CN105895880A - Preparation method of silicon dioxide composite material for negative electrode of lithium-ion battery - Google Patents
Preparation method of silicon dioxide composite material for negative electrode of lithium-ion battery Download PDFInfo
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- CN105895880A CN105895880A CN201610348117.8A CN201610348117A CN105895880A CN 105895880 A CN105895880 A CN 105895880A CN 201610348117 A CN201610348117 A CN 201610348117A CN 105895880 A CN105895880 A CN 105895880A
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 provides a preparation method of a silicon dioxide composite material for a negative electrode of a lithium-ion battery. The method comprises three processes, namely preparation of a [carbon nanotube/silicon dioxide] composite material, preparation of a silicon dioxide precursor and preparation of the silicon dioxide composite material. Ethyl alcohol, distilled water, ammonium hydroxide, hexadecyl trimethyl ammonium bromide, acid-treated carbon nanotube, ethyl orthosilicate, deionized water and absolute ethyl alcohol are utilized in the preparation process of the [carbon nanotube/silicon dioxide] composite material. The carbon nanotube in the prepared silicon dioxide composite material has relatively high conductivity, large specific surface area and relatively large expansion coefficient as an inner core; the expansion effect of the silicon dioxide in the charging and discharging process of the lithium-ion battery can be reduced; the structure stability of the silicon dioxide composite material is improved; and the cycle performance of the silicon dioxide composite material is finally improved.
Description
Technical field
The invention belongs to lithium ion battery negative material preparing technical field, especially a kind of lithium ion battery is born
The silicon dioxide composite material preparation method of pole.
Background technology
Lithium ion battery has energy density height, has extended cycle life and advantages of environment protection, has been widely used
In Portable movable electronics market, and show in the traffic such as electric automobile and peak load regulation network and energy storage field
Tempting application scape.
The lithium ion battery negative material of Current commercial mainly uses graphite, and the theoretical specific capacity of graphite is only
372mAh/g, constrains lithium ion battery as the electrokinetic cell actual application in the field such as traffic and energy storage.
Silicon, silicon-base alloy and Si oxide etc. have higher theoretical specific capacity and preferably safety, are lithiums
The preferable substitution material of ion battery cathode material. wherein silicon dioxide has preparation simplicity, low cost and ring
The advantages such as border is friendly, it has also become one of study hotspot of silicon based anode material, but the titanium dioxide of lump shaped crystalline
Its electrical conductivity of silicon is relatively low and Si-O bonding energy is relatively big, is unfavorable for the carrying out that lithium ion battery reacts in deintercalation.
Additionally, the change in volume huge during removal lithium embedded of silicon dioxide can cause the efflorescence of negative material, lose
The phenomenons such as electrical contact or specific capacity rapid decay.
Researcher realizes its reversible storage lithium row by preparing unbodied silica nano material at present
For, there is good cyclical stability.Such as Chinese patent CN104037396 A, to disclose a kind of silico-carbo polynary
Composite negative pole material and preparation method thereof, is made up of soft graphite, nano-silicon and agraphitic carbon, agraphitic carbon
Being obtained after high temperature pyrolysis by organic carbon source, soft graphite is that expanded graphite obtains after pressure, prepares
Silico-carbo multi-component composite anode material to have capacity high, but cycle performance is poor, complicated process of preparation, it is difficult to product
Industry metaplasia is produced.
Summary of the invention
For solving the problems referred to above, the invention provides the silicon dioxide composite wood of a kind of used as negative electrode of Li-ion battery
Preparation method for material, the silicon dioxide composite material prepared has that capacity is high, cycle life is good, liquid is protected in imbibition
The features such as ability is strong, preparation technology is simple.
A kind of silicon dioxide composite material preparation method of used as negative electrode of Li-ion battery, this silicon dioxide composite wood
Preparation method for material includes [CNT/silicon dioxide] prepared by composite, prepared by silica precursor and two
Silica composite material prepares three big processes, the mistake wherein prepared at [CNT/silicon dioxide] composite
Journey uses ethanol, distilled water, ammonia, cetyl trimethylammonium bromide, acid-treated carbon nanometer
Pipe, tetraethyl orthosilicate, deionized water and dehydrated alcohol, it is desirable to acid-treated carbon nano tube structure formula is
-COOH ,-OH and percent grafting controls 0.5~5%, each process is described below:
I, the preparation of [CNT/silicon dioxide] composite:
By the mL i.e. ethanol of ratio: distilled water: ammonia: cetyl trimethylammonium bromide CTAB=[100~150]:
[20~50]: [1~2]: [0.1~0.2] is sequentially added into ethanol, distilled water, ammonia and ten in reaction utensil
Six alkyl trimethyl ammonium bromides also stir and make it fully dissolve, then add 0.1~0.2g in reaction utensil
Through acid-treated CNT ultrasonic disperse 40min, treat that acid-treated CNT is completely dispersed backward
Reaction utensil is slowly added dropwise 1.0g tetraethyl orthosilicate and is stirred at room temperature 4~12h, afterwards by reaction utensil
Product successively with deionized water, dehydrated alcohol respectively be centrifuged clean, finally carry out at 80 DEG C
It is dried, [CNT/silicon dioxide] composite can be prepared;
II, the preparation of silica precursor:
[CNT/silicon dioxide] composite prepared in above-mentioned I is put in reactor and added
Colophonium, [CNT/silicon dioxide] composite: Colophonium=100g: [30~60] g, turning of reactor
Speed controls 300~1000r/min, and the fusion temperature of reactor controls at 20~100 DEG C, melting of reactor
The conjunction time controls, 200~400min, to prepare silica precursor afterwards;
III, the preparation of silicon dioxide composite material:
The silica precursor prepared in above-mentioned II is placed in the high temperature furnace of 2500~3000 DEG C and carries out stone
Inkization processes, and comes out of the stove and naturally cools to room temperature, can prepare after the complete graphitization of silica precursor
Go out silicon dioxide composite material.
Owing to using techniques described above scheme, the present invention produces following good effect:
1, relatively abundant, uniform negative charge, beneficially dioxy are contained through its surface of acid-treated CNT
The uniform deposition of SiClx layer, can improve tap density and the electric conductivity of silicon dioxide composite material.
2, the CNT in silicon dioxide composite material then has higher electrical conductivity, big ratio as kernel
Surface area and the bigger coefficient of expansion, can reduce swollen in lithium ion battery charge and discharge process of silicon dioxide
Swollen effect, improves the structural stability of silicon dioxide composite material, and finally improves silicon dioxide composite material
Cycle performance.
3, Colophonium is as external sheath silicon dioxide, can reduce silicon dioxide and lithium-ion battery electrolytes
Directly contact, reduces the side reaction of silicon dioxide composite material, makes the overall performance of silicon dioxide composite material
It is improved.
Accompanying drawing explanation
Fig. 1 is the surface sweeping Electronic Speculum SEM figure of the silicon dioxide composite material that embodiment 1 is prepared;
Fig. 2 is the cyclic curve comparison diagram of three embodiments and comparative example.
Detailed description of the invention
The present invention is the silicon dioxide composite material preparation method of a kind of used as negative electrode of Li-ion battery.System of the present invention
Standby go out silicon dioxide composite material, CNT therein then has higher electrical conductivity, big as kernel
Specific surface area and the bigger coefficient of expansion, silicon dioxide can be reduced in lithium ion battery charge and discharge process
Expansion, improve silicon dioxide composite material structural stability, and finally improve silicon dioxide be combined
The cycle performance of material.
The silicon dioxide composite material preparation method of the present invention includes [CNT/silicon dioxide] composite
Preparation, silica precursor preparation and silicon dioxide composite material prepare three big processes, wherein at [carbon
Nanotube/silicon dioxide] use to ethanol, distilled water, ammonia, hexadecane during composite preparation
Base trimethylammonium bromide, acid-treated CNT, tetraethyl orthosilicate, deionized water and dehydrated alcohol,
Require that percent grafting controls 0.5~5% acid-treated carbon nano tube structure formula for-COOH ,-OH.
According to technical scheme of the present invention, now enumerate three embodiments.
Embodiment 1:
I, the preparation of [CNT/silicon dioxide] composite: in reaction utensil, be sequentially added into 120mL second
Alcohol, 40mL distilled water, 1.5mL ammonia and 0.2mL cetyl trimethylammonium bromide also stir and make it
Fully dissolve, then in reaction utensil, add 0.15g through acid-treated CNT ultrasonic disperse 40min,
Treat acid-treated CNT to be completely dispersed in backward reaction utensil and be slowly added dropwise 1.0g tetraethyl orthosilicate and in room
Stir 8h under temperature, afterwards the product in reaction utensil is carried out respectively with deionized water, dehydrated alcohol successively from
The heart cleans, and is finally dried at 80 DEG C, can prepare [CNT/silicon dioxide] composite.
II, the preparation of silica precursor: the 100g [CNT/titanium dioxide will prepared in above-mentioned I
Silicon] composite puts in reactor and adds 50g Colophonium, and the rotating speed of reactor controls at 500r/min, instead
The fusion temperature answering still controls at 80 DEG C, and the time of fusion of reactor controls at 300min, can prepare afterwards
Go out silica precursor.
III, the preparation of silicon dioxide composite material: the silica precursor prepared in above-mentioned II is placed on
The high temperature furnace of 2800 DEG C carries out graphitization processing, comes out of the stove after the complete graphitization of silica precursor and oneself
So it is cooled to room temperature, silicon dioxide composite material can be prepared.
Embodiment 2:
I, the preparation of [CNT/silicon dioxide] composite: in reaction utensil, be sequentially added into 100mL second
Alcohol, 20mL distilled water, 1.0mL ammonia and 0.1mL cetyl trimethylammonium bromide also stir and make it
Fully dissolve, then in reaction utensil, add 0.1g through acid-treated CNT ultrasonic disperse 40min,
Treat that acid-treated CNT is completely dispersed in backward reaction utensil and be slowly added dropwise 1.0g tetraethyl orthosilicate also
At room temperature stir 4h, afterwards the product in reaction utensil is entered respectively with deionized water, dehydrated alcohol successively
Row eccentric cleaning, is finally dried at 80 DEG C, can prepare [CNT/silicon dioxide] and be combined
Material.
II, the preparation of silica precursor: the 100g [CNT/titanium dioxide will prepared in above-mentioned I
Silicon] composite puts in reactor and adds 30g Colophonium, and the rotating speed of reactor controls at 300r/min, instead
The fusion temperature answering still controls at 20 DEG C, and the time of fusion of reactor controls at 200min, can prepare afterwards
Go out silica precursor.
III, the preparation of silicon dioxide composite material: the silica precursor prepared in above-mentioned II is placed on
The high temperature furnace of 2500 DEG C carries out graphitization processing, comes out of the stove after the complete graphitization of silica precursor and oneself
So it is cooled to room temperature, silicon dioxide composite material can be prepared.
Embodiment 3:
I, the preparation of [CNT/silicon dioxide] composite: in reaction utensil, be sequentially added into 150mL second
Alcohol, 50mL distilled water, 2.0mL ammonia and 0.2mL cetyl trimethylammonium bromide also stir and make it
Fully dissolve, then in reaction utensil, add 0.2g through acid-treated CNT ultrasonic disperse 40min,
Treat acid-treated CNT to be completely dispersed in backward reaction utensil and be slowly added dropwise 1.0g tetraethyl orthosilicate and in room
Stir 12h under temperature, afterwards the product in reaction utensil is carried out respectively with deionized water, dehydrated alcohol successively from
The heart cleans, and is finally dried at 80 DEG C, can prepare [CNT/silicon dioxide] composite.
II, the preparation of silica precursor: the 100g [CNT/titanium dioxide will prepared in above-mentioned I
Silicon] composite puts in reactor and adds 60g Colophonium, and the rotating speed of reactor controls at 1000r/min,
The fusion temperature of reactor controls at 100 DEG C, and the time of fusion of reactor controls at 400min, afterwards
Prepare silica precursor.
III, the preparation of silicon dioxide composite material: the silica precursor prepared in above-mentioned II is placed on
The high temperature furnace of 3000 DEG C carries out graphitization processing, comes out of the stove after the complete graphitization of silica precursor
And naturally cool to room temperature, silicon dioxide composite material can be prepared.
Fig. 1 is the surface sweeping Electronic Speculum SEM figure of the silicon dioxide composite material that embodiment 1 is prepared, embodiment 2-3
Surface sweeping Electronic Speculum SEM figure close with Fig. 1, from figure 1 it appears that silicon dioxide composite material present core-
Shell structure, with CNT as core, outside is coated with silicon oxide, through compound with reference to measuring at silicon dioxide
In material: carbon content is about 98.0~99.4%, silicone content is about 0.4~1.5%, specific surface area be about 2.5~
4.5m2/g。
Button electrical testing:
Respectively gained lithium ion battery negative material in embodiment 1~3 is assembled into button cell A1, A2, A3,
Binding agent LA132, conductive agent SP and solvent second distillation is added respectively in above-mentioned silicon dioxide composite material
Water also carries out stirring pulping, after be coated uniformly on Copper Foil, through drying, roll prepared, configuration proportion:
Silicon dioxide composite material: SP: LA132: redistilled water=95g: 1g: 4g: 220mL, electrolyte is adopted
Use LiPF6/ EC+DEC, electrolyte volume ratio LiPF6/ EC: DEC=1: 1, metal lithium sheet is to electrode, every
Film uses polythene PE, polypropylene PP and the composite membrane of poly-second propylene PEP, and button cell is assemblied in and is flushed with hydrogen gas
Glove box in carry out, chemical property is carried out on the indigo plant electricity CT2001A type cell tester of Wuhan, charge and discharge
Piezoelectric voltage scope control 0.005~2.0V, charge-discharge velocity 0.1C.
Wherein, comparative example 1 to purchase the Delanium not being modified on market as negative material, other with
On.
Button cell A1, A2, A3 see table with the electrical testing comparison reference result of buckleing of comparative example 1.
Button cell | A1 | A2 | A3 | Comparative example 1 |
Negative material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Delanium |
Discharge capacity (mAh/g) first | 478.2 | 476.4 | 472.3 | 339.5 |
Efficiency (%) first | 94.9 | 947 | 93.5 | 91.4 |
As can be seen from the above table, its discharge capacity and first first of button electricity battery that embodiment 1~3 makes is used
Efficiency, apparently higher than comparative example 1, shows that the negative pole of the silicon dioxide produced with combination of the present invention has higher electric discharge
Capacity and efficiency, it is multiple that reason is that the silicon dioxide prepared through modification may be uniformly dispersed in silicon dioxide
In condensation material, carbon nanotube mesh structures has the big coefficient of expansion simultaneously, can reduce silicon dioxide instead
Expansion rate during Ying, thus improve the stability of material.
Soft-package battery is tested:
Respectively using embodiment 1-3 as negative material, with LiFePO4 as positive electrode, electrolyte uses
LiPF6/ EC+DEC, electrolyte volume ratio LiPF6/ EC: DEC=1: 1, Celgard 2400 film be barrier film,
5AH soft-package battery B1, B2, the B3 of correspondence can be prepared respectively, and test the cryogenic property of its negative material.
Comparative example 2 is to purchase the Delanium not being modified on market as negative material, with LiFePO4 is
Positive electrode, electrolyte uses LiPF6/ EC+DEC, electrolyte volume ratio LiPF6/ EC: DEC=1: 1, Celgard
2400 films are barrier film, prepare 5AH soft-package battery C.
5AH soft-package battery B1-B3 see table at the conservation rate of different cycle-indexes from battery C.
The cyclic curve comparison diagram of three embodiments and comparative example is shown in Fig. 2, from upper table 3 and Fig. 2 it can be seen that this
Bright silicon dioxide composite material relies on CNT to be network structure, has big specific surface area and high leading
Electricity rate, can increase substantially the loop structure stability of silicon dioxide composite material, and specific surface area can reach
To 2.5~4.5m2/ g, 500 circulation conservation rate >=93.60%.
Claims (1)
1. a silicon dioxide composite material preparation method for used as negative electrode of Li-ion battery, this silicon dioxide is combined
Material preparation method include [CNT/silicon dioxide] prepared by composite, prepared by silica precursor and
Silicon dioxide composite material prepares three big processes, wherein prepares at [CNT/silicon dioxide] composite
During use and receive to ethanol, distilled water, ammonia, cetyl trimethylammonium bromide, acid-treated carbon
Mitron, tetraethyl orthosilicate, deionized water and dehydrated alcohol, it is desirable to acid-treated carbon nano tube structure formula is
-COOH ,-OH and percent grafting controls 0.5~5%, it is characterized in that:
I, the preparation of [CNT/silicon dioxide] composite:
By the mL i.e. ethanol of ratio: distilled water: ammonia: cetyl trimethylammonium bromide CTAB=[100~150]:
[20~50]: [1~2]: [0.1~0.2] is sequentially added into ethanol, distilled water, ammonia and ten in reaction utensil
Six alkyl trimethyl ammonium bromides also stir and make it fully dissolve, then add 0.1~0.2g in reaction utensil
Through acid-treated CNT ultrasonic disperse 40min, treat that acid-treated CNT is completely dispersed backward
Reaction utensil is slowly added dropwise 1.0g tetraethyl orthosilicate and is stirred at room temperature 4~12h, afterwards by reaction utensil
Product successively with deionized water, dehydrated alcohol respectively be centrifuged clean, finally carry out at 80 DEG C
It is dried, [CNT/silicon dioxide] composite can be prepared;
II, the preparation of silica precursor:
[CNT/silicon dioxide] composite prepared in above-mentioned I is put in reactor and added
Colophonium, [CNT/silicon dioxide] composite: Colophonium=100g: [30~60] g, turning of reactor
Speed controls 300~1000r/min, and the fusion temperature of reactor controls at 20~100 DEG C, melting of reactor
The conjunction time controls, 200~400min, to prepare silica precursor afterwards;
III, the preparation of silicon dioxide composite material:
The silica precursor prepared in above-mentioned II is placed in the high temperature furnace of 2500~3000 DEG C and carries out stone
Inkization processes, and comes out of the stove and naturally cools to room temperature, can prepare after the complete graphitization of silica precursor
Go out silicon dioxide composite material.
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CN109980164A (en) * | 2019-03-18 | 2019-07-05 | 宁德新能源科技有限公司 | Isolation film and electrochemical appliance |
CN111129440A (en) * | 2018-10-30 | 2020-05-08 | 天津大学 | Silicon dioxide-carbon composite material, preparation method thereof and application thereof in lithium ion battery cathode material |
CN115064664A (en) * | 2021-12-24 | 2022-09-16 | 温州大学 | Confined silicon dioxide/multi-walled carbon nanotube composite material and preparation method and application thereof |
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CN108134052A (en) * | 2016-12-01 | 2018-06-08 | 内蒙古欣源石墨烯科技有限公司 | High-volume silicon-carbon negative electrode material and preparation method thereof used in a kind of power battery |
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CN111129440A (en) * | 2018-10-30 | 2020-05-08 | 天津大学 | Silicon dioxide-carbon composite material, preparation method thereof and application thereof in lithium ion battery cathode material |
CN109980164A (en) * | 2019-03-18 | 2019-07-05 | 宁德新能源科技有限公司 | Isolation film and electrochemical appliance |
CN115064664A (en) * | 2021-12-24 | 2022-09-16 | 温州大学 | Confined silicon dioxide/multi-walled carbon nanotube composite material and preparation method and application thereof |
WO2023116943A1 (en) * | 2021-12-24 | 2023-06-29 | 温州大学 | Confinement silicon dioxide/multi-walled carbon nanotube composite material, and preparation method and use therefor |
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