CN106058190A - Preparation method for high-capacity anode material for lithium ion battery - Google Patents
Preparation method for high-capacity anode material for lithium ion battery Download PDFInfo
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- CN106058190A CN106058190A CN201610566813.6A CN201610566813A CN106058190A CN 106058190 A CN106058190 A CN 106058190A CN 201610566813 A CN201610566813 A CN 201610566813A CN 106058190 A CN106058190 A CN 106058190A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
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- 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 invention relates to a method for synthesizing a high-capacity core-shell structural anode material for a lithium ion battery. The method comprises the following steps: placing a proper amount of intermediate-phase carbon microspheres, pitch coke, needle coke or artificial graphite in a ball milling jar respectively, then adding a proper amount of fumed silica, performing uniform mixing on such a basis, and performing ball milling in all directions for a proper time at proper rotating speed and ball-material ratio; wrapping the surface of a product with a layer of amorphous carbon after ball milling, and carrying out high-temperature carbonization. The product is a high-capacity core-shell structural anode material employing high-capacity nanoparticles as an outer wrapping layer and employing the relatively harder needle coke, pitch coke, intermediate-phase carbon microspheres or artificial graphite as an inner core. Compared with a conventional synthesis process, the method has the advantages of extensive industrial sources, simple process conditions, high electrochemical performance and the like.
Description
Technical field
The invention belongs to lithium ion battery material technical field, relate generally to a kind of lithium ion battery high power capacity negative pole material
The preparation method of material.
Background technology
Business-like lithium ion battery is typically with graphite carbons as negative pole, but with electric automobile and the pole of energy storage technology
Great development, business-like lithium ion battery is no longer able to meet the production of new and high technology and application requirement, high-energy-density
Negative material becomes enterprise and the target of each laboratory searching and the direction of research already.Silicon content occupies second and silicon
Material rich content on earth, silicon is the novel energy material that most probable substitutes material with carbon element.
Along with going deep into of research, we can find that silicon materials can form Li during removal lithium embedded12Si7、Li15Si4、
Li22Si5Deng alloy, more there is Li4.4Si alloy has the advantage such as high power capacity, low removal lithium embedded current potential.But it has been found that silicon
When embedding lithium, volume change is up to 300%, causes material efflorescence in charge and discharge process, can not between active material and collector
Effectively contact, electrode structure destroys, thus causes cycle performance to decline to a great extent, secondly, the electronic conductivity of silicon and ionic conductance
Rate is the most relatively low, and can not be at LiPF6Electrolyte is formed stable solid electrolyte film.These shortcomings limit silicon at business lithium
Application in ion battery.
Solve or buffering problems proposes the nanorize of multiple method, such as silicon, Si/C composite, Si-metal
Composite with Si-nonmetal oxide.But this type of method or relatively costly, or it is not suitable with commercial production, simply stop
Stay the experimental stage.In recent years, the research of silicon dioxide achieved some breakthroughs in terms of lithium ion battery, in removal lithium embedded process
In, SiO2With Li, chemical reaction can occur, the formation silicon that can attach during generating positive Lithium metasilicate and lithium bisilicate.So
Hope is brought to our research.And the stability of silicon dioxide structure and the inertness of material, can effectively buffer
Volumetric expansion and the destruction avoiding electrode structure, thus reach to improve capacity and the purpose of cyclical stability.
Summary of the invention
The present invention is technically characterized in that aerosil (white carbon, particle diameter 7-40nm) by ball milling integration technology
It is coated on the surface of MCMB, pitch coke, needle coke or Delanium, and uses the material such as Colophonium, resin at its table
One layer of agraphitic carbon of cladding is continued in face, ultimately form with electric conductivity preferably, needle coke that Mohs' hardness is higher, pitch coke, centre
Phase carbon microspheres or the new type structure of hud composite that Delanium is kernel.The present invention can be by nano level gas phase titanium dioxide
Silicon is coated on MCMB, pitch coke, needle coke or Delanium surface, increases silicon dioxide granule and material with carbon element
Contact area, has effectively buffered the bulk effect during charge and discharge cycles, improves its cycle performance, simultaneously because gas
The existence of aerosil, improves the reversible capacity of this composite, has given full play to aerosil nanoparticle high
Capacity and the feature of material with carbon element stable circulation.
For achieving the above object, the invention discloses following technology contents: about the compound shared proportion of bi-material,
The method of ball milling and the preparation method of nucleocapsid structure.
The preparation method of a kind of lithium ion battery high-capacity cathode material, it is characterised in that carry out by the steps:
(1) first take appropriate carbon source and put in ball grinder, and then aerosil is added, be allowed to mix all with carbon source
Even, aerosil proportion in the mixture is: 5-70%；Place into the quality of Achates bead, Achates bead and feed liquid
Portion rate is 30:1, and then with Ball-milling Time 1-20h, rotating speed 200-1000rpm carries out comprehensive ball milling；Described carbon source refers to
It is: MCMB, pitch coke, needle coke or Delanium；
(2) product after ball milling passes through vapour deposition or the liquid phase method composite wood at its one layer of agraphitic carbon of Surface coating subsequently
Material；Covering amount 0% 20%(w/ w), preferred covering amount is 10%.The precursor material of described agraphitic carbon refers to: breast
Change Colophonium or resin；
(3) by product carbonization in atmosphere furnace, heating rate is 1-15 DEG C/min, and carburizing temperature is 600 DEG C-1200 DEG C, insulation
Time is 1h-12h.
The preferred aerosil of the present invention and the matter of the carbon microspheres of mesophase carbon source, green coke, needle coke or Delanium
Amount is than respectively 7:3,5:5,3:7 and 1:9.
The present invention further discloses the preparation method of lithium ion battery high-capacity cathode material and is improving lithium ion
Battery capacity improves the application in terms of cycle performance.Experimental result shows:
(1) simple do not carry out the needle coke of ball milling, carbonaceous mesophase spherules, the specific capacity of artificial graphite material are 100 mAh/g
To 300mAh/g
(2) the negative material initial specific capacities using the inventive method to prepare is 500mAh/g to 1000mAh/g, circulates 140
Zhou Yihou capacity is the most significantly decayed.
More detailed description of the present invention is as follows:
First appropriate MCMB, pitch coke, needle coke or Delanium are put in ball grinder, and then by gas phase two
Silicon oxide adds, and additional proportion scope is 5% to 70%, is merged by bi-material high speed ball milling on this basis.Due to needle coke
Higher Deng material with carbon element Mohs' hardness, particle diameter is distributed in 6 to 30 microns, and aerosil has, and particle diameter is little, specific surface area
Greatly, superficial attractive forces is strong, dispersive property good, chemical purity high, so in the middle of comprehensive ball milling fusion process, gas phase
Silicon dioxide granule is easily coated on carbon core surface, then passes through vapour deposition or liquid phase method in one layer of Colophonium of its Surface coating or tree
Fat, covering amount is 0-20%(preferably 10% agraphitic carbon covering amount, and the amorphous carbon presoma of cladding is emulsified asphalt).By product
Carbonization in atmosphere furnace, heating rate is 1-15 DEG C/min, and carburizing temperature is 600 DEG C-1200 DEG C, and temperature retention time is 1h-12h.
This product is with high power capacity nanoparticle as clad, needle coke, green coke, MCMB or the Delanium that hardness is higher
Nucleocapsid structure negative material for the high power capacity of kernel.This composite material of core-shell structure is conducive to lifting and the cyclicity of its capacity
The improvement of energy.
The present invention is simple to operate, and required condition easily reaches, and experimental raw used is technical grade material, in industry
It is easily achieved in application, the nucleocapsid knot with excellent cycling performance that specific capacity is 400mAh/g to 1000mAh/g can be prepared
Structure Novel anode material.
Accompanying drawing illustrates:
Fig. 1 be embodiments of the invention 1 through 900 DEG C, 3 hours process, do not carry out the SEM picture of the needle coke of ball milling.
Fig. 2 is that in embodiments of the invention 1, needle coke does not carries out ball milling, through 900 DEG C, and the electrochemistry processed for 3 hours
Can picture；
Fig. 3 be the addition of embodiments of the invention 2 aerosil be 70%, ratio of grinding media to material 30:1, rotating speed 500rpm, ball milling
Carry out 900 DEG C of carbonizations after time 20h, be incubated the SEM picture of 3 hours；
Fig. 4 be embodiments of the invention 3 aerosil addition be 70%, ratio of grinding media to material 30:1, rotating speed 500rpm, ball milling time
Between after 20 h, products therefrom carries out liquid phase method at its Surface coating one coating emulsified asphalt, carries out 900 DEG C of carbonizations subsequently, and insulation 3 is little
Time SEM picture；
Fig. 5 is the matched group experiment of embodiments of the invention 3, and other conditions are same as Example 3, simply the addition of aerosil
Amount is the SEM picture of 50%；
Fig. 6 is the matched group experiment of embodiments of the invention 3, and other conditions are same as Example 3, simply the addition of aerosil
Amount is the SEM picture of 30%；
Fig. 7 is the matched group experiment of embodiments of the invention 3, and other conditions are same as Example 3, simply the addition of aerosil
Amount is the SEM picture of 10%；
Fig. 8 is the chemical property picture that embodiments of the invention 3 obtain composite material of core-shell structure；
Fig. 9 is the EDS Mapping of the nucleocapsid clad structure of embodiments of the invention 3 preparation；
Figure 10 is the TEM picture of the nucleocapsid clad structure of embodiments of the invention 3 preparation.
Detailed description of the invention
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.It addition, embodiment is interpreted as illustrative, and the unrestricted present invention
Scope, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this
On the premise of invention spirit and scope, the various changes carrying out the material component in these embodiments and consumption or change are also
Belong to protection scope of the present invention.The present invention is raw materials used and reagent is commercially available.
In order to contrast with the present invention, embodiment 1 gives through 900 DEG C, and process in 3 hours does not carries out high-energy ball milling
Needle coke (Fig. 1), illustrates: the needle coke after ball milling is that particle diameter is at 15 microns, the granule of surface smoother.Embodiment 1
Give through 900 DEG C, the chemical property figure (Fig. 2) processing the needle coke not carrying out high-energy ball milling in 3 hours, illustrate: carry out
The capacity not carrying out ball milling needle coke after high-temperature process only has about 270mAh/g.
Embodiment 2 gives the SEM photograph (Fig. 3) after aerosil and the comprehensive ball milling of needle coke high energy, and this is
The pattern picture of the composite that ball milling is later, can intuitively prove that the aerosil of Nano grade is attached to needle coke table
Face..
After embodiment 3 gives aerosil and needle coke ball milling, appearance is coated with one layer of agraphitic carbon again with laggard
900 DEG C of high temperature of row, temperature retention time 3 hours (Fig. 4, white carbon shared by content 70%) illustrates, again cladding add silicon dioxide with
The contact area of carbon source, makes nucleocapsid structure more reliable and more stable, makes battery material surface in cyclic process be not easy to come off, presses down
Powder process.And other conditions are same as Example 3, the SEM photograph (figure that simply needle coke is different with the mass ratio of aerosil
5, Fig. 6, Fig. 7), this is the contrast experiment of covering amount of different aerosils, and the gas phase dioxy of different covering amount is described
SiClx can be coated to the surface of needle coke.
Embodiment 3 gives after carrying out ball milling, then one layer of agraphitic carbon of its Surface coating (covering amount is 10%), subsequently
900 DEG C of carbonizations, are incubated composite chemical property figure (Fig. 8) of 3 hours gained nucleocapsid structures, illustrate: at circulation 140 circle
After, the battery specific capacity of this composite is maintained at about 570mAh/g, and stability is preferable, than the material ratio in embodiment 1
Capacity has had significant raising.Embodiment 3 gives the EDS Mapping (Fig. 9) of the nucleocapsid structure prepared, and this kind is described
Composite comprises element in carbon, silicon, oxygen 3 and aerosil and the needle coke structure composite with nucleocapsid.And prepare
The TEM picture (Figure 10) of composite material of core-shell structure illustrate after carrying out high-energy ball milling, aerosil nano-particle
It is coated on needle coke surface and cladding thickness is about 20nm.
Embodiment 1
Preprepared needle coke is laid in the middle of porcelain boat, porcelain boat is put into tube furnace and tube furnace is passed through the argon of flowing
Gas, rises to 200 DEG C with the time of 40 minutes by temperature subsequently, is incubated 40 minutes often, secondly with the heating rate liter of 5 DEG C/min
Temperature, to 900 DEG C, is incubated duration 3 hours.Naturally cool to room temperature stand-by.
Embodiment 2
First ready 0.3g needle coke is put in the middle of ball grinder, add the gas phase titanium dioxide accounting for total content 70% and then
Silicon, is allowed to uniformly mix with needle coke, and placing into ratio of grinding media to material is 30:1, and quality is the Achates bead of the 4mm of 30g, then with ball
Time consuming 20h, rotating speed 500rpm carry out comprehensive ball milling, and products therefrom is stand-by
Embodiment 3
Products therefrom in embodiment 2 is carried out liquid phase method one layer of agraphitic carbon (forerunner of selected agraphitic carbon of external sheath
Body is emulsified asphalt), the product in embodiment 2 is put in beaker and stirs, be slowly added dropwise emulsified asphalt, subsequently at a high speed
Stir and make solution mix homogeneously in 15 hours.Solution is poured in the middle of porcelain boat, put into 12h in vacuum drying oven, 100 DEG C of drying.With
After porcelain boat put into high temperature process furnances and is passed through argon, temperature rises to 200 DEG C, and insulation duration 40 minutes, then with 5 DEG C/min
Heating rate be warming up to 900 DEG C of carbonizations, insulation duration 3 hours, natural cooling is stand-by, obtains amorphous carbon gas phase titanium dioxide
The composite of silicon needle coke nucleocapsid structure.
The control experiment of embodiment 3:
Change total amount (50%, 30%, 10%) shared by aerosil, carry out comprehensive high-energy ball milling, carry out liquid phase method subsequently and exist
One layer of agraphitic carbon of its Surface coating (identical with carbon source in embodiment 3, covering amount is 10%), high temperature cabonization.Natural cooling is treated
With.
Claims (4)
1. the preparation method of a lithium ion battery high-capacity cathode material, it is characterised in that carry out by the steps:
(1) first take appropriate carbon source and put in ball grinder, and then aerosil is added, be allowed to mix all with carbon source
Even, wherein, aerosil proportion in the mixture is: 5% 70%；Place into Achates bead, Achates bead and thing
The mass ratio of material is 30:1, and then with Ball-milling Time 1-20h, rotating speed 200-1000rpm carries out comprehensive ball milling；Described carbon
Source refers to: MCMB, pitch coke, needle coke or Delanium；
(2) product after ball milling passes through vapour deposition or the liquid phase method composite wood at its one layer of agraphitic carbon of Surface coating subsequently
Material；Covering amount is 0% 20%(w/ w)；The precursor material of described agraphitic carbon refers to: emulsified asphalt or resin；
(3) by product carbonization in atmosphere furnace, heating rate is 1-15 DEG C/min, and carburizing temperature is 600 DEG C-1200 DEG C, insulation
Time is 1h-12h.
2. the preparation method described in claim 1, wherein the covering amount of step (2) is 10%(w/ w).
3. the preparation method described in claim 1, aerosil and the carbon microspheres of mesophase carbon source, green coke, needle coke or
The mass ratio of Delanium is respectively 7:3,5:5,3:7 and 1:9.
4. the preparation method of lithium ion battery high-capacity cathode material described in claim 1 is improving the specific volume of lithium ion battery
Amount, improve the application in terms of cycle performance.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107046125A (en) * | 2017-02-22 | 2017-08-15 | 深圳市金润能源材料有限公司 | Silicon-carbon composite cathode and preparation method thereof and lithium ion battery |
| CN107394162A (en) * | 2017-07-25 | 2017-11-24 | 陕西科技大学 | A kind of electrode material that lithium ion battery is prepared using sludge and its preparation method and application |
| CN108832090A (en) * | 2018-06-11 | 2018-11-16 | 陕西科技大学 | Lithium ion battery SiO2/ AG composite negative pole material and preparation method thereof |
| CN109524626A (en) * | 2017-09-18 | 2019-03-26 | 浙江工业大学 | A kind of Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method thereof |
| CN113745471A (en) * | 2020-05-29 | 2021-12-03 | 刘全璞 | Electrode composite material, manufacturing method of electrode composite material and rechargeable battery electrode |
| CN113851614A (en) * | 2020-06-28 | 2021-12-28 | 上海昱瓴新能源科技有限公司 | Low-temperature quick-charging artificial graphite cathode material, preparation method thereof and low-temperature quick-charging battery |
| CN115036511A (en) * | 2022-08-11 | 2022-09-09 | 溧阳天目先导电池材料科技有限公司 | Low-expansion silicon-based negative electrode material and preparation method and application thereof |
-
2016
- 2016-07-19 CN CN201610566813.6A patent/CN106058190A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107046125A (en) * | 2017-02-22 | 2017-08-15 | 深圳市金润能源材料有限公司 | Silicon-carbon composite cathode and preparation method thereof and lithium ion battery |
| CN107046125B (en) * | 2017-02-22 | 2020-08-04 | 深圳市金润能源材料有限公司 | Composite negative electrode, preparation method thereof and lithium ion battery |
| CN107394162A (en) * | 2017-07-25 | 2017-11-24 | 陕西科技大学 | A kind of electrode material that lithium ion battery is prepared using sludge and its preparation method and application |
| CN109524626A (en) * | 2017-09-18 | 2019-03-26 | 浙江工业大学 | A kind of Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method thereof |
| CN108832090A (en) * | 2018-06-11 | 2018-11-16 | 陕西科技大学 | Lithium ion battery SiO2/ AG composite negative pole material and preparation method thereof |
| CN113745471A (en) * | 2020-05-29 | 2021-12-03 | 刘全璞 | Electrode composite material, manufacturing method of electrode composite material and rechargeable battery electrode |
| CN113745471B (en) * | 2020-05-29 | 2023-03-21 | 刘全璞 | Electrode composite material, manufacturing method of electrode composite material and rechargeable battery electrode |
| CN113851614A (en) * | 2020-06-28 | 2021-12-28 | 上海昱瓴新能源科技有限公司 | Low-temperature quick-charging artificial graphite cathode material, preparation method thereof and low-temperature quick-charging battery |
| CN115036511A (en) * | 2022-08-11 | 2022-09-09 | 溧阳天目先导电池材料科技有限公司 | Low-expansion silicon-based negative electrode material and preparation method and application thereof |
| CN115036511B (en) * | 2022-08-11 | 2022-11-22 | 溧阳天目先导电池材料科技有限公司 | Low-expansion silicon-based negative electrode material and preparation method and application thereof |
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