CN106848276A - A kind of titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material and preparation method thereof - Google Patents
A kind of titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN106848276A CN106848276A CN201710258227.XA CN201710258227A CN106848276A CN 106848276 A CN106848276 A CN 106848276A CN 201710258227 A CN201710258227 A CN 201710258227A CN 106848276 A CN106848276 A CN 106848276A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- 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 titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material and preparation method thereof, it is characterised in that：After silica flour and ammonium titanium fluoride are reacted under hydrothermal conditions, products therefrom is further heat-treated, that is, obtain with titanium dioxide as shell, with nano silicon particles as kernel and the titanium dioxide of core-shell structure with cavity coats silicon lithium ion battery cathode material between shell and kernel.Preparation method of the invention is easy and effective, the shell of prepared silicon based anode material is that constitutionally stable titanium dioxide, kernel are the cavitys that bulk effect during silicon removal lithium embedded can be also buffered between elementary silicon, the nucleocapsid that can provide height ratio capacity during removal lithium embedded, thus with good storage lithium performance.
Description
Technical field
The present invention relates to a kind of lithium ion battery silicon cathode material and preparation method thereof.
Background technology
Lithium ion battery because with it is easy to use, low in the pollution of the environment, without geographical restrictions, transformation efficiency high, specific energy and
The advantages of specific power is high and it is wide concerned.It is new under New Energy Industry and the booming background of new-energy automobile industry
Efficient energy storage device plays very important effect herein with the design and exploitation of material, and has turned into this field of restriction
One of fast-developing bottleneck.
Lithium ion battery is divided into positive pole, negative pole, barrier film, electrolyte and shell from structure.Negative pole generally comprises copper afflux
Body, active material, conductive agent and binding agent.Graphite is current commercial Li-ion battery often with negative material, but its theory ratio
Capacity is only 372mAh/g, it is impossible to meet New Energy Industry and new-energy automobile industry for energy storage device in energy density side
The requirement in face.Compared with traditional graphite cathode, silicon can form Li with lithium at room temperature15Si4Alloy, theoretical capacity is reachable
3590mAh/g, is nearly ten times or so of graphite theoretical specific capacity, and its discharge platform is slightly above graphite, and security is more preferable.But
It is, the Li that the embedding lithium of silicium cathode material is formed15Si4Meeting causes the enormousness more than 300% to expand, and silicon is in lithiumation and de- lithium
During produce volumetric expansion repeatedly and shrink so as to cause the broken of particle, and cause silicon and conductive additive and collector
Lose good electrical contact.Due to this volumetric expansion-blockage effect, silicon is also difficult to be formed in the electrolytic solution the solid electricity of stabilization
Solution matter interface (SEI) film, along with the destruction of electrode structure, new SEI films is constantly formed in the silicon face for exposing, and aggravates silicon
Corrosion and capacity attenuation.Core shell structure silicon composite of the design with certain cavity volume is solve the above problems effective
Method, it is the material that stabilization SEI films can be formed during removal lithium embedded that outer shell is selected, and cavity certain between nucleocapsid
Volume can buffer the bulk strain effect of silicon.
The content of the invention
For the weak point existing for above-mentioned prior art, prepared the invention provides a kind of simple effective method and had
There is the titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material of certain cavity volume, to lithium-ion electric can be lifted
High rate performance and cyclical stability of pond silicon based anode material etc..
The present invention solves technical problem, adopts the following technical scheme that：
Titanium dioxide of core-shell structure of the present invention coats the preparation method of silicon lithium ion battery cathode material, is with ammonium titanium fluoride
Used as titanium source, the mechanism cladding titanium dioxide for passing through " hydrolysis-etching-deposition " to silicon, surface is oxidized silicon under hydrothermal conditions
Into silica, ammonium titanium fluoride hydrolysis generation titanium dioxide while also producing HF, can etch the silicon oxide layer of silicon face, make two
Titanium oxide is formed in silicon face and coated, while the cavity structure of certain volume can be produced.Specifically carry out as follows：
(1) by silica flour addition ammonium titanium fluoride solution, ultrasound obtains mixture to being uniformly dispersed；Also can be by by fluorine titanium
Acid ammonium solution obtains mixture in adding silica flour suspension；
(2) by the mixture at a temperature of 50~200 DEG C 0.5~24h of hydro-thermal reaction, be then centrifuged for separate, to institute
Obtain solid product washing, dry；
(3) solid product obtains target product with 300~800 DEG C of 0.5~24h of heat treatment after drying.
Preferably, silica flour described in step (1) and the mass ratio of ammonium titanium fluoride are 0.2~5, the concentration of the ammonium titanium fluoride
It is 1~50mM.
Preferably, the average grain diameter of silica flour described in step (1) is less than 1 μm.
Preferably, described in step (1) ultrasound temperature for room temperature, the time be 0.5~2h.
Preferably, step (3) heat treatment is in nitrogen, argon gas, nitrogen/argon gas gaseous mixture, nitrogen/hydrogen mixed gas
Or under the atmosphere of argon gas/hydrogen mixed gas.
Silicon lithium ion is coated the present invention further discloses through the titanium dioxide of core-shell structure prepared by above-mentioned preparation method
Cell negative electrode material, it is that, with titanium dioxide as shell, with nano silicon particles as kernel, have between the shell and kernel
The cavity of certain volume.
Compared with prior art, beneficial effects of the present invention are embodied in：
The internal cavities of the core shell structure silicon based composite material with cavity reported are hard in outer silicon cladding in advance
Template (such as silica, calcium carbonate), then realizes, step complexity is cumbersome by way of acid etch hard template.And this hair
Bright preparation method is easy and effective, and the step hydro-thermal reaction by ammonium titanium fluoride and silicon is the product that can obtain object construction, after
Continuous heat treatment step can further regulate and control the storage lithium performance of product；The final products shell obtained according to preparation method of the invention
It is titanium dioxide, there is the structure of stabilization during removal lithium embedded；Internal core is elementary silicon, can provide specific capacity high；
There is certain cavity volume between nucleocapsid, the bulk effect during silicon removal lithium embedded can be buffered, so that the negative material
With good chemical property.
Brief description of the drawings
Fig. 1 is the titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material prepared by the embodiment of the present invention 1
TEM photos；
Fig. 2 is the XRD that titanium dioxide of core-shell structure prepared by the embodiment of the present invention 1 coats silicon lithium ion battery cathode material
Figure；
Fig. 3 is titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material and original prepared by the embodiment of the present invention 1
Cycle performance figure of the beginning silicon materials under 0.1C multiplying powers.
Specific embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out under premised on technical solution of the present invention
Implement, give detailed implementation method and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment 1
The present embodiment prepares titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material as follows：
(1) by 0.1g silica flours (average grain diameter is 200nm) add 34mL 15mM ammonium titanium fluoride solution in, at room temperature ultrasound
Treatment 1h, obtains mixture；
(2) mixture is transferred in water heating kettle and reacts 3h in 80 DEG C, be then centrifuged for separating, gained solid product is spent
Ion water washing, 70 DEG C dry 12h；
(3) under nitrogen atmosphere protection, solid product after drying is heat-treated 2h in 500 DEG C, is obtained after being cooled to room temperature
Final products.
Fig. 1 is that the TEM of the titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material prepared by the present embodiment shines
Piece, it can be seen that product is core shell structure, shell titanium dioxide, kernel elementary silicon, and has the cavity of certain volume between nucleocapsid.
Fig. 2 is the XRD of the titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material prepared by the present embodiment,
It can be seen that resulting materials include two kinds of diffraction maximums of material of titanium dioxide and silicon.Figure Plays card PDF#21-
Corresponding to 1272 is TiO2Diffraction maximum, corresponding to standard card PDF#27-1402 be Si diffraction maximum.
Fig. 3 is titanium dioxide of core-shell structure cladding silicon lithium ion battery cathode material and the original silicon prepared by the present embodiment
Cycle performance figure of the material under 0.1C multiplying powers.During test, two kinds of materials respectively with sodium alginate as binding agent, acetylene black be
Conductive additive, according to 6:2:2 ratio applies making electrode slice on Copper Foil and carries out half-cell performance test.Can be with from Fig. 3
Find out, original silicon material circulates specific capacity under 0.1C multiplying powers and decays rapidly, specific capacities are close to 0 after 50 times.And the present embodiment
Prepared coated by titanium dioxide silicium cathode material circulates 100 specific volumes later under 0.1C (defining 1C=3590mA/g) multiplying power
Amount can still remain 1069mAh/g.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of titanium dioxide of core-shell structure coats the preparation method of silicon lithium ion battery cathode material, it is characterised in that including
Following steps：
(1) by silica flour addition ammonium titanium fluoride solution, ultrasound obtains mixture to being uniformly dispersed；
(2) by the mixture at a temperature of 50~200 DEG C 0.5~24h of hydro-thermal reaction, be then centrifuged for separating, it is solid to gained
Body product is washed, dried；
(3) solid product obtains target product with 300~800 DEG C of 0.5~24h of heat treatment after drying.
2. titanium dioxide of core-shell structure according to claim 1 coats the preparation method of silicon lithium ion battery cathode material,
It is characterized in that：Silica flour described in step (1) is 0.2~5 with the mass ratio of ammonium titanium fluoride, and the concentration of the ammonium titanium fluoride is 1
~50mM.
3. titanium dioxide of core-shell structure according to claim 1 coats the preparation method of silicon lithium ion battery cathode material,
It is characterized in that：The average grain diameter of silica flour described in step (1) is less than 1 μm.
4. titanium dioxide of core-shell structure according to claim 1 coats the preparation method of silicon lithium ion battery cathode material,
It is characterized in that：The temperature of ultrasound described in step (1) is room temperature, the time is 0.5~2h.
5. titanium dioxide of core-shell structure according to claim 1 coats the preparation method of silicon lithium ion battery cathode material,
It is characterized in that：Step (3) heat treatment is in nitrogen, argon gas, nitrogen/argon gas gaseous mixture, nitrogen/hydrogen mixed gas or argon
Under the atmosphere of gas/hydrogen mixed gas.
6. the titanium dioxide of core-shell structure coated Si lithium in a kind of Claims 1 to 5 described in any one prepared by preparation method
Ion battery cathode material.
7. negative material according to claim 6, it is characterised in that：It with titanium dioxide as shell, with silicon grain is interior to be
Core, has cavity between the shell and kernel.
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Cited By (8)
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| CN107623104A (en) * | 2017-09-25 | 2018-01-23 | 常州市宇科不绣钢有限公司 | A kind of structure silicon-based negative material of multi-buffer and preparation method thereof |
| CN109761239A (en) * | 2019-01-18 | 2019-05-17 | 齐鲁工业大学 | It is a kind of sensing, photoelectricity or lithium ion battery composite material and preparation method |
| CN109888256A (en) * | 2019-04-01 | 2019-06-14 | 中南大学 | A kind of Si@SiOx@N doping TiO2-δMaterial and its preparation method and application |
| CN110085852A (en) * | 2019-05-28 | 2019-08-02 | 中国科学院重庆绿色智能技术研究院 | Conductive structure and electrode |
| CN110459757A (en) * | 2019-08-29 | 2019-11-15 | 蜂巢能源科技有限公司 | Negative electrode material of lithium ion battery and preparation method thereof |
| CN111463419A (en) * | 2020-04-28 | 2020-07-28 | 苏州宇豪纳米材料有限公司 | Silicon-based @ titanium niobium oxide core-shell structure anode material and preparation method thereof |
| CN111477858A (en) * | 2020-05-08 | 2020-07-31 | 广西师范大学 | Si @ TiO2Preparation method of hollow core-shell composite material |
| CN115784300A (en) * | 2022-12-19 | 2023-03-14 | 攀钢集团研究院有限公司 | Preparation method of titanium dioxide coated silicon composite material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107623104A (en) * | 2017-09-25 | 2018-01-23 | 常州市宇科不绣钢有限公司 | A kind of structure silicon-based negative material of multi-buffer and preparation method thereof |
| CN109761239A (en) * | 2019-01-18 | 2019-05-17 | 齐鲁工业大学 | It is a kind of sensing, photoelectricity or lithium ion battery composite material and preparation method |
| CN109888256A (en) * | 2019-04-01 | 2019-06-14 | 中南大学 | A kind of Si@SiOx@N doping TiO2-δMaterial and its preparation method and application |
| CN110085852A (en) * | 2019-05-28 | 2019-08-02 | 中国科学院重庆绿色智能技术研究院 | Conductive structure and electrode |
| CN110459757A (en) * | 2019-08-29 | 2019-11-15 | 蜂巢能源科技有限公司 | Negative electrode material of lithium ion battery and preparation method thereof |
| CN111463419A (en) * | 2020-04-28 | 2020-07-28 | 苏州宇豪纳米材料有限公司 | Silicon-based @ titanium niobium oxide core-shell structure anode material and preparation method thereof |
| CN111463419B (en) * | 2020-04-28 | 2022-04-01 | 苏州宇豪纳米材料有限公司 | Silicon-based @ titanium niobium oxide core-shell structure anode material and preparation method thereof |
| CN111477858A (en) * | 2020-05-08 | 2020-07-31 | 广西师范大学 | Si @ TiO2Preparation method of hollow core-shell composite material |
| CN115784300A (en) * | 2022-12-19 | 2023-03-14 | 攀钢集团研究院有限公司 | Preparation method of titanium dioxide coated silicon composite material |
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Application publication date: 20170613 |