CN107579229A - A kind of super flexible silicon aeration cell fiber and preparation method thereof - Google Patents
A kind of super flexible silicon aeration cell fiber and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to field of new energy technologies, specially a kind of super flexible silicon aeration cell fiber and preparation method thereof.The super flexible silicon aeration cell fiber is made up of lithiumation silicon/carbon nano tube composite fibre, high-molecular gel electrolyte, CNT air electrode and heat-shrink tube protective layer with holes in the form of coaxial configuration.The super flexible silicon aeration cell fiber, aerial discharge energy density can reach 512 Wh/kg, and can under 20000 bend cycles steady operation；With super flexibility, stable chemical property can be all kept under different degrees of deformation；Simultaneously as its fibrous profile, can individually be woven into fabric, can also be had broad application prospects with textile mixed weaving into fabric in wearable electronic field.
Description
Technical field
The invention belongs to field of new energy technologies, and in particular to a kind of super flexible silicon aeration cell fiber and its preparation side
Method.
Background technology
Portable wearable electronic equipment has become a kind of epoch trend, has attracted increasing concern, its
In, the flexible highly important role of energy supply device performer.[1-2] in terms of corresponding battery is developed although paid
Many effort, still suffers from the problem of some are common.Existing battery generally use sandwich layer structure as thin as possible.
[3-6] flexible realization often to sacrifice chemical property as cost, such as, it is desirable to too many active material can not be loaded, this
Its energy density of sample is generally very low.[7] in addition, under deformation, the sliding between two membrane electrodes may result in short circuit.[8]
In addition, they can bear some slight deformation, such as bend, but in some larger deformation, such as distortion and knotting
Under, its structure may be destroyed.Two fiber electrode distortions are formed one kind completely newly by [9-10] together therefore, someone uses
Film lithium ion battery structure, show higher flexibility.[11-13] but, on the one hand, the structural energy of this distortion is close
Degree is very low；[13] on the other hand, two fiber electrodes may possibly be separated under larger or repetition deformation, so as to cause electrochemistry
Energy declines to a great extent with stability.[12] development has that the battery of high-energy-density and high flexibility is very urgent simultaneously, and has
Very big challenge.
The content of the invention
It is an object of the invention to provide a kind of preparation method of super flexible silicon aeration cell fiber, effectively to overcome at present
The problem of flexible battery is present.
Super flexible silicon aeration cell fiber provided by the present invention, by lithiumation silicon/carbon nano tube composite fibre, Macromolecule
Glue electrolyte, CNT air electrode and heat-shrink tube protective layer with holes are formed in the form of coaxial configuration.
The preparation method of super flexible silicon aeration cell fiber provided by the present invention, is comprised the following steps that：
（1）Lithiumation silicon/carbon nano tube composite fibre is prepared, as negative pole；
（2）Lithiumation silicon/carbon nano tube composite fibre is totally immersed into gel electrolyte precursor solution, then taken out；
（3）Lithiumation silicon/carbon nano tube composite fibre 5-20s with ultraviolet light impregnated of gel electrolyte precursor solution,
Solidify gel electrolyte presoma；
（4）Wind CNT air electrode：It is the wide carbon nano-tube films of 0.8-1.5cm with 45-70 ° of helical angle by width
It is wrapped in through step（3）On the gel electrolyte of processing, control lithiumation silicon/carbon nano tube composite fibre negative pole and CNT are just
The mass ratio of pole is 1.1-1.5:1；
（5）One layer of heat-shrink tube with holes is covered as protective layer.
In the present invention, the specific preparation process of described lithiumation silicon/carbon nano tube composite fibre negative pole is as follows：（1）By can
Spinning carbon nano pipe array, which continuously pulls, prepares orientation carbon nanotube film；（2）Silica flour was dried in vacuum drying oven at 70-90 DEG C
At night, 15-25mg silica flour is dispersed in DMF in 15-20mL, is sufficiently stirred to obtain dispersion liquid；（3）It will divide
Dispersion liquid is uniformly dropped on two layers wide of carbon nano-tube film of 1-3cm, is rolled into silicon/carbon nano tube composite fibre；（4）In gloves
Composite fibre and lithium piece are assembled into 2025 button cells in case, 1M double trifluoromethanesulfonimide lithiums are dissolved in fluoro ethylene
Alkene ester and tetraethyleneglycol dimethyl ether（Volume ratio 3-3.5:1, this volume ratio refers to fluorinated ethylene carbonate and tetraethyleneglycol dimethyl ether
Volume ratio）In, as electrolyte.After assembling, the charge and discharge cycles under voltage range 0.01-3V, electric current 0.05-0.15mA
One week.Finally, the battery discharges into 0.05V under 0.05-0.15mA, then discharges into 0.01V under 0.02-0.06mA.In hand
Tetraethyleneglycol dimethyl ether rinse is used after being dismantled in casing, obtains lithiumation silicon/carbon nano-tube fibre negative pole.
In the present invention, the specific preparation process of described gel electrolyte presoma is as follows：（1）Double the three of 0.05-0.2M
Fluoromethane sulfimide lithium and 0.2-1.0M lithium nitrate are dissolved in 0.5-3mL tetraethyleneglycol dimethyl ether and obtain solution A；（2）
0.3-1.2g, which gathers inclined fluorine vinyl chloride-hexafluoropropene and is dissolved in 2-5gN- methyl pyrrolidones, obtains solution B；（3）0.01-0.1g2- hydroxyls
Base -2- methyl isophthalic acids-phenyl -1- acetone is added in 1-5g ethoxylated trimethylolpropane triacrylates and obtains solution C；
（4）By solution A, B and C are with mass ratio 3.5-5:4.5-6:3 mixing, are sufficiently stirred to obtain gel electrolyte presoma.
In the present invention, the orientation carbon nanotube film is obtained from that can spin pull-out in aligned carbon nanotube array.It can spin
Aligned carbon nanotube array is prepared by chemical vapour deposition technique, and its specific preparation method is：Pass through electron beam evaporation plating
It is Al that film instrument deposits a Rotating fields on silicon chip2O3/ Fe catalyst, wherein Al2O3Thickness be 2-20 nm, Fe thickness be
0.5-1.5 nm.By chemical vapour deposition technique, by the use of argon gas as carrier gas, ethene is as carbon source, and hydrogen is as reducing agent, pre-
First it is coated with the silicon chip of catalyst and synthesizes height-oriented carbon nano pipe array.Wherein argon gas flow is 350-450
Sccm, ethylene gas flow are 60-120 sccm, and hydrogen gas flow is 30-90 sccm.Reaction temperature is 700-800
DEG C, the reaction time is 10-15 min.
Super flexible silicon aeration cell fiber prepared by the present invention, directly can work in atmosphere, have the energy of superelevation
Density, preferable cyclical stability and good flexibility（Aerial discharge energy density can reach 512 Wh/kg,
And can under 20000 bend cycles steady operation）；It has it is super flexible, can all be kept under different degrees of deformation
Stable chemical property；Simultaneously as its fibrous profile, can individually be woven into fabric, can also be mixed with textile
Woven into fabric is compiled in collaboration with, is had broad application prospects in wearable electronic field.
Brief description of the drawings
Fig. 1 is the super flexible silicon aeration cell fibre structure diagram of the present invention.
Fig. 2 is the super aerial cycle charge-discharge curve of flexible silicon aeration cell fiber in embodiment.
Fig. 3 is the super aerial cycle performance curve of flexible silicon aeration cell fiber in embodiment.
Fig. 4 is influence of the differently curved period to super flexible silicon aeration cell fibre property in embodiment.
Fig. 5 is charging and discharging curve of the super flexible silicon aeration cell fiber under different deformation pattern in embodiment.
Fig. 6 is super flexible silicon aeration cell fiber in embodiment and fabric Co-knit and lights the photo of LED screen.
Embodiment
Below in conjunction with specific implementation case, exemplary explanation and help further understand the present invention, but case study on implementation has
Body details does not represent technical scheme whole under present inventive concept, therefore should not be construed as pair merely to the explanation present invention
The restriction of the total technical scheme of the present invention, some in technical staff, unsubstantiality increase without departing from present inventive concept and
Change, such as simply change or replace with the technical characteristic with same or similar technique effect, belong to present invention protection model
Enclose.
Embodiment 1：Prepare orientation carbon nanotube film.One Rotating fields are deposited on silicon chip by electron beam evaporation deposition instrument
For Al2O3/ Fe catalyst, wherein Al2O3Thickness be 3 nm, Fe thickness is 1.2 nm.By chemical vapour deposition technique,
By the use of argon gas as carrier gas, ethene is as carbon source, and hydrogen is as reducing agent, and synthesis height takes on the silicon chip of catalyst is coated with advance
To carbon nano pipe array.Wherein argon gas flow is 400 sccm, and ethylene gas flow is 90 sccm, hydrogen gas
Flow is 60 sccm.Reaction temperature is 740 DEG C, and the reaction time is 10 min.Directly from can spin in aligned carbon nanotube array
Pull-out obtains orientation carbon nanotube film.
Prepare lithiumation silicon/carbon nano tube composite fibre negative pole.Preparation orientation carbon is continuously pulled by carbon nano pipe array can be spun
Nano-tube film；Silica flour is dried overnight in vacuum drying oven at 70 DEG C, and 15mg silica flour is dispersed in into 15mLN, N- dimethyl methyls
In acid amides, it is sufficiently stirred to obtain dispersion liquid；Homogeneous dispersion is dropped on two layers wide of carbon nano-tube film of 1cm, is rolled into
Silicon/carbon nano tube composite fibre；Composite fibre and lithium piece are assembled into 2025 button cells, 1M double fluoroforms in glove box
Alkane sulfimide lithium is dissolved in fluorinated ethylene carbonate and tetraethyleneglycol dimethyl ether（Volume ratio is 3.0:1）In, as electrolyte.Group
After installing, in voltage range 0.01-3V, electric current is charge and discharge cycles one week under 0.05mA.Finally, the battery is transferred in 0.05mA
Electricity arrives 0.05V, then discharges into 0.01V under 0.02mA.Tetraethyleneglycol dimethyl ether rinse is used after being dismantled in glove box, obtains lithium
SiClx/carbon nano-tube fibre negative pole.
Prepare gel electrolyte.The lithium nitrate of 0.05M double trifluoromethanesulfonimide lithiums and 0.2M is dissolved in 0.5mL's
Solution A is obtained in tetraethyleneglycol dimethyl ether；0.3g is gathered into inclined fluorine vinyl chloride-hexafluoropropene to be dissolved in 2gN- methyl pyrrolidones and obtain
Solution B；0.01g2- hydroxy-2-methyl -1- phenyl -1- acetone is added to the acrylic acid of 1g ethoxylated trimethylolpropanes three
Solution C is obtained in ester；By solution A, solution B and solution C are with mass ratio 3.5:4.5:3 ratio mixing, is sufficiently stirred and is coagulated
Glue electrolyte presoma, is kept in dark place.
Assemble silicon aeration cell fiber.Lithiumation silicon/carbon nano tube composite fibre is totally immersed into gel electrolyte presoma
Taken out after in solution；Ultraviolet lighting 5s, solidify gel electrolyte presoma；The wide CNTs of 0.8cm are wound with 45 ° of helical angles
Film is as air electrode；One layer of heat-shrink tube with holes is covered as protective layer.
Embodiment 2：Prepare orientation carbon nanotube film.One Rotating fields are deposited on silicon chip by electron beam evaporation deposition instrument
For Al2O3/ Fe catalyst, wherein Al2O3Thickness be 3 nm, Fe thickness is 1.2 nm.By chemical vapour deposition technique,
By the use of argon gas as carrier gas, ethene is as carbon source, and hydrogen is as reducing agent, and synthesis height takes on the silicon chip of catalyst is coated with advance
To carbon nano pipe array.Wherein argon gas flow is 400 sccm, and ethylene gas flow is 90 sccm, hydrogen gas
Flow is 60 sccm.Reaction temperature is 740 DEG C, and the reaction time is 10 min.Directly from can spin in aligned carbon nanotube array
Pull-out obtains orientation carbon nanotube film.
Prepare lithiumation silicon/carbon nano tube composite fibre negative pole.Preparation orientation carbon is continuously pulled by carbon nano pipe array can be spun
Nano-tube film；Silica flour is dried overnight in vacuum drying oven at 80 DEG C, and 20mg silica flour is dispersed in into 17mLN, N- dimethyl methyls
In acid amides, it is sufficiently stirred to obtain dispersion liquid；Homogeneous dispersion is dropped on two layers wide of carbon nano-tube film of 2cm, is rolled into
Silicon/carbon nano tube composite fibre；Composite fibre and lithium piece are assembled into 2025 button cells, 1M double fluoroforms in glove box
Alkane sulfimide lithium is dissolved in fluorinated ethylene carbonate and tetraethyleneglycol dimethyl ether（Volume ratio is 3.2:1）In, as electrolyte.Group
After installing, in voltage range 0.01-3V, electric current is charge and discharge cycles one week under 0.10mA.Finally, the battery is transferred in 0.10mA
Electricity arrives 0.05V, then discharges into 0.01V under 0.04mA.Tetraethyleneglycol dimethyl ether rinse is used after being dismantled in glove box, obtains lithium
SiClx/carbon nano-tube fibre negative pole.
Prepare gel electrolyte.The lithium nitrate of 0.15M double trifluoromethanesulfonimide lithiums and 0.5M is dissolved in the four of 2mL
Solution A is obtained in glycol dimethyl ether；By 0.7g gather inclined fluorine vinyl chloride-hexafluoropropene be dissolved in 4gN- methyl pyrrolidones obtain it is molten
Liquid B；0.05g2- hydroxy-2-methyl -1- phenyl -1- acetone is added to 3g ethoxylated trimethylolpropane triacrylates
In obtain solution C；By solution A, solution B and solution C are with mass ratio 4:5:3 ratio mixing, is sufficiently stirred to obtain gel electrolyte
Liquid presoma, is kept in dark place.
Assemble silicon aeration cell fiber.Lithiumation silicon/carbon nano tube composite fibre is totally immersed into gel electrolyte presoma
Taken out after in solution；Ultraviolet light 10s, solidify gel electrolyte presoma；It is thin that the wide CNTs of 1cm are wound with 60 ° of helical angles
Film is as air electrode；One layer of heat-shrink tube with holes is covered as protective layer.
Embodiment 3：Prepare orientation carbon nanotube film.One Rotating fields are deposited on silicon chip by electron beam evaporation deposition instrument
For Al2O3/ Fe catalyst, wherein Al2O3Thickness be 3 nm, Fe thickness is 1.2 nm.By chemical vapour deposition technique,
By the use of argon gas as carrier gas, ethene is as carbon source, and hydrogen is as reducing agent, and synthesis height takes on the silicon chip of catalyst is coated with advance
To carbon nano pipe array.Wherein argon gas flow is 400 sccm, and ethylene gas flow is 90 sccm, hydrogen gas
Flow is 60 sccm.Reaction temperature is 740 DEG C, and the reaction time is 10 min.Directly from can spin in aligned carbon nanotube array
Pull-out obtains orientation carbon nanotube film.
Prepare lithiumation silicon/carbon nano tube composite fibre negative pole.Preparation orientation carbon is continuously pulled by carbon nano pipe array can be spun
Nano-tube film；Silica flour is dried overnight in vacuum drying oven at 90 DEG C, and 25mg silica flour is dispersed in into 20mLN, N- dimethyl methyls
In acid amides, it is sufficiently stirred to obtain dispersion liquid；Homogeneous dispersion is dropped on two layers wide of carbon nano-tube film of 3cm, is rolled into
Silicon/carbon nano tube composite fibre；Composite fibre and lithium piece are assembled into 2025 button cells, 1M double fluoroforms in glove box
Alkane sulfimide lithium is dissolved in fluorinated ethylene carbonate and tetraethyleneglycol dimethyl ether（Volume ratio is 3.5:1）In, as electrolyte.Group
After installing, in voltage range 0.01-3V, electric current is charge and discharge cycles one week under 0.15mA.Finally, the battery is transferred in 0.15mA
Electricity arrives 0.05V, then discharges into 0.01V under 0.06mA.Tetraethyleneglycol dimethyl ether rinse is used after being dismantled in glove box, obtains lithium
SiClx/carbon nano-tube fibre negative pole.
Prepare gel electrolyte.The lithium nitrate of 0.20M double trifluoromethanesulfonimide lithiums and 1.0M is dissolved in the four of 3mL
Solution A is obtained in glycol dimethyl ether；By 1.2g gather inclined fluorine vinyl chloride-hexafluoropropene be dissolved in 5gN- methyl pyrrolidones obtain it is molten
Liquid B；0.1g2- hydroxy-2-methyl -1- phenyl -1- acetone is added in 5g ethoxylated trimethylolpropane triacrylates
Obtain solution C；By solution A, solution B and solution C are with mass ratio 5:6:3 ratio mixing, is sufficiently stirred to obtain gel electrolyte
Presoma, it is kept in dark place.
Assemble silicon aeration cell fiber.Lithiumation silicon/carbon nano tube composite fibre is totally immersed into gel electrolyte presoma
Taken out after in solution；Ultraviolet lighting 20s, solidify gel electrolyte presoma；The wide carbon nanometers of 1.5cm are wound with 75 ° of helical angles
Pipe film is as air electrode；One layer of heat-shrink tube with holes is covered as protective layer.
Prepared super flexible silicon aeration cell fiber（Fig. 1）Energy density with superelevation, in atmosphere its discharge energy
Metric density can reach 512Wh/kg, can stablize charge and discharge cycles up to 100 times（Fig. 2, Fig. 3）.It has the flexibility of superelevation,
Under different degrees of bending, stable chemical property can be maintained, can be in 20000 bend cycles and various strain modes
Lower steady operation（Fig. 4, Fig. 5）.And due to threadiness configuration, its can be very good with textile mixed weaving into fabric simultaneously
Energized for device（Fig. 6）, had broad application prospects in wearable electronic field.
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Claims (4)
1. a kind of preparation method of super flexible silicon aeration cell fiber, it is characterised in that comprise the following steps that：
（1）Lithiumation silicon/carbon nano tube composite fibre is prepared, as negative pole；
（2）Lithiumation silicon/carbon nano tube composite fibre is totally immersed into gel electrolyte precursor solution, then taken out；
（3）Lithiumation silicon/carbon nano tube composite fibre 5-20s with ultraviolet light impregnated of gel electrolyte precursor solution,
Solidify gel electrolyte presoma；
（4）Wind CNT air electrode：It is the wide carbon nano-tube films of 0.8-1.5cm with 45-70 ° of helical angle by width
It is wrapped in through step（3）On the gel electrolyte of processing, control lithiumation silicon/carbon nano tube composite fibre negative pole and CNT are just
The mass ratio of pole is 1.1-1.5:1；
（5）One layer of heat-shrink tube with holes is covered as protective layer.
2. the preparation method of super flexible silicon aeration cell fiber as claimed in claim 1, it is characterised in that the lithiumation silicon/
The preparation process of carbon nano tube composite fibre negative pole is as follows：
（1）Continuously pulled by carbon nano pipe array can be spun and prepare orientation carbon nanotube film；
（2）Silica flour is dried overnight in vacuum drying oven at 70-90 DEG C, and 15-25mg silica flour is dispersed in into 15-20mLN, N- diformazans
In base formamide, it is sufficiently stirred to obtain dispersion liquid；
（3）Homogeneous dispersion is dropped on two layers wide of carbon nano-tube film of 1-3cm, is rolled into the compound fibre of silicon/CNT
Dimension；
（4）Composite fibre and lithium piece are assembled into 2025 button cells, 1M double trifluoromethanesulfonimide lithiums in glove box
It is dissolved in fluorinated ethylene carbonate and tetraethyleneglycol dimethyl ether, as electrolyte, wherein, fluorinated ethylene carbonate and tetraethylene glycol
The volume ratio of dimethyl ether is 3-3.5:1；After assembling, under voltage range 0.01-3V, electric current 0.05-0.15mA discharge and recharge follow
Ring one week；Finally, the battery discharges into 0.05V under 0.05-0.15mA, then discharges into 0.01V under 0.02-0.06mA；
Tetraethyleneglycol dimethyl ether rinse is used after being dismantled in glove box, obtains lithiumation silicon/carbon nano-tube fibre negative pole.
3. the preparation method of super flexible silicon aeration cell fiber as claimed in claim 1, it is characterised in that the gel electrolyte
The specific preparation process of liquid presoma is as follows：
（1）The lithium nitrate of 0.05-0.2M double trifluoromethanesulfonimide lithiums and 0.2-1.0M is dissolved in 0.5-3mL tetrem two
In diethylene glycol dimethyl ether, solution A is obtained；
（2）0.3-1.2g is gathered into inclined fluorine vinyl chloride-hexafluoropropene to be dissolved in 2-5gN- methyl pyrrolidones, obtains solution B；
（3）0.01-0.1g2- hydroxy-2-methyl -1- phenyl -1- acetone is added to 1-5g ethoxylated trimethylolpropanes three
In acrylate, solution C is obtained；
（4）By solution A, solution B and solution C with mass ratio 3.5-5:4.5-6:3 mixing, are sufficiently stirred, obtain gel electrolyte
Presoma.
4. the super flexible silicon aeration cell fiber being prepared as the preparation method described in one of claim 1-3, by lithiumation silicon/
Carbon nano tube composite fibre, high-molecular gel electrolyte, CNT air electrode and heat-shrink tube protective layer with holes are with coaxial
Structure type forms.
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| CN107579229B (en) | 2020-03-20 |
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