CN110061237A - A kind of amorphous carbon cell negative electrode material and its preparation method and application - Google Patents
A kind of amorphous carbon cell negative electrode material and its preparation method and application Download PDFInfo
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- CN110061237A CN110061237A CN201910340717.3A CN201910340717A CN110061237A CN 110061237 A CN110061237 A CN 110061237A CN 201910340717 A CN201910340717 A CN 201910340717A CN 110061237 A CN110061237 A CN 110061237A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The present invention relates to battery material technical fields more particularly to a kind of amorphous carbon cell negative electrode material and its preparation method and application.The invention discloses a kind of preparation methods of amorphous carbon cell negative electrode material, comprising the following steps: carbon source and ball milling pearl are carried out ball milling, obtain amorphous carbon cell negative electrode material；The revolving speed of ball milling is 400~1000r/min.The preparation method of the amorphous carbon cell negative electrode material is simple, cost is relatively low, and the amorphous carbon cell negative electrode material being prepared is good to sodium ion/lithium ion deintercalation effect, provides a large amount of space for the storage of sodium ion/lithium ion and provides higher specific capacity, and good cycle.
Description
Technical field
The present invention relates to battery material technical field more particularly to a kind of amorphous carbon cell negative electrode material and its preparation sides
Method and application.
Background technique
Fossil energy is currently by most widely used energy resources.And the use nature of the energy is needed in view of accumulation of energy
Technology.Instantly, secondary cell is considered as most promising storage because of its flexibility, high-energy source transfer efficiency and simple later maintenance
Can technology, and main use lithium ion battery in industrial production and life at present.But as the demand to lithium is continuous
Increase, the price of lithium also persistently skyrockets.In addition, lithium is not a kind of resource abundant.According to the calculating of stakeholder, at present
The lithium resource having on ball can only continue to use most 65 years, this will greatly limit the sustainable development of all kinds of industries.At this point,
Urgently more agree with environment instantly and resource, the energy-storage battery system that can be actually widely used in industrial production and life.And sodium
The best breach that ion battery is.
Sodium has wide endless distribution as element abundant the fourth-largest on the earth.Although sodium is in discharge voltage, storage
It deposits and is partial to disadvantage compared to lithium in condition, weight and volume, but the characteristics such as its abundance, cheap, environmental-friendly are also
It is very prominent.In addition, in terms of battery component and electric memory mechanism, the basic phase of the theory of sodium-ion battery and lithium ion battery
Together, so conversion between the two can't have larger problem.
Currently, the preparation step of anode material of lithium-ion battery is more, and energy consumption is high.
Summary of the invention
In view of this, the present invention provides a kind of amorphous carbon cell negative electrode material and its preparation method and application, the nothing
The preparation method for the carbon battery negative electrode material that shapes is simple, and cost is relatively low, and the amorphous carbon cell negative electrode material pair being prepared
Sodium ion/lithium ion deintercalation effect is good, provides a large amount of space and specific capacity, and good cycle for the storage of sodium ion.
Its specific technical solution is as follows:
The present invention provides a kind of preparation methods of amorphous carbon cell negative electrode material, comprising the following steps:
Carbon source and ball milling pearl are subjected to ball milling, obtain amorphous carbon cell negative electrode material；
The revolving speed of the ball milling be 400~1000r/min, more preferably 400~500r/min, further preferably
450r/min。
Hard carbon can promote the reversible deintercalation of sodium and lithium ion, extend the service life of battery, and due to biggish interlayer
Away from and scrambling, hard carbon can provide good embedding off line system for sodium ion, in addition, carbon base body has lithium/sodium-ion battery
Good electro-chemical activity.
In the present invention, the ball milling is high-energy ball milling.Compared to general milling, high-energy ball-milling process is capable of providing higher
Energy to be conducive to the progress of preparation, and can be shortened preparation time.The ball milling specifically: every ball milling 60min stops
Ball milling 30min guarantees the heat dissipation of ball mill.
In the prior art, the preparation of amorphous carbon cell negative electrode material needs chemically synthesized method mostly and carries out high temperature
Processing, above method synthesis step is more, and energy consumption is high, and surfactant is needed to be assisted.In the present invention, without at high temperature
Reason, it is only necessary to which carbon source, which is carried out the processing of high energy ball milling physical condition, can be obtained amorphous carbon.
Preferably, the time of the ball milling is 5~40h, more preferably 15-30h, further preferably 20h.
Preferably, the mass ratio of the carbon source and the ball milling pearl is 1:15~1:40, and more preferably 1:25-1:40 is into one
Step is preferably 1:30.In the present invention, the additional amount of carbon source is 5-50g.
Preferably, the carbon source and the volume of ball milling pearl are the 1/5~1/3 of the ball milling tank volume that the ball milling uses, more
Preferably 1/4.
In the present invention, the carbon source is added in ball grinder together with the ball milling pearl, and by the air displacement in ball grinder
At inert gas, high-energy ball milling is then carried out again；Inert gas is preferably argon gas (Ar)；Ball milling pearl is preferably iron ball；Ball grinder
Material be preferably stainless steel, tungsten carbide or zirconium oxide；The volume of ball grinder is 200-1000mL.
Preferably, the carbon source includes natural graphite, artificial graphite, graphene, Pintsch process carbon, acetylene black, interphase
One of carbosphere, petroleum coke, carbon fiber and thermal decomposed resins carbon are a variety of, more preferably natural graphite.
The present invention also provides amorphous carbon cell negative electrode materials made from above-mentioned preparation method.
In the present invention, amorphous carbon cell negative electrode material is the carbon material with certain non-crystallization degree, passes through high energy ball
The structure of the original rule of carbon source is deformed and has been reset by mill, and original layer structure is disturbed, and is formed more serious
Plicated layer structure, since biggish displacement has occurred in atom site in material original structure, the interlamellar spacing of material becomes larger, by
Big in the radius ratio lithium ion of sodium ion, the interlamellar spacing before material ball milling is smaller relative to sodium ion, can be used for the embedding of lithium ion
Enter abjection, but is unfavorable for the insertion and abjection of sodium ion.Interlamellar spacing becomes larger after ball-milling treatment, which is conducive to sodium ion or lithium
Insertion and abjection of the ion in charge and discharge process, preferably sodium ion.Compared to lithium ion battery, agraphitic carbon cathode is more suitable
Closing sodium-ion battery is because sodium-ion battery radius is larger, it is easier to insertion abjection is carried out in agraphitic carbon.
The present invention also provides a kind of sodium ion/negative electrode of lithium ion battery, including collector, binder and negative electrode active material
The bed of material；
The anode active material layer is bonded at least one surface of the collector by the binder；
The anode active material layer is above-mentioned amorphous carbon cell negative electrode material.
In the present invention, collector is preferably one of copper foil, aluminium foil, nickel foil, copper mesh, aluminium net and nickel screen or a variety of, more
Preferably copper foil；Binder is preferably Kynoar, polytetrafluoroethylene (PTFE), Lithium polyacrylate lithium, polyvinyl alcohol, carboxymethyl cellulose
One of plain sodium, polyurethane and butadiene-styrene rubber are a variety of, more preferably polypropylene lithium.
It is 660mAh/g through 400 that negative electrode active material stores up the specific capacity of sodium for the first time in the present invention, in sodium-ion battery cathode
After circle circulation, specific capacity 200mAh/g, and remain the coulombic efficiency close to 99.99%.
The present invention also provides a kind of sodium ion/lithium ion batteries, including anode and cathode；
The cathode is above-mentioned sodium ion/negative electrode of lithium ion battery.
In the present invention, just extremely vanadium phosphate sodium or the Prussian of sodium-ion battery are not specifically limited herein.
As can be seen from the above technical solutions, the invention has the following advantages that
The present invention provides a kind of preparation methods of amorphous carbon cell negative electrode material, comprising the following steps:
Carbon source and ball milling pearl are subjected to ball milling, obtain amorphous carbon cell negative electrode material；The revolving speed of ball milling be 400~
1000r/min。
Cost is relatively low for above-mentioned preparation method, and raw material sources are extensive, easy to operate, and preparation efficiency is high, and carbon source is carried out high energy
Ball milling can obtain amorphous carbon cell negative electrode material, the decrystallized carbon material of the negative electrode material, by high-energy ball milling, by carbon
The structure of the original rule in source is deformed and has been reset, and original layer structure is disturbed, and forms more serious plicated layer
Structure, which is conducive to the insertion and abjection of sodium ion or lithium ion in charge and discharge process, so as to depositing for sodium ion
Storage provides a large amount of space and then promotes specific capacity.By experimental data it is found that the negative electrode material is deformed into seriously by layer structure
Plicated layer structure, and as sodium-ion battery cathode when specific capacity with higher, and good cycle.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other attached drawings according to these attached drawings.
Fig. 1 is the agraphitic carbon cell negative electrode material X-ray diffraction test result that the embodiment of the present invention 1 provides；
Fig. 2 is the agraphitic carbon cell negative electrode material transmissioning electric mirror test result that the embodiment of the present invention 1 provides；
Fig. 3 is the cycle performance test result for the sodium-ion battery cathode that the embodiment of the present invention 3 and comparative example 1 provide.
Specific embodiment
It in order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below will be to of the invention real
The technical solution applied in example is clearly and completely described, it is clear that the embodiments described below are only present invention a part
Embodiment, and not all embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creation
Property labour under the premise of all other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
The present embodiment is the preparation of agraphitic carbon cell negative electrode material
5 grams of graphite and 5 grams of acetylene blacks are weighed, its iron ball for being 10 centimetres with 40 diameters is put into togerther ball grinder
In, ball grinder is transferred in argon gas glove box and is sealed.Taking-up, is carried out ball milling, drum's speed of rotation is set as after having sealed
500 rpms, stop 30 minutes within every ball milling 1 hour, after running 20 times repeatedly by agraphitic carbon cell negative electrode material and
Ball separation, obtains agraphitic carbon cell negative electrode material.
Embodiment 2
1 agraphitic carbon cell negative electrode material of embodiment is subjected to X-ray diffraction test and transmissioning electric mirror test to analyze material
The state of material.
Fig. 1 is the X-ray diffraction test result figure of 1 agraphitic carbon cell negative electrode material of the embodiment of the present invention, compared to mark
Quasi- graphite material X-ray diffraction standard diagram (PDF#65-6212), the amorphous carbon material X-ray diffraction material as the result is shown
Material is decrystallized carbon material, and shows that the material upsets graphite and the layer structure itself having, and has been made it have
Conducive to the characteristic of insertion and the abjection of the sodium ion bigger than lithium ion, so as to improve the specific capacity of material.
Fig. 2 is the transmission electron microscope picture of 1 agraphitic carbon cell negative electrode material of the embodiment of the present invention, passes through the observation of transmission electron microscope
The plicated layer structure that material has following deformation more serious can be intuitively found out from pattern, compared to Fig. 2 upper right footmark
The ordered structure of meta anthracite, for agraphitic carbon since the arrangement of atom deviates original position, interlamellar spacing is greater than the original layer of graphite
Spacing, this is because having been carried out the originally regular structure of material by the method for mechanical force during high-energy ball milling
It deformation and resets.This makes the structure be more advantageous to insertion and abjection of the sodium ion in charge and discharge process simultaneously.
Embodiment 3
The present embodiment is the preparation of sodium-ion battery cathode.
The agraphitic carbon cell negative electrode material and Li- that a certain amount of embodiment 1 provides are weighed according to the ratio of mass ratio 9:1
PAA binder weighs 135 milligrams of agraphitic carbon cathode herein, and 0.3 milliliter of Li-PAA binder solution is (in 0.3 milliliter of binder
Contain 15 milligrams of Li-PAA after solvent volatilization, wherein the specific ingredient of binder and concentration are to contain 1 milligram of Li- in every 0.02 milliliter of water
PAA).On copper foil after agraphitic carbon and binder are sufficiently mixed uniformly coated on 9 millimeters thicks, done under 60 degree of vacuum conditions
It is taken out after dry 12 hours, obtains sodium-ion battery cathode.
Comparative example 1
This comparative example difference from Example 3 is to obtain using graphite material as anode material of lithium-ion battery
Sodium-ion battery cathode.
Embodiment 4
The sodium-ion battery cathode of embodiment 3 and comparative example 1 is subjected to cycle performance test.
Fig. 3 is the cycle performance test result figure of 1 sodium-ion battery cathode of the embodiment of the present invention 3 and comparative example, Cong Tuzhong
As can be seen that the sodium process of storage for the first time of the material shows the specific capacity of 660mAh/g, and graphite only has 60mAh/g, and
Hereafter specific capacity has been maintained 200mAh/g in 400 circle circulations, and has remain the coulombic efficiency close to 99.99%.Without fixed
Coulombic efficiency is also apparently higher than graphite to the cathode of type carbon battery for the first time, this greatly meets in practical application to battery material
It is required that.
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features；And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of amorphous carbon cell negative electrode material, which comprises the following steps:
Carbon source and ball milling pearl are subjected to ball milling, obtain amorphous carbon cell negative electrode material；
The revolving speed of the ball milling is 400~1000r/min.
2. the preparation method of amorphous carbon cell negative electrode material according to claim 1, which is characterized in that the carbon source with
The mass ratio of the ball milling pearl is 1:15~1:40.
3. the preparation method of amorphous carbon cell negative electrode material according to claim 1, which is characterized in that the ball milling
Time is 5~40h.
4. the preparation method of amorphous carbon cell negative electrode material according to claim 3, which is characterized in that the ball milling
Revolving speed is 400~500r/min, and the time of the ball milling is 15~30h.
5. the preparation method of amorphous carbon cell negative electrode material according to claim 2, which is characterized in that the carbon source with
The mass ratio of the ball milling pearl is 1:25~1:40.
6. the preparation method of amorphous carbon cell negative electrode material according to claim 1, which is characterized in that the carbon source packet
Include natural graphite, artificial graphite, graphene, Pintsch process carbon, acetylene black, carbonaceous mesophase spherules, petroleum coke, carbon fiber and pyrolysis
One of resin carbon is a variety of.
7. the preparation method of amorphous carbon cell negative electrode material according to claim 3, the ball milling specifically: every ball milling
60min stops ball milling 30min.
8. amorphous carbon cell negative electrode material made from preparation method described in claim 1 to 7 any one.
9. a kind of sodium ion/negative electrode of lithium ion battery, which is characterized in that including collector, binder and anode active material layer；
The anode active material layer is bonded at least one surface of the collector by the binder；
The anode active material layer is amorphous carbon cell negative electrode material according to any one of claims 8.
10. a kind of sodium ion/lithium ion battery, which is characterized in that including anode and cathode；
The cathode is sodium ion/negative electrode of lithium ion battery as claimed in claim 9.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111200126A (en) * | 2020-01-17 | 2020-05-26 | 三峡大学 | Preparation method of amorphous tin/carbon material as lithium ion battery negative electrode material |
| CN114604847A (en) * | 2022-02-28 | 2022-06-10 | 武汉理工大学 | Method for preparing amorphous carbon through heterogeneous atom doping and application |
| CN115881895A (en) * | 2021-09-27 | 2023-03-31 | 天津理工大学 | Amorphous carbon negative electrode material and preparation method and application thereof |
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| CN103337605A (en) * | 2013-07-22 | 2013-10-02 | 深圳市斯诺实业发展有限公司永丰县分公司 | Method for preparing natural graphite cathode material of lithium ion battery by wet ball milling |
| CN105789608A (en) * | 2016-03-29 | 2016-07-20 | 华南师范大学 | Preparation method and application of Si/MnO2/graphene/carbon lithium ion battery anode material |
| CN108358188A (en) * | 2018-01-24 | 2018-08-03 | 西安交通大学 | A kind of secondary cell carbon negative pole material and preparation method thereof |
| CN109599546A (en) * | 2018-12-05 | 2019-04-09 | 中南大学 | Asphalt carbon-coated natural mixed graphite material and method for preparing lithium ion battery cathode by using same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103337605A (en) * | 2013-07-22 | 2013-10-02 | 深圳市斯诺实业发展有限公司永丰县分公司 | Method for preparing natural graphite cathode material of lithium ion battery by wet ball milling |
| CN105789608A (en) * | 2016-03-29 | 2016-07-20 | 华南师范大学 | Preparation method and application of Si/MnO2/graphene/carbon lithium ion battery anode material |
| CN108358188A (en) * | 2018-01-24 | 2018-08-03 | 西安交通大学 | A kind of secondary cell carbon negative pole material and preparation method thereof |
| CN109599546A (en) * | 2018-12-05 | 2019-04-09 | 中南大学 | Asphalt carbon-coated natural mixed graphite material and method for preparing lithium ion battery cathode by using same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111200126A (en) * | 2020-01-17 | 2020-05-26 | 三峡大学 | Preparation method of amorphous tin/carbon material as lithium ion battery negative electrode material |
| CN115881895A (en) * | 2021-09-27 | 2023-03-31 | 天津理工大学 | Amorphous carbon negative electrode material and preparation method and application thereof |
| CN114604847A (en) * | 2022-02-28 | 2022-06-10 | 武汉理工大学 | Method for preparing amorphous carbon through heterogeneous atom doping and application |
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