CN108039461A - A kind of silicium cathode material of coated and preparation method thereof - Google Patents
A kind of silicium cathode material of coated and preparation method thereof Download PDFInfo
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- CN108039461A CN108039461A CN201711170946.2A CN201711170946A CN108039461A CN 108039461 A CN108039461 A CN 108039461A CN 201711170946 A CN201711170946 A CN 201711170946A CN 108039461 A CN108039461 A CN 108039461A
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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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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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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- 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 discloses a kind of silicium cathode material of coated, and the silicium cathode material is using silicon grain as core, and using alumina doped Zinc oxide film as shell, certain space is left between silicon grain and shell.The problems such as this space is in order to adapt to volumetric expansion of the silicon grain after embedding lithium, avoid dusting and the decline of electric conductivity.Present invention also offers the preparation method of the negative material, and in one layer of PMMA of silicon grain outer wrapping, one layer of alumina doped zinc-oxide film is then deposited on PMMA, finally removes PMMA and obtains the silicon grain negative material wrapped up with film.Silicium cathode material specific capacity provided by the invention is high, has extended cycle life.
Description
Technical field
The present invention relates to electrochemical technology field, and in particular to field of lithium ion battery, it is more particularly to a kind of as lithium electricity
The method for preparing silicon material of the coated of pond negative material.
Background technology
Clean in energy saving, environmentally friendly trend is pursued now, the development and utilization of the reproducible energy seems particularly heavy
Will.Wherein, the lithium ion battery for having the advantages that operating voltage is high, specific capacity is big, energy density is high and having extended cycle life is subject to
Extensive concern.At present, lithium ion battery is used in electric vehicle, electrostatic storage and can carry electronics
Deng field.It is continuously improved with the performance of lithium ion battery, it is also believed that lithium ion battery will play the part of in following human lives
Drill indispensable role.Therefore, the electrode material for having decisive role to the performance of lithium ion battery is researched and developed energetically.
Silica-base material has at present the theoretical specific capacity 4200mAh/g of maximum in the world, is 10 times of commercial graphite anode.
In addition, silicon is second largest element on the earth, reserves are plentiful, and environment is not polluted.Therefore, silica-base material is considered as most to have hair
Open up the lithium ion battery negative material of potentiality.
But as the negative material of lithium ion battery, silica-base material have two it is very serious the problem of.In lithium ion battery
In lasting charge and discharge process, the volume of silicon can occur acutely to expand, and cause structure to be destroyed, cause silica flour.In addition, electrolyte
It can reduce to form one layer of solid electrolyte film at silicon face.The unstability of silicon volume also results in solid electrolyte film breakage,
After multiple charge and discharge cycles, the film of silicon face becomes increasingly thicker, this not only causes the electric conductivity of electrode to weaken, and also causes
Efficiency of transmission of the lithium ion in negative material reduces.
In recent years, people study emphatically and improve the performance of silicium cathode material.First, people from change material structure side
Face improves the performance of silica-base material.The structure of silica-base material realizes the transformation from the film to nano wire or nano particle.
Volumetric expansion caused by Lithium-ion embeding has been relaxed in the space of naturally occurring in nano wire or nano particle.Except silica-base material
The compound circulation longevity for also greatly enhancing negative material of change on this body structure, silica-base material and other materials
Life.For example carbon and silica-base material can form core shell structure.The space reserved between carbon shell and silicon grain plays volumetric expansion
When cushioning effect.Carbon shell also has it certain inhibitory action.
The content of the invention
The technical problems to be solved by the invention are that the silicon based anode material of lithium ion battery easily occurs dusting and causes electricity
The cycle performance in pond is unstable.
First aspect present invention provides a kind of preparation method of the silicium cathode material of coated, includes the following steps：
A. it is covered in silicon grain surface with coupling agent and obtains the silicon grain on coupling agent modified surface；
B. and then addition PMMA monomers, emulsifying agent, buffer, initiator, crosslinking agent and scattered medium are reacted, in silicon
Particle surface forms PMMA film, obtains the silicon grain of PMMA parcels；
C. the silicon grain of PMMA parcels is infiltrated in the reaction solution containing zinc source and silicon source, and stirred, reaction generation
One layer of alumina doped zinc-oxide film is covered in PMMA film outer surface；
D. PMMA is removed in argon atmosphere high temperature, finally obtained the silicium cathode material of lithium ion battery, the silicium cathode
Material is using silicon grain as core, using alumina doped Zinc oxide film as shell, there is certain space between silicon grain and shell.
In technical scheme, the specific method of step A is as follows：
A-1. nano silicon particles are mixed with ethanol in proper amount, are stirred with magnetic stirrer,
A-2. coupling agent, deionized water, ethanol being mixed, ultrasound mixes,
A-3. the mixed solution of step A-2 is slowly instilled in the nano silicon particles solution of step A-1, and stirred until mixed
Close uniformly, obtain the solution of the silicon grain containing coupling agent modified surface.
In the method for above-mentioned steps A, coupling agent is 3- (isobutene acyl-oxygen) propyl trimethoxy silicane (MPS), and silicon is received
The particle diameter of rice grain is 100nm -5um.
In technical scheme, the thickness of the PMMA film in silicon grain outer wrapping is 100-500nm.
In technical scheme, the specific method of step B is as follows：
B-1. the silicon grain solution on coupling agent modified surface is centrifuged, then alcohol is cleaned by ultrasonic and centrifuges again, repeats several
It is secondary, finally it is dried in vacuo,
B-2. it is put into reaction vessel, stirs evenly after mixing the silicon grain after vacuum drying and deionized water；
B-3. and then PMMA monomers, emulsifying agent, buffer, initiator, crosslinking agent are added, and in nitrogen atmosphere, in 50-
Under 90 DEG C of water baths, magnetic agitation for a period of time, finally obtains the solution for the silicon grain that PMMA films are covered with containing surface.
In the method for above-mentioned steps B-3, methyl methacrylate (MMA), detergent alkylate sodium carbonate, bicarbonate are added
Sodium, potassium peroxydisulfate, triaminotriphenyl-methane (BVA) are reacted.
In technical scheme, the specific method of step C is as follows：
C-1. the solution for the silicon grain that PMMA films are covered with containing surface is centrifuged, then deionized water ultrasound is clear
Wash and centrifuge again, be repeated several times, be finally dried in vacuo；
C-2. dried silicon grain is put into deionized water, under 50-90 DEG C of water bath, magnetic agitation, and adjust
Section solution ph is 8-11；
C-3. then, zinc acetate and aluminium chloride are added in solution, and it is 8- to adjust solution ph with sodium hydroxide solution
11, under 50-90 DEG C of water bath, magnetic agitation is for a period of time；Then solution is centrifuged, then is cleaned by ultrasonic again with deionized water
Centrifugation, is repeated several times, is finally dried in vacuo；
C-4. foregoing C-3 is obtained into solid particle, in the atmosphere of argon gas, 300 DEG C of -400 DEG C of annealing remove PMMA, most
The structure with alumina doped Zinc oxide film parcel silicon grain is obtained afterwards.
In technical scheme, in step C-2 and C-3, the pH value for adjusting solution is 8.5.
In technical scheme, the nano silicon particles of particle diameter 100nm -5um of silicon grain.
The second aspect of the present invention provide a kind of cycle performance available for lithium ion battery well and specific capacity greatly
Silicium cathode material.A kind of silicium cathode material of coated, the silicium cathode material is using silicon grain as core, with alumina doped oxidation
Zinc film is shell, there is certain space between silicon grain and shell.
In technical scheme, a diameter of 100nm -5um of the silicon grain.
In technical scheme, the thickness of the alumina doped zinc-oxide film is 100-500nm, oxidation
The doping concentration of aluminum-doped zinc oxide films is 2-10%.
Third aspect present invention provides a kind of lithium ion battery, it includes：Battery plus-negative plate housing, membrane, electrolyte, bullet
Piece, steel disc, positive and negative anodes current collector, positive and negative pole material, the negative material are the silicium cathode material of foregoing coated.
The silicium cathode material for the lithium ion battery that the present invention is prepared, the silicium cathode material using silicon grain as core, with
Alumina doped Zinc oxide film is shell, there is certain space between silicon grain and shell.This space exists to adapt to silicon grain
The problems such as volumetric expansion after embedding lithium, avoids dusting and the decline of electric conductivity, and solid electrolyte membrane is unstable.
Brief description of the drawings
Attached drawing is for providing a further understanding of the present invention, and becomes part for specification, with the present invention's
Embodiment explains the present invention jointly, does not limit the invention.In the accompanying drawings,
Fig. 1 is one of silicium cathode material preparation flow figure of coated of the present invention.In figure, 1 it is silicon grain, 2 is PMMA, 3
For Zinc oxide doped aluminum oxide film.
Embodiment
The specific embodiment of the invention is described below in conjunction with attached drawing.
With reference to shown in Fig. 1, a kind of silicium cathode material of coated, including it is followed successively by silicon grain 1 from inside to outside, PMMA 2,
Zinc oxide doped aluminum oxide film 3.A diameter of 100nm-the 5um of silicon grain of the present invention, the alumina doped oxidation
The thickness of zinc film is 100-500nm, and the doping concentration of alumina doped zinc-oxide film is 2-10%.First use PMMA films
Silicon grain is wrapped up, then by Zinc oxide doped deposited aluminum oxide thin film in PMMA surface, finally in argon atmosphere, high temperature removal
PMMA to leave certain space between silicon grain and Zinc oxide doped aluminum oxide film.
Present invention also offers the preparation method of the negative material, specific steps include：
(1) nano silicon particles of a diameter of 100nm -5um of 0.1-2g are mixed with 100-500mL ethanol, uses magnetic agitation
Machine stirs 1-30 minutes.
(2) 0.001-0.5g coupling agents, 1-10g deionized waters, 1-20g ethanol are mixed, then ultrasound 1-30 minutes.
(3) mixed solution that step (2) obtains slowly is instilled into the silicon grain solution that step 1) obtains, and at 1-100 DEG C
At a temperature of magnetic agitation 1-24 it is small when, finally obtain the silicon grain with coupling agent modified surface.
(4) solution that step (3) obtains is centrifuged, then is cleaned with EtOH Sonicate, then centrifuged again.Repeat this step
1-3 times.
(5) silicon grain for crossing the surface modification that step (4) centrifugation obtains, is put into vacuum drying chamber, in 1-100 DEG C of ring
Under border, when vacuum drying 1-24 is small.
(6) three necks are put into after the silicon grain after vacuum drying in step (5) is mixed with 1-500mL deionized waters
Flask, is stirred 1-30 minutes with magnetic stirrer.
(7) by 0.1-10mL PMMA monomers, 0.1-1g emulsifying agents, 0.1-1g buffers, 0.1-1g initiators, 0.1-1g
Crosslinking agent pours into three-neck flask, and in nitrogen atmosphere, when magnetic agitation 1-24 is small at a temperature of 1-100 DEG C, finally obtains table
Face is covered with the silicon grain of PMMA films.
(8) solution for obtaining step (7) centrifuges, then is cleaned by ultrasonic with deionized water, then centrifuges again.Repeat this step
1-3 times.
(9) solid that step (8) obtains is put into vacuum drying chamber, in the environment of 1-100 DEG C, vacuum drying 1-24 is small
When.
(10) the dried solid in step (9) is put into 50-500mL deionized waters, in 1-100 DEG C of water bath
Under, when magnetic agitation 1-5 is small, and it is 8-11 with the pH value of ammonium hydroxide adjusting solution, then, by the zinc acetate and 0.2-5g of 0.2-5g
Aluminium chloride add in solution, and it is 8-11 to adjust the pH value of solution with sodium hydroxide solution, when keeping magnetic agitation 1-24 small.
(11) centrifugation of step (10) obtains solution, then with EtOH Sonicate, then centrifuge again.Repeat this step 1-3 times.
(12) solid that step (11) obtains is put into vacuum drying chamber, in the environment of 1-100 DEG C, is dried in vacuo 1-
24。
(13) solid particle that will be obtained in step (12), in the atmosphere of argon gas, 350 DEG C of annealing remove PMMA.Finally
Obtain the structure with alumina doped Zinc oxide film parcel silicon grain.
(14) material obtained in step (13) is mixed to be dissolved in dispersant with bonding agent, conductive agent and slurry is made, it is living
The quality of property material proportion in whole slurry is 60-90%.
(15) with coating machine by slurry film on copper foil made from step (14), and be dried in vacuo 1-24 it is small when, anode
The thickness of film is 10-1000um.
(16) negative electrode film is washed into pole piece with the punching pin of a diameter of 13-18um, and each pole piece is weighed.
(17) battery is assembled and pressed according to the order of anode cover, pole piece, membrane, lithium piece, steel disc, shrapnel and negative electrode casing
Piece.In an assembling process, 1-10 drop electrolyte is added.
The method of the present invention improves the expansion of silicium cathode material volume, the instability problem of solid electrolyte, so that very well
The efficiency for charge-discharge for improving battery and battery cycle performance.
Embodiment
(1) nano silicon particles of 0.4g are mixed with 200mL ethanol, is stirred 15 minutes with magnetic stirrer.
(2) it is 0.35g coupling agents, 7g deionized waters, the mixing of 13g ethanol is then 10 minutes ultrasonic.
(3) mixed solution that step (2) obtains slowly is instilled into the silicon grain solution that step 1) obtains, and in 80 DEG C of temperature
When lower magnetic agitation 12 is small.Finally obtain the silicon grain with coupling agent modified surface.
(4) solution that step (3) obtains is centrifuged, then is cleaned with EtOH Sonicate, then centrifuged again, repeat this step
3 times.
(5) silicon grain for crossing the surface modification that step (4) centrifugation obtains, is put into vacuum drying chamber, in 60 DEG C of environment
Under, when vacuum drying 12 is small.
(6) three necks are put into after the silicon grain after vacuum drying in step (5) is mixed with 150mL deionized waters to burn
Bottle, is stirred 5 minutes with magnetic stirrer.
(7) by 0.019g detergent alkylates sodium carbonate (SDBS), 0.24g sodium acid carbonates (NaHCO3), 0.006g persulfuric acid
Potassium (KPS), 6mL methyl methacrylates (MMA), 0.12g triaminotriphenyl-methanes (BVA) pour into three-neck flask, and in nitrogen
In atmosphere, when magnetic agitation 4 is small at a temperature of 80 DEG C.Finally obtain the silicon grain that surface is covered with PMMA films.
(8) solution obtained step (7) centrifuges, then with EtOH Sonicate, then centrifuges again.Repeat this step 3 time.
(9) solid that step (8) obtains is put into vacuum drying chamber, in the environment of 60 DEG C, when vacuum drying 12 is small.
(10) dried solid in step (9) is put into 100mL deionized waters, under 80 DEG C of water baths, magnetic force
Stir 1.5 it is small when, and with ammonium hydroxide adjust solution pH value be 8.5, then, by the two water zinc acetates of 1.2g and six water of 0.05g
Aluminium chloride is added in solution, and is 8.5 with the pH value of sodium hydroxide solution adjusting solution, when keeping magnetic agitation 18 small.
(11) centrifugation of step (10) obtains solution, then with EtOH Sonicate, then centrifuge again.Repeat this step 3 time.
(12) solid that step (11) obtains is put into vacuum drying chamber, in the environment of 60 DEG C, when vacuum drying 12 is small.
(13) solid particle that will be obtained in step (12), in the atmosphere of argon gas, 350 DEG C keep 2 hour annealing to go
Except PMMA.Finally obtain the structure with alumina doped Zinc oxide film parcel silicon grain.
(14) material obtained in step (13) is mixed with Kynoar (PVDF), carbon black and is dissolved in N- crassitudes
Slurry is made in ketone (NMP), the mass ratio of active material, bonding agent and conductive agent is 7:1:2, and the quality of NMP is activity
10 times of material.
(15) with coating machine by slurry film on copper foil made from step (14).And it is dried in vacuo 8 under 120 DEG C of environment
Hour, the average thickness of negative electrode film is 100-160um.
(16) negative electrode film is washed into pole piece with the punching pin of a diameter of 13um, and each pole piece is weighed.
(17) battery is assembled and pressed according to the order of anode cover, pole piece, membrane, lithium piece, steel disc, shrapnel and negative electrode casing
Piece, in an assembling process, adds 5 drop electrolyte.
The method of the present invention improves the expansion of silicium cathode material volume and solid electrolyte stability.
Basic principle, main feature and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention simply illustrates the present invention described in examples detailed above and specification from the limitation of examples detailed above
Principle, various changes and modifications of the present invention are possible without departing from the spirit and scope of the present invention, these change and
Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its is equal
Thing defines.
Claims (10)
1. a kind of preparation method of the silicium cathode material of coated, includes the following steps：
A. it is covered in silicon grain surface with coupling agent and obtains the silicon grain on coupling agent modified surface；
B. and then addition PMMA monomers, emulsifying agent, buffer, initiator, crosslinking agent and scattered medium are reacted, in silicon grain
Surface forms PMMA film, obtains the silicon grain of PMMA parcels；
C. the silicon grain of PMMA parcels is infiltrated in the reaction solution containing zinc source and silicon source, and stirred, reaction generates one
The alumina doped zinc-oxide film of layer is covered in PMMA film outer surface；
D. PMMA is removed in argon atmosphere high temperature, finally obtained the silicium cathode material of lithium ion battery, the silicium cathode material
Using silicon grain as core, using alumina doped Zinc oxide film as shell, there is certain space between silicon grain and shell.
2. preparation method according to claim 1, it is characterised in that step A specifically includes as follows：
A-1. nano silicon particles are mixed with ethanol in proper amount, is stirred with magnetic stirrer；
A-2. coupling agent, deionized water, ethanol are mixed, ultrasound mixes；
A-3. the mixed solution of step A-2 is slowly instilled in the nano silicon particles solution of step A-1, and stirred equal until mixing
It is even, obtain the solution of the silicon grain containing coupling agent modified surface.
3. preparation method according to claim 1, it is characterised in that step B specifically includes as follows：
B-1. the silicon grain solution on coupling agent modified surface is centrifuged, then alcohol is cleaned by ultrasonic and centrifuges again, is repeated several times, most
After be dried in vacuo；
B-2. it is put into reaction vessel, stirs evenly after mixing the silicon grain after vacuum drying and deionized water；
B-3. and then PMMA monomers, emulsifying agent, buffer, initiator, crosslinking agent are added, and in nitrogen atmosphere, at 50-90 DEG C
Under water bath, magnetic agitation for a period of time, finally obtains the solution for the silicon grain that PMMA films are covered with containing surface.
4. preparation method according to claim 3, it is characterised in that in above-mentioned steps B-3, add methyl methacrylate
Ester (MMA), detergent alkylate sodium carbonate, sodium acid carbonate, potassium peroxydisulfate, triaminotriphenyl-methane (BVA) are reacted.
5. preparation method according to claim 1, it is characterised in that step C specifically includes as follows：
C-1. the solution for the silicon grain that PMMA films are covered with containing surface is centrifuged, then deionized water is cleaned by ultrasonic again
Centrifugation, is repeated several times, is finally dried in vacuo；
C-2. dried silicon grain is put into deionized water, under 50-90 DEG C of water bath, magnetic agitation, and use ammonium hydroxide
Adjusting solution ph is 8-11；
C-3. then, zinc acetate and aluminium chloride are added in solution, and it is 8-11 to adjust solution ph with sodium hydroxide solution,
Under 50-90 DEG C of water bath, magnetic agitation is for a period of time；Then solution is centrifuged, then is cleaned with deionized water and centrifuged again, repeated
Several times, finally it is dried in vacuo；
C-4. foregoing C-3 is obtained into solid particle, in the atmosphere of argon gas, 300 DEG C of -400 DEG C of annealing remove PMMA, finally
To the structure with alumina doped Zinc oxide film parcel silicon grain.
6. preparation method according to claim 5, it is characterised in that in step C-2 and C-3, adjust the pH value of solution
For 8.5.
7. a kind of silicium cathode material for the coated being prepared according to any one of claim 1-6 method, it is characterised in that should
Silicium cathode material is using silicon grain as core, using alumina doped Zinc oxide film as shell, has between silicon grain and shell certain
Space.
8. the silicium cathode material of coated according to claim 7, it is characterised in that the silicon grain is a diameter of
100nm—5um。
9. the silicium cathode material of coated according to claim 7, it is characterised in that the alumina doped zinc oxide
The thickness of film is 100-500nm, and the doping concentration of alumina doped zinc-oxide film is 2-10%.
10. a kind of lithium ion battery, it includes：Battery plus-negative plate housing, membrane, electrolyte, shrapnel, steel disc, positive and negative anodes afflux
Device, positive and negative pole material, it is characterised in that the negative material is claim 7-9 any one of them coated silicium cathode materials
Material or the coated silicium cathode material that such as claim 1-6 any one of them methods are prepared.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109560263A (en) * | 2018-10-24 | 2019-04-02 | 东莞理工学院 | A kind of preparation method of oxide coated by zinc silicium cathode material |
| CN112993223A (en) * | 2021-02-07 | 2021-06-18 | 西南科技大学 | Lithium ion battery cathode material with double-layer coating structure and preparation method thereof |
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