CN106654194B - A kind of SiO of element dopingxAnode material and its preparation method and application - Google Patents
A kind of SiO of element dopingxAnode material and its preparation method and application Download PDFInfo
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- CN106654194B CN106654194B CN201610976331.8A CN201610976331A CN106654194B CN 106654194 B CN106654194 B CN 106654194B CN 201610976331 A CN201610976331 A CN 201610976331A CN 106654194 B CN106654194 B CN 106654194B
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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
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- H—ELECTRICITY
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- H—ELECTRICITY
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- 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
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Abstract
A kind of SiO of element doping is providedxAnode material and its preparation method and application.The SiO of the element dopingxSiO in anode materialxContent is 30 80%, and carbon content is 20 70%, and doped chemical content is below 5%, which is 3 25 μm, and 1.5≤(D90 D10)/D50≤2, BET specific surface area is (8 ± 5) m2·g‑1.Doped chemical is the one or more in following element：Boron, nitrogen phosphate and sulfur, lithium, sodium, potassium, magnesium, aluminium, zinc, copper, tin, doped chemical is preferably combined using nonmetalloid and metallic element, such as boron lithium, boron zinc, boron copper, nitrogen aluminium, boron aluminium lithium, the combination of the combination, most preferably boron aluminium lithium of boron copper lithium.
Description
Technical field
The present invention relates to a kind of SiO of element dopingxThe SiO of negative material, more particularly to element dopingxNegative material is made
For the application of height ratio capacity lithium ion battery negative material.
Background technology：
Lithium ion battery have it is higher than energy, self discharge is small, service life is long, green non-pollution outstanding advantages of it is wide
General is applied in portable electronic products and electric automobile.With the development and progress of society, lithium ion battery further should
With there is an urgent need for improving energy density, the electrode material for developing height ratio capacity is one of effective way.
In negative material, mainly carbon material commercialized at present, its theoretical specific capacity is relatively low, about 372mAhg-1.And silicon is because having high theoretical specific capacity (about 3579mAhg-1) and receive more and more attention, it is considered as most to have
One of material of graphite cathode may be substituted.It is huge but silicon can produce about 300% volume change during Li insertion extraction
Volume change the dusting of silicon electrode can be caused to peel off, make to lose electrical contact between silicon grain and between silicon and collector.Oxygen
Silicon nitride material, although its theoretical specific capacity is smaller than pure silicon material, its bulk effect in battery charge and discharge process is relatively
Small (about 200%), therefore, silica material are easier to break through limitation, realize commercialization early.Industrial most common SiOx
(0<x<2) material is exactly to aoxidize sub- silicon, SiOxIt is a kind of binary phase materials, SiOxBy particle diameter it is minimum (<Amorphous Si 1nm) and
SiO2 is formed.SiOxStructure can be adjusted by the simple means such as heat treatment, ball milling and etching.By in protective atmosphere
Under to SiOxSiO can be promoted by carrying out heat treatmentxGeneration disproportionated reaction, forms Si and SiO2Two-phase.In general, SiOx800
Original impalpable structure is kept below DEG C；When temperature rises to 900~1000 DEG C, SiOxDisproportionated reaction takes place；With
Temperature to continue to rise, SiOxDisproportionation it is obvious all the more, the crystal grain of Si simple substance is also gradually grown up.The generation of disproportionated reaction also promotees
Make SiOxChemical property change:With the intensification of disproportionation degree, SiOxThe specific capacity of electrode is gradually reduced；Work as disproportionation
Reache a certain level, SiOxSubstantially electro-chemical activity is lost.Therefore the control for sintering temperature is also a problem.
Element doping can effectively reduce the internal resistance of material, improve the electric conductivity of material, improve the multiplying power of electrode material
Performance and cycle performance.Such as：Nitrogen, phosphorus, boron doped carbon material have excellent electric conductivity；Using metal-doped, formation conjunction
Aurification material can improve cycle performance, meanwhile, unnecessary metal can improve material electric conductivity；Adulterated using oxide material
The stability of solid electrolyte film can effectively be increased, so as to achieve the purpose that stable circulation.Therefore, using element doping
SiOxAs negative material, some defects are created by doping, the electronics and ion transport ability of material is improved, is at the same time
Certain position is reserved in volumetric expansion, it is possible to achieve high specific capacity takes into account excellent cycle performance.
The content of the invention
Present invention aims at pass through rational structure design and testing program, there is provided one kind uses the sub- silicon of oxidation as original
Material prepares the SiO of element dopingxThe method of negative material, and its performance is studied.
Present invention firstly provides a kind of SiO of element dopingxNegative material, the wherein SiO of the composite materialxContent is 30-
80%, carbon content 20-70%, doped chemical content below 5%, wherein, the scope of x is 0<x<2, preferably 0.5<x<1.5
The average diameter of the composite material is 3-25 μm, and 1.5≤(D90-D10)/D50≤2, BET specific surface area is (8 ± 5) m2·g-1,
It is characterized in that, doped chemical is the one or more in following element：Boron, nitrogen phosphate and sulfur, lithium, sodium, potassium, magnesium, aluminium, zinc, copper,
Tin, doped chemical is preferably combined using nonmetalloid and metallic element, such as boron lithium, boron zinc, boron copper, nitrogen aluminium, boron aluminium lithium, boron copper
The combination of the combination of lithium, most preferably boron aluminium lithium or boron copper lithium.
The present invention obtains optimal element doping and is combined as metal and nonmetallic mixed by being made choice to doped chemical
Close.By nonmetallic structure negative material defect, the intrinsic ion transport capability of material is improved, meanwhile, metal is mixed with SiOx
Conductive network improves material conductivity.
Further, the SiO of the element dopingxNegative material average diameter is 7-15 μm, 1.5≤(D90-D10)/
D50≤2, BET specific surface area are (5 ± 2) m2·g-1。
Further, the composite material surface has pothole, a diameter of 0.5-3 μm of pothole.
Further object of the present invention is to provide the SiO of the element dopingxThe application of negative material.
Application provided by the present invention is the SiO of element dopingxApplication of the negative material as battery electrode material, especially
It is the application as lithium ion battery negative material.
The present invention further provides the SiO of element dopingxThe preparation method of negative material, including it is as follows：
Step 1), carries out ball mill grinding by the sub- silica flour of oxidation after solvent disperses, adds the compound containing doped chemical,
Co-grinding, obtains uniformly mixed slurry；
Step 2), is dried processing by the slurry obtained by step 1) and obtains powders A；
Step 3), gained powders A obtain solid powder B in inert non-oxidizing property atmosphere high temperature calcination processing；
Step 4), solid powder B is mixed with carbon source, and ball milling mixing is carried out under conditions of solvent disperses and is crushed to conjunction
Suitable particle diameter；
Step 5), solid powder C is obtained by slurry drying process obtained by step 4)；
Step 6), obtains element in inert non-oxidizing property atmosphere high temperature carbonization treatment by the powder C that step 5) obtains and mixes
Miscellaneous SiOxNegative material；
Wherein, it is 8nm-10mm, preferably 500nm-5mm that sub- silicon is aoxidized described in step 1)；Material particle size after grinding is
10nm-3 μm, preferably 100nm-300nm；One or more below solvent selected as：Water, ethanol, ethyl acetate, ethylene glycol,
N-hexane, polymethyl siloxane；Doped chemical is the one or more in following element：Boron, nitrogen phosphate and sulfur, lithium, sodium, potassium, magnesium,
Aluminium, zinc, copper, tin, doped chemical is preferably combined using nonmetalloid and metallic element, such as boron lithium, boron zinc, boron copper, nitrogen aluminium, boron
Aluminium lithium, the combination of the combination, most preferably boron aluminium lithium of boron copper lithium.It is sub- siliceous that compound addition containing doped chemical is not more than oxidation
The 5% of amount.
Wherein, step 2) and the step 5) drying mode are one kind in following scheme：Vacuum drying, filter, spraying
It is dry.
Wherein, step 3) is provided with non-oxidizing atmosphere described in step 6) by following at least one gases：Nitrogen, argon
Gas, helium；The sintering temperature is 400-1600 DEG C, is preferably 450-1200 DEG C, and programming rate is 1-15 DEG C/min, is preferably
1-5 DEG C/min, sintering time 1-15h, be preferably 2-6h.
Wherein, the step 4) carbon source is selected from following at least one：Delanium, native graphite, mesocarbon microspheres, stone
Black alkene, carbon nanotubes, phenolic resin, pitch, polyvinylidene fluoride (PVDF), polyvinylpyrrolidone (PVP), polyvinyl alcohol
(PVA), polyethylene glycol oxide (PEO), polyvinyl chloride (PVC), polyacrylonitrile (PAN), polyacetylene, polyaniline, polythiophene, grape
Sugar, sucrose, citric acid, sodium alginate, carboxymethyl cellulose, hydroxypropyl cellulose, gelatin, starch, chitosan, alginic acid.Step
It is rapid 4) in powder C and the mass ratio of carbon source be (1-8)：(2-9), is preferably (3-7)： (3-7)；Suitable particle diameter is after ball milling
10nm-3 μm, be preferably 50nm-1 μm.
Further object of the present invention is to provide the SiO for the element doping that preceding method is preparedxNegative material.In addition,
The SiO for the element doping that preceding method is prepared also is providedxThe application of negative material, the application are the SiO of element dopingx
Application of the negative material as battery electrode material, especially as the application of lithium ion battery negative material.
In addition, the present invention also provides a kind of energy storage elements, the energy storage elements contain preceding method and are prepared into
The SiO of the element doping arrivedxNegative material, the preferred lithium ion battery of the energy storage elements.
The present invention also provides a kind of portable electric appts, which uses the member being prepared containing preceding method
The SiO of element dopingxThe above-mentioned energy storage elements of negative material, the preferred mobile phone of the portable electric appts, camera, take the photograph
Camera, MP3, MP4, laptop.
Compared with prior art, the present invention effectively raises leading for the sub- silicon materials of oxidation using the method for element doping
Electrically, the performance of material capacity and the optimization of high rate performance are conducive to, simply easily prepared by amplification for technique, material prepared SiOx
Well dispersed, surface formation SEI films are uniform and stable, and cycle performance is excellent with high rate performance.The present invention by doped chemical into
Row selection, obtains optimal element doping and is combined as metal and nonmetallic mixing.By nonmetallic structure negative material defect, carry
The intrinsic ion transport capability of high material, meanwhile, metal improves material conductivity with SiOx hybrid conductives network, while is volume
The reserved certain position of expansion, it is possible to achieve high specific capacity takes into account excellent cycle performance.
Brief description of the drawings
Fig. 1 is the SiO of 8 gained element doping of embodimentxThe electron scanning micrograph of negative material.
Fig. 2 is the SiO of 8 gained element doping of embodimentxThe X ray diffracting spectrum (XRD) of negative material.
Fig. 3 is the SiO for the element doping that embodiment 8 obtainsxTest number of the negative material under 100mA/g current densities
According to.
Embodiment
The present invention is further described with reference to specific embodiment, the present invention is not limited to following case study on implementation.
Test method described in following embodiments, is conventional method unless otherwise specified；The reagent and material, such as
Without specified otherwise, can obtain from commercial channels.
Embodiment 1
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add phosphorus
Acid, weight are the 5% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；The slurry of gained is carried out
Drying process obtains powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sintering
6h, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, is divided equally again
Son amount is 300000 mixing, and ball milling mixing is carried out under conditions of solvent disperses and is crushed to suitable particle diameter；By gained slurry
Drying process obtains solid powder C.Powder C is obtaining P elements doping in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material：
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 14.1 μm, (D90-D10)/
D50 is 1.72, BET specific surface area 5.60m2·g-1。
The SiO of element dopingxThe Electrochemical Characterization of negative material：
By the SiO of the element doping prepared in embodiment 1xNegative material, acetylene black and sodium carboxymethylcellulose (bond
Agent) with mass ratio 80：10：10 mixing are made into slurry, are homogeneously applied to obtain electrode diaphragm in copper foil current collector.With lithium metal
Piece is used as to electrode, and microporous polypropylene membrane (Celgard 2400) is used as membrane, and (solvent is that volume ratio is 1 to 1mol/L LiPF6：
1 ethylene carbonate and dimethyl carbonate mixed liquor, wherein the vinylidene carbonic ester of addition 5%, 2% vinylene carbonate)
As electrolyte, button cell is assembled into the glove box of argon gas protection, carries out charge-discharge test, test program 100mA/
G, charging/discharging voltage section are 0.01~1.0V, and cell testing results are listed in table 1.
Embodiment 2
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add five oxygen
Change two phosphorus, weight is the 5% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；By the slurry of gained
Processing is dried and obtains powders A, powders A is sintered for 400 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, is burnt
6h is tied, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, and weight is equal
Molecular weight is 300000 mixing, and ball milling mixing is carried out under conditions of solvent disperses and is crushed to suitable particle diameter；Gained is starched
Material drying process obtains solid powder C.Powder C is obtaining element phosphorus doping in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 14.3 μm, (D90-D10)/
D50 is 1.81, BET specific surface area 6.7m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 3
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add oxidation
Boron, weight are the 5% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；The slurry of gained is carried out
Drying process obtains powders A, powders A is sintered for 500 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sintering
6h, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, is divided equally again
Son amount is 350000 mixing, and ball milling mixing is carried out under conditions of solvent disperses and is crushed to suitable particle diameter；By gained slurry
Drying process obtains solid powder C.Powder C is to obtain element in inertia pure nitrogen gas atmosphere high temperature carbonization treatment boron doped
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 13.4 μm, (D90-D10)/
D50 is 1.9, BET specific surface area 6.9m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 4
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add metal
Aluminium, weight are the 10% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；By the slurry of gained into
Row drying process obtains powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, is burnt
6h is tied, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, adds polyvinylpyrrolidone as polymerization
Thing additive, weight average molecular weight are 300000 mixing, and ball milling mixing is carried out under conditions of solvent disperses and is crushed to suitably
Particle diameter；Gained slurry drying process is obtained into solid powder C.Powder C is obtained in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
To the SiO of element aluminum dopingxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 12.3 μm, (D90-D10)/
D50 is 1.7, BET specific surface area 5.5m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 5
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add oxidation
Aluminium, weight are the 4% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；The slurry of gained is carried out
Drying process obtains powders A, powders A is sintered for 1400 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sintering
6h, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, is divided equally again
Son amount is 300000 mixing, and ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；By gained slurry
Drying process obtains solid powder C.Powder C is obtaining element aluminum doping in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 13.7 μm, (D90-D10)/
D50 is 1.77, BET specific surface area 5.85m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 6
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add metal
Copper, weight are the 2% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；The slurry of gained is carried out
Drying process obtains powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sintering
6h, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, is divided equally again
Son amount is 300000 mixing, and ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；By gained slurry
Drying process obtains solid powder C.Powder C is obtaining element Copper-cladding Aluminum Bar in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 14.5 μm, (D90-D10)/
D50 is 1.81, BET specific surface area 6.05m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 7
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add oxidation
Copper, weight are the 3% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；The slurry of gained is carried out
Drying process obtains powders A, powders A is sintered for 1400 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sintering
6h, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, is divided equally again
Son amount is 300000 mixing, and ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；By gained slurry
Drying process obtains solid powder C.Powder C is obtaining element Copper-cladding Aluminum Bar in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 12.5 μm, (D90-D10)/
D50 is 1.90, BET specific surface area 7.0m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 8
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add oxidation
Titanium, weight are the 5% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；The slurry of gained is carried out
Drying process obtains powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sintering
6h, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, is divided equally again
Son amount is 300000 mixing, and ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；By gained slurry
Drying process obtains solid powder C.Powder C is to obtain element in inertia pure nitrogen gas atmosphere high temperature carbonization treatment titanium doped
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 12.8 μm, (D90-D10)/
D50 is 1.67, BET specific surface area 5.35m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 9
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add hydrogen-oxygen
Change lithium, weight is the 4% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；By the slurry of gained into
Row drying process obtains powders A, powders A is sintered for 1000 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, is burnt
6h is tied, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, and weight is equal
Molecular weight is 300000 mixing, and ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；Gained is starched
Material drying process obtains solid powder C.Powder C is obtaining element lithium doping in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 13.9 μm, (D90-D10)/
D50 is 1.75, BET specific surface area 5.75m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 10
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add carbonic acid
Lithium, weight are the 5% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；The slurry of gained is carried out
Drying process obtains powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sintering
6h, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, is divided equally again
Son amount is 300000 mixing, and ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；By gained slurry
Drying process obtains solid powder C.Powder C is obtaining element lithium doping in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 13.4 μm, (D90-D10)/
D50 is 1.83, BET specific surface area 6.15m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 11
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add oxidation
Tin, weight are the 3% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；The slurry of gained is carried out
Drying process obtains powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sintering
6h, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, is divided equally again
Son amount is 300000 mixing, and ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；By gained slurry
Drying process obtains solid powder C.Powder C is obtaining element tin dope in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 14.8 μm, (D90-D10)/
D50 is 1.90, BET specific surface area 6.50m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 12
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add hydrogen-oxygen
Change lithium, weight is the 5% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；By the slurry of gained into
Row drying process obtains powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, is burnt
6h is tied, obtains solid powder B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, and weight is equal
Molecular weight is 300000 mixing, and ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；Gained is starched
Material drying process obtains solid powder C.Powder C is obtaining element lithium doping in inertia pure nitrogen gas atmosphere high temperature carbonization treatment
SiOxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that for the size distribution of Si-C composite material than more uniform, average grain diameter is 13.2 μm, (D90-D10)/
D50 is 1.69, BET specific surface area 5.45m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 13
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to add hydrogen-oxygen
Change lithium, weight is the 5% of the sub- siliceous amount of oxidation, and further co-grinding, obtains uniformly mixed slurry；By the slurry of gained into
Row drying process obtains powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, is burnt
6h is tied, obtains solid powder B.By powder B：Pitch：Native graphite=1：1：1 mass ratio mixing, under conditions of ethanol disperses
Carry out ball milling mixing and be crushed to suitable particle diameter；Gained slurry drying process is obtained into solid powder C.Powder C is in inertia
Pure nitrogen gas atmosphere high temperature carbonization treatment obtains the SiO of element lithium dopingxNegative material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that the size distribution of Si-C composite material than more uniform, particle diameter between 7-15 μm, (D90-D10)/
D50 is 1.72, BET specific surface area 5.60m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Embodiment 14-22
It is different only in that doped chemical is different from embodiment 1, corresponding doped chemical, copper, zinc using simple substance form,
Lithium uses aluminium hydroxide, and aluminium element uses aluminium oxide.Different element compound equimolar ratios add, the compound gross weight of doping
Measure as the 5% of the sub- siliceous amount of oxidation.
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 2.
Comparative example 1
Sub- Si powder will be aoxidized, is directly used as electrode material.
The characterization of the electrode material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that the size distribution of Si-C composite material is than more uniform, and average grain diameter is 5 μm, (D90-D10)/D50
For 1.9, BET specific surface area 8.45m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the composition and electricity of the electrode obtained material
The test result in pond is listed in table 1.
Comparative example 2
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to be dried to obtain
Powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sinters 6h, obtains SiOxAnode
Material.
The characterization of the material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that the size distribution of Si-C composite material is than more uniform, and average grain diameter is 3 μm, (D90-D10)/D50
For 1.9, BET specific surface area 8.55m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the composition and electricity of the electrode obtained material
The test result in pond is listed in table 1.
Comparative example 3
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to be dried to obtain
Powders A, by powders A：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, and weight average molecular weight is
300000 mixing, ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；At gained slurry drying
Reason obtains SiOxComposite material.
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that the size distribution of Si-C composite material than more uniform, particle diameter between 5-18 μm, (D90-D10)/
D50 is 1.79, BET specific surface area 9.45m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
Comparative example 4
Will the sub- silica flour of oxidation disperse in ethanol after carry out ball mill grinding, be crushed to median diameter after 3 μm, to be dried to obtain
Powders A, powders A is sintered for 1200 DEG C in inertia pure nitrogen gas atmosphere, heating rate is 5 DEG C/min, sinters 6h, obtains solid powder
B.By powder B：Delanium=1：2 mass ratio mixing, addition PVP is polymeric additive, weight average molecular weight 300000
Mixing, ball milling mixing is carried out under conditions of ethanol disperses and is crushed to suitable particle diameter；Gained slurry drying process is obtained
Solid powder C.Powder C is obtaining the SiO of element doping in inertia pure nitrogen gas atmosphere high temperature carbonization treatmentxNegative material.Member
The SiO of element dopingxThe characterization of negative material is same as Example 1.
The particle diameter of the Si-C composite material obtained under above-mentioned condition is detected with Japan Electronics scanning electron microscope (JEOL-6700F)
And size distribution, the results showed that the size distribution of Si-C composite material than more uniform, particle diameter between 5-20 μm, (D90-D10)/
D50 is 1.89, BET specific surface area 7.45m2·g-1。
Cathode, anode, electrolyte and the battery of battery assemble same as Example 1, the sub- silicon of gained oxidation and carbon electrode material
The composition of material and the test result of battery are listed in table 1.
1 negative material test result of table
2 negative material test result of table
Claims (10)
- A kind of 1. SiO of element dopingxAnode material, the wherein SiO of the composite materialxContent is 30-80%, carbon content For 20-70%, doped chemical content below 5%, wherein, the scope of x is 0.5<x<1.5, the average diameter of the composite material For 3-25 μm, 1.5≤(D90-D10)/D50≤2, BET specific surface area is (8 ± 5) m2·g-1, it is characterised in that doped chemical For the combination of boron aluminium lithium or boron copper lithium.
- 2. the anode material described in claim 1, the SiO of the element dopingxAnode material average diameter is 7- 15 μm, 1.5≤(D90-D10)/D50≤2, BET specific surface area is (5 ± 2) m2·g-1。
- 3. according to the preparation method of claim 1-2 any one of them anode materials, comprise the following steps that：Step 1) will aoxidize sub- silica flour and ball mill grinding carried out after solvent disperses, and add the compound containing doped chemical, mix Crush, obtain uniformly mixed slurry；Slurry obtained by step 1) is dried processing and obtains powders A by step 2)；Powders A obtained by step 3) obtains solid powder B in inert non-oxidizing property atmosphere high temperature calcination processing；Step 4) mixes solid powder B with carbon source, and ball milling mixing is carried out under conditions of solvent disperses and is crushed to suitable grain Footpath；Slurry drying process obtained by step 4) is obtained solid powder C by step 5)；The powder C that step 5) obtains is obtained element doping by step 6) in inert non-oxidizing property atmosphere high temperature carbonization treatment SiOxAnode material.
- 4. preparation method according to claim 3, it is characterised in that after wherein, described in step 1) aoxidizing sub- silicon grinding Material particle size be 100nm-300nm；One or more below solvent selected as：Water, ethanol, ethyl acetate, ethylene glycol, just Hexane, polymethyl siloxane；Compound addition containing doped chemical, which is not more than, aoxidizes the 5% of sub- siliceous amount.
- 5. according to claim 3-4 any one of them preparation methods, it is characterised in that wherein, step 2) and step 5) are described Drying mode is one kind in following scheme：Vacuum drying, filter, spray drying.
- 6. according to claim 3-4 any one of them preparation methods, it is characterised in that wherein, step 3) and institute in step 6) Non-oxidizing atmosphere is stated to be provided by following at least one gases：Nitrogen, argon gas, helium；The sintering temperature is 450-1200 DEG C, Programming rate is 1-5 DEG C/min, sintering time 2-6h；Wherein, the step 4) carbon source is selected from following at least one：Delanium, native graphite, mesocarbon microspheres, graphite It is alkene, carbon nanotubes, phenolic resin, pitch, polyvinylidene fluoride, polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol oxide, poly- Vinyl chloride, polyacrylonitrile, polyacetylene, polyaniline, polythiophene, glucose, sucrose, citric acid, sodium alginate, carboxymethyl cellulose Element, hydroxypropyl cellulose, gelatin, starch, chitosan, alginic acid.
- 7. the SiO for the element doping that claim 3-6 any one of them methods are preparedxThe application of anode material, institute State using the SiO for being element dopingxApplication of the anode material as battery electrode material.
- 8. the application described in claim 7, it is the application of lithium ion battery negative material.
- A kind of 9. energy storage elements, it is characterised in that：The member being prepared containing claim 3-6 any one of them methods The SiO of element dopingxAnode material.
- A kind of 10. portable electric appts, it is characterised in that：Energy storage elements described in usage right requirement 9.
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