CN106450188A - Preparation method of positive electrode material of lithium-ion battery - Google Patents

Preparation method of positive electrode material of lithium-ion battery Download PDF

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Publication number
CN106450188A
CN106450188A CN201610884779.7A CN201610884779A CN106450188A CN 106450188 A CN106450188 A CN 106450188A CN 201610884779 A CN201610884779 A CN 201610884779A CN 106450188 A CN106450188 A CN 106450188A
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preparation
ion battery
anode material
lithium ion
leaf
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晏荦
周豪杰
仰韻霖
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Guangdong Kaijin New Energy Technology Co Ltd
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Guangdong Kaijin New Energy Technology Co Ltd
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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
    • 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
    • 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
    • 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
    • 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 invention belongs to the technical field of lithium-ion batteries, and particularly relates to a preparation method of a positive electrode material of the lithium-ion battery. The positive electrode material of the lithium-ion battery comprises a core layer and a shell layer coating the outside of the core layer, wherein the core layer is SiOx, x is 0.5-2.0 and the shell layer is carbon. The preparation method of the positive electrode material at least comprises the following steps of putting leaves of gramineous plants into a high-temperature furnace; heating the leaves to 300-1200 DEG C at a speed of 10 DEG C/min to 50 DEG C/min in an inert gas atmosphere; and burning the leaves for 10s to 30min, naturally cooling the leaves, cleaning the leaves by using an acid solution, cleaning the leaves by using a solvent and then airing the leaves to obtain the positive electrode material. Compared with the prior art, the positive electrode material prepared by the method provided by the invention has relatively high initial coulomb efficiency, relatively good cycle performance and relatively low volume expansion.

Description

The preparation method of lithium ion battery anode material
Technical field
The invention belongs to technical field of lithium ion, more particularly, to a kind of preparation side of lithium ion battery anode material Method.
Background technology
All the time, because the sub- silicon (SiO) of oxidation has good bulk effect, people attempt as lithium ion battery Composite it is considered that, SiO negative pole Mechanism of electrochemical behaviors of anhydrous is as follows：
SiO+Li→Li2O+Si(1)
SiO+Li→Li4SiO4+Si(2)
Si+Li→Li4.4Si(3)
When SiO is as composite, its initial coulomb efficiency is low, is primarily due to first step reaction (formula 1) and (formula 2) and is Irreversible reaction, the Li of generation2O、Li4SiO4And the oxide of silicon is contacted the reaction such as decomposition and condensation and disappears with organic electrolyte Consume more lithium ion.
The Li generating2O、Li4SiO4Separated out with back bone network, act as a kind of good original position buffer matrix, effectively press down Make the bulk effect of active metal silicon grain in charge and discharge process；The two also plays support and dispersed metal silicon is assembled simultaneously The effect of area's particle, it is to avoid agglomeration during later stage charge and discharge cycles for the small and dispersed metallic silicon accumulation regions particle, Favourable to cyclical stability.This also exactly aoxidizes sub- silicon (SiO) material and is had an optimistic view of by people always, and realistic meaning becomes the soonest The topmost reason of composite of future generation.
Additionally, SiO material electric conductivity extreme difference, the electrical conductivity order of magnitude in the range of insulator (<10-12S/cm).
In view of this, it is necessory to provide a kind of preparation method of lithium ion battery anode material, using the method preparation Anode material there is higher coulombic efficiency first, preferable cycle performance and relatively low volumetric expansion.
Content of the invention
It is an object of the invention to：For the deficiencies in the prior art, and provide a kind of system of lithium ion battery anode material Preparation Method, the anode material using the method preparation has a higher coulombic efficiency first, preferable cycle performance and relatively low Volumetric expansion.
In order to achieve the above object, the present invention adopts the following technical scheme that：
The preparation method of lithium ion battery anode material, described lithium ion battery anode material includes stratum nucleare and is coated on institute State the shell outside stratum nucleare, described stratum nucleare is SiOx, wherein, x is 0.5-2.0, and described shell is carbon, the preparation of described anode material Method at least comprises the following steps：
The leaf of grass is placed in high temperature furnace, under inert gas atmosphere with 10 DEG C/min-50 DEG C/min's Speed is warming up to 300 DEG C -1200 DEG C, calcines 10s-30min, after Temperature fall cooling, is cleaned with acid solution, with except deoxidation Thing, metal and alloy etc., then with solvent clean, then dry, obtain final product anode material.Temperature is preferably 600 DEG C -1000 DEG C, This is because, carburizing temperature is low, and carbon graphite degree is little, and conductance is relatively low, and carburizing temperature height is then conducive to generating high conductivity Carbon.
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, described grass is bamboo At least one in son, reed, corn, cattail and reed, paddy rice, oat, Chinese sorghum and wheat.
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, leaf is being placed in high temperature furnace In the past, first with water, leaf was carried out and was dried, to remove the dust on leaf and soil.
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, leaf is carried out and is dried Afterwards, leaf is pulverized so that the size of leaf is (50 μm of -3mm) × (50 μm of -3mm).
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, described inert gas is helium, Argon gas or nitrogen.
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, described acid solution is that hydrochloric acid is molten At least one in liquid, salpeter solution, sulfuric acid solution and acetum, the concentration of described acid solution is 0.05mol/L-1mol/ L, temperature when being cleaned with acid solution is 20 DEG C -50 DEG C；Described solvent is absolute ethyl alcohol, deionized water, acetone, in methyl alcohol extremely Few one kind.
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, the temperature of Temperature fall cooling is 25 DEG C -250 DEG C, then it is placed in the air 30s-10min so that this material somewhat aoxidizes in atmosphere, thus can Simply to adjust the ratio of Si-C, method is simple, is then cleaned with acid solution again.
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, the BET ratio of described anode material Surface area is 0.6m2/g-200m2/g.Specific surface area is too little, is that the space that Li-Si alloy process volumetric expansion is reserved is inadequate, Easily cause the efflorescence of active particle in cyclic process, constantly have exposed active material to occur, electrolyte is difficult on its surface Form stable SEI film, thus leading to the deterioration of cycle performance.Although specific surface area can be good at greatly alleviating SiOxIn deintercalation Bulk effect during lithium and internal stress, thus improve cycle performance.But, it also increases silicon grain surface and electrolysis The contact area of liquid, leads to the decomposition of electrolyte to aggravate, leads to the less efficient first of composite.
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, described shell sections embed described In stratum nucleare, and the thickness of described shell is 20nm-5 μm, and carbon-coating is too thin, and the absolute volume effect of this composite is larger, lives Property material structure easily destroyed, suitably increase carbon content, the absolute volume effect of this composite can be reduced, be conducive to increase Plus the long-term cycle stability of composite.Carbon-coating too thick and can hinder embedded abjection in Si for the lithium ion and reduce it can Inverse capacity, this is because carbon specific capacity itself is low, is directly reduced the reversible capacity of composite, the too thick pliability of carbon-coating simultaneously Can reduce, easily cause carbon-coating on the contrary and rupture and lead to SiOxThe efflorescence in cyclic process of/carbon composite.
As a kind of improvement of the preparation method of lithium ion battery anode material of the present invention, the particle diameter of described stratum nucleare is 0.5 μ m-5μm.
With respect to prior art, the present invention at least has the advantages that：
First, the present invention utilizes the leaf of grass, not only energy-conserving and environment-protective, and can turn waste into wealth, by nature The leaf of the grass that boundary is widely present is become by simple conversion greatly the anode of purposes in new energy field Material, cost is extremely low；This is because, contain carbohydrate, protein, Si and a small amount of metal oxygen in the leaf of grass Compound etc., during burning, can be converted into the SiO of carbon coatingx, a small amount of metal oxide then can be washed by acid solution Go.
Second, in SiOxUpper carbon coated, can improve the electron conduction of this material, this is because, after carbon coated, electronics Active material particle top layer can be passed freely through, whole electrode forms good conductive network, thus reducing intergranular Interface impedance；
3rd, in SiOxUpper carbon coated, can improve chemistry and the electrochemical stability of material, this is because in electrolyte LiPF6Meet water very sensitive, even if touching the water of trace, LiPF6Also easily hydrolyze, produce HF, thus corroding silicon face, And carbon has excellent chemical stability, will not be corroded by HF, after carbon coating, this carbon-coating inhibits HF to silicon grain to silicon grain The corrosion on surface, in addition, carbon electrochemical window width in organic electrolyte, so it has only in the case of current potential is low-down There is electro-chemical activity, and under high voltages also will not be oxidized.
4th, carbon coating not only increases the electric conductivity of active material, also serves as elastic layer alleviation active material simultaneously and exists Volumetric expansion in process of intercalation, stabilizes the structure of material.
5th, carbon coating can also significantly improve SiOxThe coulombic efficiency first of material and capacity play.
Brief description
Fig. 1 is the structural representation of lithium ion battery anode material in the present invention.
Specific embodiment
The invention provides a kind of preparation method of lithium ion battery anode material.
Embodiment 1
The preparation method of the lithium ion battery anode material that the present embodiment provides, as shown in figure 1, this anode of lithium ion battery Material includes stratum nucleare 1 and the shell 2 being coated on outside stratum nucleare 1, and stratum nucleare 1 is SiOx, wherein, x is 0.5-2.0, and shell 2 is carbon, should The preparation method of anode material at least comprises the following steps：
First with water, the leaf of bamboo is carried out and is dried, to remove the dust on leaf and soil, then to leaf Pulverized so that the size of leaf is 1mm × 1mm, the leaf of bamboo is placed in high temperature furnace, with 25 under helium atmosphere DEG C/speed of min is warming up to 800 DEG C, calcine 10min, after Temperature fall is cooled to 100 DEG C, be placed in the air 1min, use The concentration soaking and washing at 30 DEG C of the hydrochloric acid solution for 0.1mol/L, then deionized water cleaning, then dry, obtain final product anode material Material.
The BET specific surface area of this anode material is 1.2m2/g.Shell 2 is partially submerged in stratum nucleare 1, and the thickness of shell 2 For 20nm-5 μm.The particle diameter of stratum nucleare 1 is 0.5 μm -5 μm.
Embodiment 2
The preparation method of the lithium ion battery anode material that the present embodiment provides, as shown in figure 1, this anode of lithium ion battery Material includes stratum nucleare 1 and the shell 2 being coated on outside stratum nucleare 1, and stratum nucleare 1 is SiOx, wherein, x is 0.5-2.0, and shell 2 is carbon, should The preparation method of anode material at least comprises the following steps：
First with water, the leaf of reed is carried out and is dried, to remove the dust on leaf and soil, then to leaf Pulverized so that leaf size be 0.5mm × 0.5mm, the leaf of reed is placed in high temperature furnace, under an argon atmosphere with The speed of 15 DEG C/min is warming up to 1000 DEG C, calcines 15min, after Temperature fall is cooled to 150 DEG C, is placed in the air 5min, the sulfuric acid solution being 0.5mol/L with concentration cleans at 35 DEG C, then with washes of absolute alcohol, then dries, and obtains final product sun Pole material.
The BET specific surface area of anode material is 10m2/ g, shell 2 is partially submerged in stratum nucleare 1, and the thickness of shell 2 is 20nm-5 μm, the particle diameter of stratum nucleare 1 is 0.5 μm -5 μm.
Embodiment 3
The preparation method of the lithium ion battery anode material that the present embodiment provides, as shown in figure 1, this anode of lithium ion battery Material includes stratum nucleare 1 and the shell 2 being coated on outside stratum nucleare 1, and stratum nucleare 1 is SiOx, wherein, x is 0.5-2.0, and shell 2 is carbon, should The preparation method of anode material at least comprises the following steps：
First with water, the leaf of corn is carried out and is dried, to remove the dust on leaf and soil, then to leaf Pulverized so that leaf size be 100 μm of 100 μ m, the leaf of corn is placed in high temperature furnace, in a nitrogen atmosphere with The speed of 20 DEG C/min is warming up to 900 DEG C, calcines 15min, after Temperature fall is cooled to 200 DEG C, is placed in the air 8min, The salpeter solution being 0.3mol/L with concentration cleans at 40 DEG C, and again with methanol is cleaned, and then dries, obtains final product anode material.
The BET specific surface area of anode material is 20m2/g.Shell 2 is partially submerged in stratum nucleare 1, and the thickness of shell 2 is 20nm-5μm；The particle diameter of stratum nucleare 1 is 0.5 μm -5 μm.
Embodiment 4
The preparation method of the lithium ion battery anode material that the present embodiment provides, as shown in figure 1, this anode of lithium ion battery Material includes stratum nucleare 1 and the shell 2 being coated on outside stratum nucleare 1, and stratum nucleare 1 is SiOx, wherein, x is 0.5-2.0, and shell 2 is carbon, should The preparation method of anode material at least comprises the following steps：
First with water, the leaf of paddy rice is carried out and is dried, to remove the dust on leaf and soil, then to leaf Pulverized so that leaf size be 2.5mm × 2.5mm, the leaf of paddy rice is placed in high temperature furnace, under helium atmosphere with The speed of 35 DEG C/min is warming up to 950 DEG C, calcines 25min, after Temperature fall is cooled to 150 DEG C, is placed in the air 2min, The acetum being 0.7mol/L with concentration cleans at 40 DEG C, then is cleaned with acetone, then dries, obtains final product anode material.
The BET specific surface area of anode material is 15m2/g.Shell 2 is partially submerged in stratum nucleare 1, and the thickness of shell 2 is 20nm-5μm.The particle diameter of stratum nucleare 1 is 0.5 μm -5 μm.
Embodiment 5
The preparation method of the lithium ion battery anode material that the present embodiment provides, as shown in figure 1, this anode of lithium ion battery Material includes stratum nucleare 1 and the shell 2 being coated on outside stratum nucleare 1, and stratum nucleare 1 is SiOx, wherein, x is 0.5-2.0, and shell 2 is carbon, should The preparation method of anode material at least comprises the following steps：
First with water, the leaf of oat is carried out and is dried, to remove the dust on leaf and soil, then to leaf Pulverized so that leaf size be 500 μm of 500 μ m, the leaf of oat is placed in high temperature furnace, under an argon atmosphere with The speed of 12 DEG C/min is warming up to 700 DEG C, calcines 18min, after Temperature fall is cooled to 50 DEG C, is placed in the air 4min, The salpeter solution being 0.6mol/L with concentration cleans at 25 DEG C, then with washes of absolute alcohol, then dries, and obtains final product anode material Material.
The BET specific surface area of anode material is 8m2/g.Shell 2 is partially submerged in stratum nucleare 1, and the thickness of shell 2 is 20nm-5μm.The particle diameter of stratum nucleare 1 is 0.5 μm -5 μm.
Embodiment 6
The preparation method of the lithium ion battery anode material that the present embodiment provides, as shown in figure 1, this anode of lithium ion battery Material includes stratum nucleare 1 and the shell 2 being coated on outside stratum nucleare 1, and stratum nucleare 1 is SiOx, wherein, x is 0.5-2.0, and shell 2 is carbon, should The preparation method of anode material at least comprises the following steps：
First with water, the leaf of Chinese sorghum is carried out and is dried, to remove the dust on leaf and soil, then to leaf Pulverized so that the size of leaf is 700 μm of 700 μ m, the leaf of Chinese sorghum is placed in high temperature furnace, under a nitrogen with 20 DEG C/speed of min is warming up to 750 DEG C, calcine 7min, after Temperature fall is cooled to 70 DEG C, be placed in the air 6min, with dense Spend the sulfuric acid solution for 0.9mol/L to clean at 45 DEG C, then cleaned with acetone, then dry, obtain final product anode material.
The BET specific surface area of anode material is 18m2/g.Shell 2 is partially submerged in stratum nucleare 1, and the thickness of shell 2 is 20nm-5μm.The particle diameter of stratum nucleare 1 is 0.5 μm -5 μm.
Embodiment 7
The preparation method of the lithium ion battery anode material that the present embodiment provides, as shown in figure 1, this anode of lithium ion battery Material includes stratum nucleare 1 and the shell 2 being coated on outside stratum nucleare 1, and stratum nucleare 1 is SiOx, wherein, x is 0.5-2.0, and shell 2 is carbon, should The preparation method of anode material at least comprises the following steps：
First with water, the leaf of high wheat is carried out and is dried, to remove the dust on leaf and soil, then to leaf Son is pulverized so that the size of leaf is 900 μm of 900 μ m, the leaf of wheat is placed in high temperature furnace, under a nitrogen with 22 DEG C/speed of min is warming up to 750 DEG C, calcine 15min, after Temperature fall is cooled to room temperature, be placed in the air 30s, with dense Spend the hydrochloric acid solution for 0.3mol/L to clean at 40 DEG C, again with methanol is cleaned, and then dries, obtains final product anode material.
The BET specific surface area of anode material is 50m2/g.
Shell 2 is partially submerged in stratum nucleare 1, and the thickness of shell 2 is 20nm-5 μm.
The particle diameter of stratum nucleare 1 is 0.5 μm -5 μm.
Comparative example 1
The material that this comparative example provides is commercially available SiO2Particle, its BET specific surface area is 18m2/g.
Comparative example 2
The material that this comparative example provides is commercially available SiO particle, and its BET specific surface area is 15m2/g.
By the anode material of embodiment 1-7 and comparative example 1,2 respectively with butadiene-styrene rubber, sodium carboxymethylcellulose and superconduction carbon Add in distilled water, be uniformly mixing to obtain anode slurry；Then anode slurry is coated in anode collector, obtains anode Piece, number consecutively is S1-S7 and D1, D2.
By numbering be S1-S7 and D1, D2 anode strip be assembled into lithium-ion electric with cathode sheets, barrier film and electrolyte respectively Pond, and number consecutively is B1-B7 and C1, C2.
To numbering be B1-B7 and C1, C2 lithium ion battery tested as follows：
(1), coulombic efficiency test first：First discharged with the electric current of 0.2mA, be discharged to 0.005V, allowed anode material Embedding lithium, after standing 10min, then charges to 2.000V, the discharging efficiency first of test graphite, acquired results with the electric current of 0.2mA It is shown in Table 1.
(2), cell expansion test：Before chemical conversion, first test No. is the initial thickness of the lithium ion battery of B1-B7 and C1, C2 Degree, is designated as d0, the lithium ion battery discharge and recharge at 25 ± 2 DEG C being then B1-B7 and C1, C2 by numbering, rate of charge is 0.5C, charge cutoff voltage is 4.20V, and cut-off current is 0.05C；Discharge current is 0.5C, and discharge cut-off voltage is 3.0V；Note Cell thickness d after 200 circulations of record200, then calculate the thickness swelling after circulating battery 200 times again.Thickness swelling Computing formula is (d200-d0)/d0, acquired results are shown in Table 1.
(3), cycle performance of battery test：By numbering be B1-B7 and C1, C2 battery at 25 DEG C filling with 0.5C/1C Discharge-rate carries out charge and discharge cycles test, and record circulates the capability retention after 200 times, and acquired results are shown in Table 1.
Table 1：Numbering is B1-B7 and C1, the performance test results of the battery of C2.
From table 1 it follows that higher coulombic efficiency first is had using the anode material of method of the present invention preparation, Preferably cycle performance and relatively low volumetric expansion.
The announcement of book and elaboration according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party Formula is changed and is changed.Therefore, the invention is not limited in specific embodiment disclosed and described above, to the present invention's Some equivalent modifications and change should also be as in the scope of the claims of the present invention.Although additionally, making in this specification With some specific terms, but these terms are merely for convenience of description, do not constitute any restriction to the present invention.

Claims (10)

1. lithium ion battery anode material preparation method it is characterised in that：Described lithium ion battery anode material includes stratum nucleare With the shell being coated on outside described stratum nucleare, described stratum nucleare is SiOx, wherein, x is 0.5-2.0, and described shell is carbon, described anode The preparation method of material at least comprises the following steps：
The leaf of grass is placed in high temperature furnace, under inert gas atmosphere with the speed of 10 DEG C/min-50 DEG C/min It is warming up to 300 DEG C -1200 DEG C, calcine 10s-30min, after Temperature fall cooling, cleaned with acid solution, then with solvent clean, so After dry, obtain final product anode material.
2. lithium ion battery anode material according to claim 1 preparation method it is characterised in that：Described grass family is planted Thing is at least one in bamboo, reed, corn, cattail and reed, paddy rice, oat, Chinese sorghum and wheat.
3. lithium ion battery anode material according to claim 1 preparation method it is characterised in that：Leaf is being placed in Before in high temperature furnace, first with water, leaf is carried out and is dried, to remove the dust on leaf and soil.
4. lithium ion battery anode material according to claim 3 preparation method it is characterised in that：Leaf is carried out clearly After washing and being dried, leaf is pulverized so that the size of leaf is (50 μm of -3mm) × (50 μm of -3mm).
5. lithium ion battery anode material according to claim 1 preparation method it is characterised in that：Described inert gas For helium, argon gas or nitrogen.
6. lithium ion battery anode material according to claim 1 preparation method it is characterised in that：Described acid solution is At least one in hydrochloric acid solution, salpeter solution, sulfuric acid solution and acetum, the concentration of described acid solution is 0.05mol/L- 1mol/L, temperature when being cleaned with acid solution is 20 DEG C -50 DEG C；Described solvent is absolute ethyl alcohol, deionized water, acetone, methyl alcohol In at least one.
7. lithium ion battery anode material according to claim 1 preparation method it is characterised in that：Temperature fall cools down Temperature be 25 DEG C -250 DEG C, be then placed in the air 30s-10min, then cleaned with acid solution again.
8. lithium ion battery anode material according to claim 1 preparation method it is characterised in that：Described anode material BET specific surface area be 0.6m2/g-200m2/g.
9. lithium ion battery anode material according to claim 1 preparation method it is characterised in that：Described shell sections Embed in described stratum nucleare, and the thickness of described shell is 20nm-5 μm.
10. lithium ion battery anode material according to claim 1 preparation method it is characterised in that：Described stratum nucleare Particle diameter is 0.5 μm -5 μm.
CN201610884779.7A 2016-10-10 2016-10-10 Preparation method of positive electrode material of lithium-ion battery Pending CN106450188A (en)

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