CN107706417A - A kind of preparation method of the spherical carbon cathode material of lithium ion battery - Google Patents
A kind of preparation method of the spherical carbon cathode material of lithium ion battery Download PDFInfo
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- CN107706417A CN107706417A CN201711160144.3A CN201711160144A CN107706417A CN 107706417 A CN107706417 A CN 107706417A CN 201711160144 A CN201711160144 A CN 201711160144A CN 107706417 A CN107706417 A CN 107706417A
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- ion battery
- lithium ion
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- starch
- spherical carbon
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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
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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 preparation method of the spherical carbon cathode material of lithium ion battery.Using starch as raw material, it is uniformly mixed by a certain percentage with iron powder, carries out stabilization processes in 200 250 DEG C in air atmosphere, then high temperature cabonization under an inert atmosphere, spherical carbon cathode material is obtained through overpickling, washing, suction filtration, drying.Add iron powder to be spaced from each other starch granules, avoid the phenomenon of starch granules uneven heating, substantially reduce and stabilize the time, the carbon microspheres of preparation maintain the primary morphology of starch granules, and its particle diameter is 2 40 μm.This method technique is simple, low for equipment requirements, and gained carbon microspheres pattern is excellent, uses it for lithium ion battery negative material, shows superior chemical property.
Description
Technical field
Application the present invention relates to a kind of preparation method of spherical carbon and its in terms of lithium ion battery, belongs to lithium-ion electric
Pond negative material technical field.
Background technology
Electronic product plays more and more important role, Battery Market dog-eat-dog, lithium in our daily life
Ion battery is because energy density is big, and average output voltage is high, good cycling stability, service life length, small volume, light weight, nothing
Memory effect, the advantage such as safe and reliable, is widely used in fields such as consumer electronics, electric automobile and energy storage.
The raising of lithium ion battery negative material capacity is one of key that its energy density improves.Carbon Materials are lithium ions
The ideal chose of cell negative electrode material, is mainly most widely used with graphite type material at present.As lithium ion battery applications are led
The extension in domain, its performance requirement is improved constantly, the office of ratio energy, cycle performance and security of graphite cathode material etc.
It is sex-limited more and more prominent.Carbon microspheres have good heat endurance, thermal conductivity, bulk density height, surface-to-volume than low,
The irreversible capacity loss caused by the side reactions such as SEI films can be reduced, so as to beneficial to the electrochemistry for improving lithium ion battery
Can, it is study hotspot.
Document " Non-catalytic CVD preparation of carbon spheres with a specific
In size (Carbon, 2004,42 (4), 761-766) ", author is using toluene as raw material, using homemade twin furnace chemical vapor deposition
Product device prepares spherical Carbon Materials under conditions of catalyst is not added.Document " The production of carbon
materials by hydrothermal carbonization of cellulose Carbon,2009.47(9):2281-
In 2289 ", with cellulose, eucalyptus wood chip etc. for carbon source, carbon microspheres are prepared by hydro-thermal method and KOH activation.Li Yongfeng etc. is used
Coal is raw material, and carbon microspheres have been made in the condition for changing plasma, and the preparation process is tested in Arc plasma evaporation
(a kind of novel coal base spherical carbon and its formation mechenism Journal of Dalian University of Technology Total, 2002,42 (6) are completed on device:663-
668).Document is " with sucrose in Monodispersed hard carbon spherules with uniform nanopores "
For carbon source, it is dehydrated under confined conditions at 190 DEG C, carries out high temperature carbonization under an argon atmosphere, having prepared specific surface area is
400m2/ g monodispersed carbon microspheres.From the point of view of to sum up, the requirement of many preparation methods of carbon microspheres to experiment condition and equipment compared with
Height, significantly limits the commercialization process of carbon microsphere cathode material, and prepares most of presoma of carbon microspheres and be
The disagreeableness presoma of non-renewable or environment.So simplifying preparation technology, using the presoma of environmental protection, improving yield turns into charcoal
The direction of microballoon research.Starch source enriches, and cost is cheap, and by the oxidation processes of early stage, holding starch granules can be made
The carbon microspheres material of original spherical morphology, not only reduces balling technique difficulty, reduces the system of lithium ion battery negative material
Standby cost, and raw material is green renewable, alleviates the problem of fossil resource shortage.
Patent CN103647082A prepares hard charcoal microballoon at reduced pressure conditions, by low temperature stabilization, high temperature carbonization and born
Pole material, this method can avoid the caking phenomenon of carbon microspheres after charing, reduce the irreversible capacity of hard charcoal microballoon, improve material
Cyclical stability.The method is in order to eliminate the foaming caking phenomenon of carbon microspheres, it is necessary to for a long time at (8-100h) low temperature stabilization
Reason so that the preparation time of carbon microspheres is long, reduces preparation efficiency.Patent CN102364727A by starch base hard charcoal microballoon with
Expanded graphite is compound, forms artificial solid space conductive network structure, improves the voltage delay phenomenon of hard carbon material, improves
The efficiency first of material.Carbon microspheres and expanded graphite combination process are cumbersome in the method, and add being prepared into for material
This.
The content of the invention
For problems of the prior art, the present invention is intended to provide one kind is using starch as presoma, by adding iron
Powder stabilizes the time to prepare the method for the spherical carbon for negative electrode of lithium ion battery to shorten.
Technical scheme used in the present invention:A kind of preparation method of spherical carbon, is comprised the following steps that:
1st, raw starch is well mixed by a certain percentage with iron powder, carries out heating surely in 200-250 DEG C of temperature range
Fixedization pre-processes;
2nd, sample will be stabilized in step 1 to be placed in high temperature process furnances, under an inert atmosphere in 600-1200 DEG C of temperature model
Interior progress high temperature carbonization 0.5-3h is enclosed, carbonizing production is obtained after cooling;
3rd, by the carbonizing production pickling in step 2, it is washed with deionized water, filters, drying, obtains lithium ion battery spherical carbon
Negative material.
Preferably, the starch material in the step 1 be farina, cornstarch, wheaten starch, tapioca,
At least one of rice starch, starch from sweet potato, green starch.
Preferably, the iron powder in the step 1 is high-purity iron powder, and particle diameter is 300-1000 mesh.
Preferably, the mixed proportion of the starch in the step 1 and iron powder is 1:1-100:1.
Preferably, the stabilization processes time is 1-12h in the step 1.
Preferably, the inert atmosphere in step 2 is high pure nitrogen.
Preferably, the carbonization temperature in step 2 is 700-1000 DEG C.
Preferably, the carbonization time in step 2 is 1-2h.
Preferably, acid used in step 3 is 1% watery hydrochloric acid.
The present invention enriched with raw material sources, cost is low, and preparation flow is simple, it is pollution-free the features such as.By in starch
Add iron powder and carry out stabilization processes, starch granules is spaced from each other, under same stabilization temperature, starch can be avoided
Intergranular melt simultaneously, starch granules because of mutual accumulation the even phenomenon of uneven heating, substantially reduce when stabilizing early stage of starch
Between, economize on resources so that preparation efficiency is lifted.
Starch granules is spaced from each other by adding iron powder, is stabilized or charing process, starch granules is heated evenly,
Improve the uniformity of prepared sample.Operating procedure is simple, low for equipment requirements, is easy to extensive and prepares production.The present invention
The starch-based carbon microsphere spherical morphology of preparation is good, for lithium ion battery negative material show excellent cyclical stability with times
Rate performance.
Brief description of the drawings
Fig. 1 is SEM (SEM) figure of the raw materials used farina of the present invention.
Fig. 2 is the scanning electron microscope diagram of starch-based carbon microsphere negative material prepared by the embodiment of the present invention 1.
Fig. 3 is the scanning electron microscope diagram of starch-based carbon microsphere negative material prepared by comparative example 1 of the present invention.
Fig. 4 is cycle performance curve of the carbon microsphere cathode material of the preparation of embodiment 1 under 50mA/g current densities.
Fig. 5 is high rate performance curve of the carbon microsphere cathode material of the preparation of embodiment 1 under 0.05-2A/g current densities.
Embodiment
The present invention is described further by way of examples below, but is not construed as limiting the invention.
Embodiment 1
10g farinas and 10g iron powders are thoroughly mixed, mixture is put into Muffle furnace, in air atmosphere
Under, 230 DEG C of insulation 8h are risen to 5 DEG C/min heating rate, carry out stabilization processes, sample will be then stabilized and is put into retort
In, in a nitrogen atmosphere, 700 DEG C of holding 1h are warming up to 1.5 DEG C/min heating rate.Carbide is placed in beaker, added
The processing of 1% watery hydrochloric acid, then it is washed with deionized for several times, filters, drying, obtain farina based carbon microsphere, its particle diameter
Scope is 5.5-32.6 μm.
Gained carbon microspheres are used as lithium ion battery negative material assembled battery, test its cycle performance, high rate performance.Survey
Strip part is:25 DEG C, current density 0.05-2A/g, voltage range 0.01-3V.
As shown in Figure 5, gained carbon microspheres are used as lithium ion battery negative material, can under 50mA/g current density
Inverse specific capacity is 323.2mAh/g.Under 2A/g current densities, reversible specific capacity 82.7mAh/g.Cycle performance is excellent, works as electricity
When current density returns 50mA/g, reversible specific capacity reaches 336.3mAh/g.
Embodiment 2
10g farinas and 0.1g iron powders are thoroughly mixed, mixture is put into Muffle furnace, in air atmosphere
Under, 230 DEG C of insulation 8h are risen to 5 DEG C/min heating rate, carry out stabilization processes, sample will be then stabilized and is put into retort
In, in a nitrogen atmosphere, 700 DEG C of holding 1h are warming up to 1.5 DEG C/min heating rate.Carbide is placed in beaker, added
The processing of 1% watery hydrochloric acid, then it is washed with deionized for several times, filters, drying, obtain farina based carbon microsphere, its particle diameter
Scope is 6.0-30.66 μm.By the assembled battery of gained Carbon Materials and electrochemical property test is carried out, current density 50mAh/g
Under, first discharge specific capacity 645.6mAh/g, reversible specific capacity 350.5mAh/g, circulation 50 times after capability retention be
70%.
Embodiment 3
10g farinas and 1g iron powders are thoroughly mixed, mixture is put into Muffle furnace, in air atmosphere
Under, 230 DEG C of insulation 8h are risen to 5 DEG C/min heating rate, carry out stabilization processes, sample will be then stabilized and is put into retort
In, in a nitrogen atmosphere, 700 DEG C of holding 1h are warming up to 1.5 DEG C/min heating rate.Carbide is placed in beaker, added
The processing of 1% watery hydrochloric acid, then it is washed with deionized for several times, filters, drying, obtain farina based carbon microsphere.Its particle diameter
Scope is 3.9-28.13 μm.
Embodiment 4
10g farinas and 1g iron powders are thoroughly mixed, mixture is put into Muffle furnace, in air atmosphere
Under, 230 DEG C of insulation 12h are risen to 5 DEG C/min heating rate, carry out stabilization processes, sample will be then stabilized and is put into charing
In stove, in a nitrogen atmosphere, 700 DEG C of holding 1h are warming up to 1.5 DEG C/min heating rate.Carbide is placed in beaker,
Add 1% watery hydrochloric acid to handle, be then washed with deionized for several times, filter, drying, obtain farina based carbon microsphere.
Embodiment 5
10g farinas and 1g iron powders are thoroughly mixed, mixture is put into Muffle furnace, in air atmosphere
Under, 230 DEG C of insulation 2h are risen to 5 DEG C/min heating rate, carry out stabilization processes, sample will be then stabilized and is put into retort
In, in a nitrogen atmosphere, 700 DEG C of holding 1h are warming up to 1.5 DEG C/min heating rate.Carbide is placed in beaker, added
The processing of 1% watery hydrochloric acid, then it is washed with deionized for several times, filters, drying, obtain farina based carbon microsphere.
Embodiment 6
10g farinas and 1g iron powders are thoroughly mixed, mixture is put into Muffle furnace, in air atmosphere
Under, 230 DEG C of insulation 8h are risen to 5 DEG C/min heating rate, carry out stabilization processes, sample will be then stabilized and is put into retort
In, in a nitrogen atmosphere, 1000 DEG C of holding 1h are warming up to 1.5 DEG C/min heating rate.Carbide is placed in beaker, added
The processing of 1% watery hydrochloric acid, then it is washed with deionized for several times, filters, drying, obtain farina based carbon microsphere.Its particle diameter
Scope is 6-32 μm.
Embodiment 7
10g cornstarch and 10g iron powders are thoroughly mixed, mixture is put into Muffle furnace, in air atmosphere,
230 DEG C of insulation 8h are risen to 5 DEG C/min heating rate, carry out stabilization processes, sample will be then stabilized and is put into retort,
In a nitrogen atmosphere, 700 DEG C of holding 1h are warming up to 1.5 DEG C/min heating rate.Carbide is placed in beaker, adds 1%
Watery hydrochloric acid processing, then it is washed with deionized for several times, filters, drying, obtain corn starch base Carbon Materials.
Embodiment 8
10g wheaten starches and 10g iron powders are thoroughly mixed, mixture is put into Muffle furnace, in air atmosphere,
230 DEG C of insulation 8h are risen to 5 DEG C/min heating rate, carry out stabilization processes, sample will be then stabilized and is put into retort,
In a nitrogen atmosphere, 700 DEG C of holding 1h are warming up to 1.5 DEG C/min heating rate.Carbide is placed in beaker, adds 1%
Watery hydrochloric acid processing, then it is washed with deionized for several times, filters, drying, obtain wheaten starch base Carbon Materials.
Comparative example 1
10g farinas are put into Muffle furnace, in air atmosphere, 230 DEG C are risen to 5 DEG C/min heating rate
8h is incubated, carries out stabilization processes, sample will be then stabilized and is put into retort, in a nitrogen atmosphere, with 1.5 DEG C/min liter
Warm speed is warming up to 700 DEG C of holding 1h, obtains farina base Carbon Materials after cooling.This example compared with Example 1, by horse
The direct stabilization processes of bell sweet potato starch, in later stage carbonization process, starch granules melt and and adhesion phenomenon, fail to protect completely
Stay the spherical morphology of potato starch particle.
The section Example of the present invention is illustrated above, but the present invention is not limited to implementation described above
Example, those skilled in the art can make equivalent modification or replacement on the premise of without prejudice to spirit of the invention, these
Equivalent modification or replacement is all contained in the application claim limited range.
Claims (7)
1. a kind of spherical carbon cathode material of lithium ion battery, grain diameter is 2-40 μm, it is characterised in that is comprised the following steps:
(1) starch material and iron powder are sufficiently mixed uniformly by a certain percentage, mixture entered in 200-250 DEG C of temperature range
Row heat stabilization pre-processes;
(2) sample will be stabilized in step (1) to be placed under inert atmosphere in high temperature carbonization 0.5- in 600-1200 DEG C of temperature range
3h, carbonizing production is obtained after cooling;
(3) by the carbide pickling in step (2), it is washed with deionized water, filters, drying, obtains lithium ion battery spherical carbon and bear
Pole material.
A kind of 2. preparation method of the spherical carbon cathode material of lithium ion battery according to claim 1, it is characterised in that:Institute
The iron powder stated is high-purity iron powder, and particle diameter is 300-1000 mesh.
A kind of 3. preparation method of the spherical carbon cathode material of lithium ion battery according to claim 1, it is characterised in that:Step
Suddenly the mixed proportion of the starch described in (1) and iron powder is 1:1-500:1, preferable mixed proportion is 1:1-100:1.
A kind of 4. preparation method of the spherical carbon cathode material of lithium ion battery according to claim 1, it is characterised in that:
Starch material described in step (1) is farina, cornstarch, wheaten starch, tapioca, rice starch and green
At least one of beans starch.
A kind of 5. preparation method of the spherical carbon cathode material of lithium ion battery according to claim 1, it is characterised in that:
The stabilisation time described in step (1) is 1-12h.
A kind of 6. preparation method of the spherical carbon cathode material of lithium ion battery according to claim 1, it is characterised in that:
Carbonization time described in step (2) is 0.5-3h, and preferable carbonization time is 1-2h.
A kind of 7. preparation method of the spherical carbon cathode material of lithium ion battery according to claim 1, it is characterised in that:
Acid described in step (3) is 1% watery hydrochloric acid.
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Cited By (6)
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CN109103440A (en) * | 2018-04-08 | 2018-12-28 | 毛强平 | A kind of lithium ion battery negative material, preparation method and lithium ion battery |
CN109686975A (en) * | 2018-12-05 | 2019-04-26 | 桑德集团有限公司 | A kind of hard charcoal negative electrode material and preparation method thereof |
CN113224300A (en) * | 2021-04-15 | 2021-08-06 | 淄博火炬能源有限责任公司 | Preparation method of lead powder for negative electrode of lead-carbon battery |
CN114988391A (en) * | 2022-06-29 | 2022-09-02 | 宜昌邦普循环科技有限公司 | Preparation method and application of hard carbon negative electrode material |
CN115602838A (en) * | 2022-10-21 | 2023-01-13 | 南自通华(南京)智能电气有限公司(Cn) | Spherical carbon negative electrode material of lithium ion battery and preparation method thereof |
GB2623150A (en) * | 2022-06-29 | 2024-04-10 | Yichang Brunp Recycling Tech Co Ltd | Preparation method for hard carbon negative electrode material, and use of preparation method |
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CN109686975A (en) * | 2018-12-05 | 2019-04-26 | 桑德集团有限公司 | A kind of hard charcoal negative electrode material and preparation method thereof |
CN113224300A (en) * | 2021-04-15 | 2021-08-06 | 淄博火炬能源有限责任公司 | Preparation method of lead powder for negative electrode of lead-carbon battery |
CN114988391A (en) * | 2022-06-29 | 2022-09-02 | 宜昌邦普循环科技有限公司 | Preparation method and application of hard carbon negative electrode material |
CN114988391B (en) * | 2022-06-29 | 2023-04-11 | 宜昌邦普循环科技有限公司 | Preparation method and application of hard carbon negative electrode material |
WO2024000817A1 (en) * | 2022-06-29 | 2024-01-04 | 宜昌邦普循环科技有限公司 | Preparation method for hard carbon negative electrode material, and use of preparation method |
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CN115602838A (en) * | 2022-10-21 | 2023-01-13 | 南自通华(南京)智能电气有限公司(Cn) | Spherical carbon negative electrode material of lithium ion battery and preparation method thereof |
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