CN106654228A - Preparation method of porous SiOx core-shell microspheres - Google Patents
Preparation method of porous SiOx core-shell microspheres Download PDFInfo
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- CN106654228A CN106654228A CN201710041941.3A CN201710041941A CN106654228A CN 106654228 A CN106654228 A CN 106654228A CN 201710041941 A CN201710041941 A CN 201710041941A CN 106654228 A CN106654228 A CN 106654228A
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 preparation method of porous SiOx core-shell microspheres. The preparation method of the porous SiOx core-shell microspheres comprises the following steps: firstly corroding SiO through an HF solution to obtain porous SiOx; ultrasonically dispersing the obtained porous SiOx and epoxy resin, then diluting by using chloroform, adding a curing agent, then slowly adding the materials into a polyvinylpyrrolidone solution together, stirring and reacting; and filtering, washing and drying the product to finally obtain epoxy resin coated porous SiOx core-shell microspheres which can be used for preparing precursors of negative materials of lithium ion batteries; the preparation method of the core-shell microspheres has the advantages of wide raw material sources, simple process and wide application.
Description
Technical field
The invention belongs to field of lithium ion battery material, and in particular to a kind of preparation method of porous SiOx core-shell particles.
Background technology
Increasingly reducing for fossil energy adds the increasingly serious of environmental pollution, and the concern that green energy resource is subject to is more and more,
Lithium ion battery is one of them.Negative material is an important component part in lithium ion battery, current most study
Silicon not only has the theoretical specific capacity more than 10 times of graphite（4200 mAh/g, Li22Si5）With big volume energy density（9786
mAh/cm3）, and the de- lithium platform of rather moderate makes it have good security performance, in addition, source is wide and low cost is also
One big advantage of silicon.However, silicon has huge bulk effect in embedding lithium（Volume Changes about 300%）, the internal stress of generation
Silica flour is easily made, causes plan increase, capacity to decay rapidly；The volumetric expansion of silicon grain during embedding lithium causes particle mutually to squeeze
Pressure, silicon grain shrinks when taking off lithium, is easily caused electrodes conduct Web Grafiti and avalanche；Huge Volume Changes also result in silicon table
The SEI in face（Solid electrolyte film）Film is destroyed, and new exposed silicon continues and electrolyte contacts form new SEI films, and circulation is repeatedly
Cause SEI films more and more thicker, efficiency for charge-discharge is reduced, electrolyte consumption, and then internal resistance increases, capacity attenuation.
For this problem of bulk effect, whole industry field all tries to overcome in idea, including the nanometer of silicon materials
Change, cladding process, loose structure and Composite etc..And it is a kind of current the most frequently used means that cladding is processed, polyethylene is typically used
Pyrrolidones, polyvinyl alcohol, glucose, citric acid etc. are coated with silica-base material ball milling, then pyrolysis processing realizes carbon coating, but its
In problem be that this cladding inherently coats incomplete, and the carbon content of these materials is relatively low, and silicon still can portion after pyrolysis
Divide exposed, generally require to carry out secondary cladding, material particle size becomes big, has agglomeration so that technique becomes loaded down with trivial details, affects production
Efficiency, also increases production cost.Also a kind of CAD cladding process, obtained material has excellent cycle performance and multiplying power
Charge-discharge performance.But the method complex operation, and it is relatively costly, be not suitable for industrialization.
The content of the invention
Present invention aims to the deficiencies in the prior art, now provide a kind of with high specific capacity, first efficiency
With the presoma of the lithium ion battery negative material of good circulation performance, and preparation process is simple, cost is relatively low, is adapted to industrialization
Porous SiOx core-shell particles preparation method.
To solve above-mentioned technical problem, the technical solution used in the present invention is：A kind of preparation of porous SiOx core-shell particles
Method, it is characterised in that：Comprise the following steps：
（1）By mass, configuration quality fraction is 100 parts of the HF solution of 1wt%-10wt%, starts stirring；
（2）The SiO samples that 15 parts were disproportionated are slowly added in HF solution, filtration washing after stirring 0.5-2h, vacuum drying
Obtain porous SiOx；
（3）By gained porous SiOx and epoxy resin ultrasonic disperse 10-30 min, then diluted with 5-15 parts chloroform, Ran Houzai
8-10 part curing agent is added, mixture is prepared；
（4）Said mixture is slowly added in the aqueous solution dissolved with surfactant, the stirring reaction under the conditions of 40-60 DEG C
Filter after 3-6h, wash and be vacuum dried, prepare the porous SiOx core-shell particles of epoxy resin cladding.
Further, the step（2）SiO in the middle SiO samples being disproportionated2Content is 10%-25%.
Further, the step（3）In curing agent be diethylaminopropylamine, double (the 3- amine propyl group) -2,4,8 of 3,9-,
One kind in the oxaspiro hendecane adducts of 10- tetra-, diaminodiphenyl-methane, 650 Versamids, triethylene tetramine.
Further, the step（4）In surfactant be polyvinylpyrrolidone, polyvinyl alcohol, dodecyl
The mixture of one or two kinds of and its above in sodium sulphate, dodecyl sodium sulfate, NPE.
Further, the step（4）In vacuum drying temperature be 50-80 DEG C, the vacuum drying time be 2-6h.
Beneficial effects of the present invention are as follows：
1st, with porous SiOx as core, epoxy resin is shell to the present invention, and the coated porous SiOx of prepared epoxy resin is with its porous
Structure and core shell structure, the aspect researched and developed in material modification, new material has broad application prospects.
2nd, using the preparation method of the present invention, by controlling reaction time and reaction temperature, epoxy resin can be caused to fill
Divide coated porous SiOx, the yield with high core-shell particles.
3rd, it is of the invention with the SiOx of porous as core, with epoxy resin as shell, the coated porous SiOx of prepared epoxy resin
Core-shell particles thermal decomposition product carbon content is high, is suitable as lithium ion battery negative material.
4th, the coated porous SiOx core-shell particles of epoxy resin provided by the present invention have stable core shell structure, after pyrolysis
Carbon can coated Si Ox completely, the bulk effect of silica-base material can either be alleviated, moreover it is possible to completely cut off electrolyte and silica-base material,
Carbon-coating forms stable solid electrolyte membrane, with high reversible specific capacity, high efficiency and excellent cycle performance first.
The 5th, the provided coated porous SiOx core-shell particles SiOx of epoxy resin is provided there is loose structure after corrosion,
The bulk effect of silica-base material can effectively be alleviated.
6th, preparation method process is simple, the raw material sources of the coated porous SiOx core-shell particles of epoxy resin that the present invention is provided
The wide advantage of wide and purposes.
Description of the drawings
Fig. 1 is the step of the embodiment of the present invention 1（1）The SEM of porous SiOx of offer（SEM）Photo；
Fig. 2 is the step of the embodiment of the present invention 1（1）The grain size distribution of porous SiOx of offer；
Fig. 3 is the step of the embodiment of the present invention 1（2）The grain size distribution of the coated porous SiOx core-shell particles of epoxy resin of offer；
Fig. 4 is the step of the embodiment of the present invention 1（2）The SEM photograph of the coated porous SiOx core-shell particles of epoxy resin of offer；
Fig. 5 be the core-shell particles of comparative example 1 pyrolysis after material as button cell loop test figure during negative pole.
Specific embodiment
Hereinafter embodiments of the present invention are illustrated by particular specific embodiment, those skilled in the art can be by this explanation
Content disclosed by book understands easily other advantages and effect of the present invention.
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）By mass, configuration quality fraction is 100 parts of the HF solution of 1wt%-10wt%, starts stirring；
（2）The SiO samples that 15 parts were disproportionated are slowly added in HF solution, filtration washing after stirring 0.5-2h, vacuum drying
Porous SiOx is obtained, the SiO in the SiO samples being disproportionated2Content is 10%-25%；
（3）By gained porous SiOx and epoxy resin ultrasonic disperse 10-30 min, then diluted with 5-15 parts chloroform, Ran Houzai
8-10 part curing agent is added, mixture is prepared, curing agent is diethylaminopropylamine, double (the 3- amine propyl group) -2,4,8 of 3,9-,
One kind in the oxaspiro hendecane adducts of 10- tetra-, diaminodiphenyl-methane, 650 Versamids, triethylene tetramine；
（4）Said mixture is slowly added in the aqueous solution dissolved with surfactant, the stirring reaction under the conditions of 40-60 DEG C
Filter after 3-6h, wash and be vacuum dried, prepare the porous SiOx core-shell particles of epoxy resin cladding, surfactant is
In polyvinylpyrrolidone, polyvinyl alcohol, lauryl sodium sulfate, dodecyl sodium sulfate, NPE one
Kind or two kinds and its above mixture, vacuum drying temperature is 50-80 DEG C, and vacuum drying time is 2-6h.
Embodiment 1
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 5wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to HF
In solution, filtration washing after 1 h of stirring, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 20, are diluted with 10g chloroforms, add 10g curing agent lignocaines
Propylamine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 60 DEG C of stirring reactions 6h, washed and be true
Sky is dried, and obtains the coated porous SiOx core-shell particles of epoxy resin.
Referring to attached Fig. 1 and 2, they are respectively the steps of embodiment 1（1）The stereoscan photograph and grain of porous SiOx of preparation
Footpath distribution map.It can be seen that its median particle diameter is 9.2 μm.
Referring to accompanying drawing 3 and 4 be embodiment 1 prepare the coated porous SiOx core-shell particles of epoxy resin grain size distribution and
SEM photograph, after epoxy resin cladding, its median particle diameter is 19.8 μm, and in the ball-type of rule.
Embodiment 2
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 6wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to HF
In solution, filtration washing after 1.5 h of stirring, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 30, are diluted with 11g chloroforms, add 9g curing agent lignocaine third
Amine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 55 DEG C of stirring reactions 5h, washed and vacuum
It is dried, obtains the coated porous SiOx core-shell particles of epoxy resin.
Comparative example 1
The preparation of the coated porous SiOx core-shell particles pyrogen button half-cell of epoxy resin
The appropriate coated porous SiOx core-shell particles of epoxy resin are placed under atmosphere batch-type furnace, nitrogen atmosphere and are warming up to 800 DEG C,
Temperature retention time is 2h, cools to room temperature with the furnace, and the heating rate of whole process is 4 DEG C/min；Take appropriate thermal decomposition product and CMC,
SBR and SP configuration slurries prepare button half-cell, carry out blue electrical testing.The specific discharge capacity that circulation is 20 times is referring to Fig. 5.
Embodiment 3
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 5wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to HF
In solution, filtration washing after stirring 2h, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 25, are diluted with 9g chloroforms, add 8g curing agent lignocaine third
Amine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 50 DEG C of stirring reactions 4h, washed and vacuum
It is dried, obtains the coated porous SiOx core-shell particles of epoxy resin.
Embodiment 4
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 5wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to HF
In solution, filtration washing after stirring 1h, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 20, are diluted with 10g chloroforms, add 8.5g curing agent lignocaines
Propylamine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 60 DEG C of stirring reactions 4.5h, washed simultaneously
Vacuum drying, obtains the coated porous SiOx core-shell particles of epoxy resin.
Embodiment 5
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 8wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to HF
In solution, filtration washing after stirring 1h, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 25, are diluted with 9.5g chloroforms, add 8.5g curing agent diethylaminos
Base propylamine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 40 DEG C of stirring reactions 5h, washed simultaneously
Vacuum drying, obtains the coated porous SiOx core-shell particles of epoxy resin.
Embodiment 6
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 7.5wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to
In HF solution, filtration washing after stirring 1.5h, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 30, are diluted with 9g chloroforms, add 10g curing agent lignocaine third
Amine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 60 DEG C of stirring reactions 5.5h, washed and be true
Sky is dried, and obtains the coated porous SiOx core-shell particles of epoxy resin.
Embodiment 7
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 6wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to HF
In solution, filtration washing after stirring 1.5h, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 30, are diluted with 8.4g chloroforms, add 8.3g curing agent diethylaminos
Base propylamine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 55 DEG C of stirring reactions 4.5h, washed
And be vacuum dried, obtain the coated porous SiOx core-shell particles of epoxy resin.
Embodiment 8
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 5wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to HF
In solution, filtration washing after stirring 2h, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 25, are diluted with 9g chloroforms, add 8g curing agent lignocaine third
Amine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 50 DEG C of stirring reactions 4h, washed and vacuum
It is dried, obtains the coated porous SiOx core-shell particles of epoxy resin.
Embodiment 9
A kind of preparation method of porous SiOx core-shell particles, comprises the following steps：
（1）The preparation of porous SiOx
Configuration quality fraction is the HF solution 100g of 6wt%, starts stirring；The SiO samples that 15g was disproportionated are slowly added to HF
In solution, filtration washing after stirring 1.5h, vacuum drying obtains porous SiOx；
（2）The preparation of the coated porous SiOx core-shell particles of epoxy resin
Gained porous SiOx and the min of epoxy resin ultrasonic disperse 25, are diluted with 10g chloroforms, add 8g curing agent lignocaine third
Amine；Mixture is slowly added in the aqueous solution dissolved with surfactant, is filtered after 55 DEG C of stirring reactions 5h, washed and vacuum
It is dried, obtains the coated porous SiOx core-shell particles of epoxy resin.
With porous SiOx as core, epoxy resin is shell to the present invention, and coated porous SiOx is more with it for prepared epoxy resin
Pore structure and core shell structure, solution product carbon content is high, lithium ion battery negative material is suitable as, in material modification, new material
Have broad application prospects in terms of research and development；Using the preparation method of the present invention, by controlling reaction time and reaction temperature,
Epoxy resin fully coated porous SiOx, the yield with high core-shell particles can be caused.
The coated porous SiOx core-shell particles of epoxy resin provided by the present invention have stable core shell structure, after pyrolysis
Carbon can coated Si Ox completely, the bulk effect of silica-base material can either be alleviated, moreover it is possible to completely cut off electrolyte and silica-base material, in carbon
Layer forms stable solid electrolyte membrane, with high reversible specific capacity, high efficiency and excellent cycle performance first.
The there is provided coated porous SiOx core-shell particles SiOx of epoxy resin of invention has loose structure, energy after corrosion
Effectively alleviate the bulk effect of silica-base material；The preparation method of the coated porous SiOx core-shell particles of epoxy resin that the present invention is provided
The advantage that process is simple, raw material sources are wide and purposes is wide.
Above-described embodiment is presently preferred embodiments of the present invention, is not the restriction to technical solution of the present invention, as long as
Without the technical scheme that creative work can be realized on the basis of above-described embodiment, it is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (5)
1. a kind of preparation method of porous SiOx core-shell particles, it is characterised in that：Comprise the following steps：
By mass, configuration quality fraction is 100 parts of the HF solution of 1wt%-10wt%, starts stirring；
The SiO samples that 15 parts were disproportionated are slowly added in HF solution, and filtration washing after stirring 0.5-2h, vacuum drying is obtained
Porous SiOx；
By gained porous SiOx and epoxy resin ultrasonic disperse 10-30 min, then diluted with 5-15 parts chloroform, then added
8-10 part curing agent, prepares mixture；
（4）Said mixture is slowly added in the aqueous solution dissolved with surfactant, the stirring reaction under the conditions of 40-60 DEG C
Filter after 3-6h, wash and be vacuum dried, prepare the porous SiOx core-shell particles of epoxy resin cladding.
2. the preparation method of a kind of porous SiOx core-shell particles according to claim 1, it is characterised in that：The step
（2）SiO in the middle SiO samples being disproportionated2Content is 10%-25%.
3. the preparation method of a kind of porous SiOx core-shell particles according to claim 1, it is characterised in that：The step
（3）In curing agent be diethylaminopropylamine, the double oxaspiro hendecane adducts of (3- amine propyl group) -2,4,8,10- four of 3,9-, two
One kind in aminodiphenylmethane, 650 Versamids, triethylene tetramine.
4. the preparation method of a kind of porous SiOx core-shell particles according to claim 1, it is characterised in that：The step
（4）In surfactant be polyvinylpyrrolidone, polyvinyl alcohol, lauryl sodium sulfate, dodecyl sodium sulfate, nonyl
The mixture of one or two kinds of and its above in phenol polyethenoxy ether.
5. the preparation method of a kind of porous SiOx core-shell particles according to claim 1, it is characterised in that：The step
（4）In vacuum drying temperature be 50-80 DEG C, the vacuum drying time be 2-6h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110783531A (en) * | 2018-07-31 | 2020-02-11 | 纳米及先进材料研发院有限公司 | Method for preparing electrode active material and battery electrode |
| CN112436148A (en) * | 2020-11-23 | 2021-03-02 | 溧阳紫宸新材料科技有限公司 | Having TiO2Mesoporous silica negative electrode material with/C composite coating layer and preparation method thereof |
| CN114079054A (en) * | 2020-08-10 | 2022-02-22 | 兰溪致德新能源材料有限公司 | Lithium battery negative electrode material and preparation method thereof |
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| CN112436148B (en) * | 2020-11-23 | 2022-03-18 | 溧阳紫宸新材料科技有限公司 | Having TiO2Mesoporous silica negative electrode material with/C composite coating layer and preparation method thereof |
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