD diagram) and scanning electron microscope (SEM) photograph (SEM figure) of material, half-cell cycle performance figure, cycle charge-discharge curve graph
Respectively as shown in Fig. 2, Fig. 3, Fig. 4 and Fig. 5.
As shown in Figure 2, it is obtained after graphene coated and high temperature graphitization processing using coal feedstocks such as anthracites
Artificial negative electrode material is in the standard diffraction that the angle of diffraction is that the sharp absorption peak occurred at 26.5 degree or so is 002 peak face of graphitized carbon
Absorption peak；At two 101 peak face diffracted absorption peaks that the angle of diffraction is 45 degree or so appearance, show the 2H that artificial graphite only exists
Phase.
As shown in figure 3, graphene coated makes graphene nano lamella pile up aggregation in particle surface, therefore obtain negative
The surface of pole material seems that more coarse material, structure are two kinds of forms of ellipticity and square block, and intergranular contact is face
Based on contact, makes to come into full contact between particle, obtain better chemical property, avoid single use ellipsoid particle and make
It is insufficient contact caused by point contact at interparticle contact.
As shown in Figure 4, the negative electrode material obtained is designed according to graphite theoretical capacity 372mAh/g, in 0.5C constant current density
Under obtain good cyclical stability, reversible capacity has reached 340mAh/g or so, 100 circle circulations, and capacity is undamped.
As shown in Figure 5, graphene coated coal feedstock is after high temperature graphitization is handled, charging and discharging curve and natural stone
Ink is similar (charging/discharging voltage 0-3.0V), has apparent removal lithium embedded platform in the voltage range of 0.1-0.2V.
Embodiment 2
100 g coking coal are taken, ball mill grinding obtains D50=16 μm of thick coking coal powder carries out deliming using alkali acid system to coarse powder material
High-purity coking coal powder is obtained after processing.It according to mass ratio is 1:0.10's by high-purity coking coal powder and oligomeric propylene liguid nitrile solution
Proportion is added deionized water according to the proportion that high-purity coal powder and solvent quality proportion are 1:3, is mixed using roller milling
8h obtains precursor pulp.Precursor pulp is placed in 50 DEG C of heat treatment 6h in convection oven, obtains forerunner's somaplasm of micro- crosslinking
Material.The precursor pulp of micro- crosslinking is dry using atomizer, and inlet air temperature is 180 DEG C, and feeding speed is 25 mL/
Min obtains dry presoma powder.Dry presoma powder is placed in low-level oxidation 8h in 150 DEG C of convection oven, is obtained micro-
Oxidic precursor powder.By lower 2600 DEG C of low-level oxidation presoma powder inert atmosphere, 6h is kept the temperature, it is negative to obtain graphene coated coal
Pole material.
According to negative electrode material active material: binder (SBR, SA, CMC or PVDF etc.): acetylene black=93:6:1 ratio
(mass percent) stirs slurry and electrode slice is made, and lithium piece makees anode assembling button cell, electricity is carried out on the indigo plant electrical measurement test system of Wuhan
Chemical property test.
Through detecting, the preparation-obtained single crystal silicon integrality of embodiment 2 is good, uniform resistivity, purity reach 9N grades
Not.
In conclusion graphene coated graphitization coal negative electrode material provided by the present invention and preparation method thereof, with coal
Charcoal is substrate, is graphitized coal by graphene coated and obtains, the preparation method simple process, raw material sources are extensive, at low cost
Honest and clean, negative electrode material has stable structure, workability, good electrolyte compatibility, simultaneously with high gram volume, Gao An
The advantages that Quan Xing, high circulation stability, high rate capability.Meanwhile using oligomeric propylene liguid nitrile solution as graphene forerunner
Body carbon source, have many advantages, such as it is at low cost, being capable of prepare with scale.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of graphene coated graphitization coal negative electrode material, which is characterized in that comprising steps of
Coal powder is mixed with graphene precursor solution according to predetermined ratio, is ground, graphene presoma cladding is obtained
Coal powdery pulp；
The slurry is spray-dried, presoma powder is obtained；
The presoma powder is calcined in an inert atmosphere, obtains the cathode material of graphene coated coated graphite coal
Material.
2. the preparation method of graphene coated graphitization coal negative electrode material according to claim 1, which is characterized in that institute
State the step of coal powder, graphene precursor solution being mixed according to predetermined ratio, wherein before coal powder and graphene
The mass ratio for driving body is 1:0.05 ~ 0. 5.
3. the preparation method of graphene coated graphitization coal negative electrode material according to claim 1, which is characterized in that institute
Stating graphene presoma is oligomerisation of propene nitrile.
4. the preparation method of graphene coated graphitization coal negative electrode material according to claim 1, which is characterized in that institute
Coal powder is stated to handle through deliming in advance.
5. the preparation method of graphene coated graphitization coal negative electrode material according to claim 1, which is characterized in that
Before the step of slurry is spray-dried, further includes: carry out hot place at a temperature of above-mentioned slurry is placed in 80 ~ 350 DEG C
Reason, obtains the precursor pulp of precrosslink.
6. the preparation method of graphene coated graphitization coal negative electrode material according to claim 1, which is characterized in that
Before the step of presoma powder is calcined in an inert atmosphere, further comprise the steps of: by the presoma powder in
It is pre-oxidized at a temperature of 180 ~ 250 DEG C, and carries out shaping.
7. the preparation method of graphene coated graphitization coal negative electrode material according to claim 1, which is characterized in that institute
Stating calcination temperature is 500 ~ 3000 DEG C, and calcination time is 2 ~ 24 h.
8. the preparation method of graphene coated graphitization coal negative electrode material according to claim 1, which is characterized in that also
Comprising steps of being doped modification to the negative electrode material of the graphene coated coal, the doping vario-property includes metal-doped
Modified and nonmetal doping is modified.
9. a kind of graphene coated is graphitized coal negative electrode material, which is characterized in that the graphene coated graphitization coal is negative
Pole material is made by preparation method a method as claimed in any one of claims 1-8.
10. a kind of battery, which is characterized in that including negative electrode, the negative electrode includes negative electrode material, binder and acetylene
Black, the negative electrode material is the negative electrode material that graphene coated as claimed in claim 9 is graphitized coal.
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| CN112038603A (en) * | 2020-09-03 | 2020-12-04 | 青海凯金新能源材料有限公司 | Graphite negative electrode material and processing technology thereof |
| CN114789998A (en) * | 2021-11-01 | 2022-07-26 | 广东一纳科技有限公司 | Negative electrode material, preparation method thereof and battery |
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| CN108383111A (en) * | 2018-05-11 | 2018-08-10 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene slurry and preparation method thereof |
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| US20150251911A1 (en) * | 2012-10-24 | 2015-09-10 | Tokai Carbon Co., Ltd. | Process for manufacturing graphite powder for lithium secondary battery negative electrode material |
| CN104332616A (en) * | 2014-09-09 | 2015-02-04 | 刘剑洪 | Graphene coated graphite composite lithium ion battery negative material and its preparation method |
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| CN112038603A (en) * | 2020-09-03 | 2020-12-04 | 青海凯金新能源材料有限公司 | Graphite negative electrode material and processing technology thereof |
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Application publication date: 20190614 |