CN109888209A - It is a kind of using aluminium oxide as carbon coating nano-tube of template and preparation method thereof - Google Patents
It is a kind of using aluminium oxide as carbon coating nano-tube of template and preparation method thereof Download PDFInfo
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- CN109888209A CN109888209A CN201910079901.7A CN201910079901A CN109888209A CN 109888209 A CN109888209 A CN 109888209A CN 201910079901 A CN201910079901 A CN 201910079901A CN 109888209 A CN109888209 A CN 109888209A
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Abstract
The present invention discloses a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, include following steps: (1) reducing agent is added after being sufficiently mixed silicon precursor and organic solvent, flow back 7-13h at 400 DEG C, then n-butyllithium solution is added and stirs 6-12h, solvent is evaporated off in 120 DEG C of backspins, it is eventually adding diluent, solution viscosity is reduced, obtains butyl silicon solution；(2) under room temperature, multiaperture pellumina is immersed in by 2-8min in butyl silicon solution using solution dipping method, is then dried in vacuo 2-6h at 200 DEG C, repeated impregnations and drying process 3-5 times obtain butyl silicon/alumina composite nanotube；(3) composite nano tube is made annealing treatment, then uses 3mol L-1 sodium hydroxide solution etching away aluminium oxide, and elute 2-5 times, be finally dried in vacuo 8-12h at 120 DEG C and obtain carbon-coated nano-tube.It applies it in lithium ion battery to improve battery head effect, capacity and cycle performance.
Description
Technical field
The present invention relates to Silicon Based Anode Materials for Lithium-Ion Batteries technical fields, refer in particular to a kind of using aluminium oxide as template
Carbon coating nano-tube and preparation method thereof.
Background technique
Lithium ion battery from early 1990s research and develop and success since, with its superior performance (such as operating voltage is high,
Specific energy height, good cycle, long service life, operating temperature range be wide, memory-less effect, self discharge are small, pollution-free etc. excellent
Point) have become the best battery system of current comprehensive performance.But with portable electronic product miniaturization and lithium ion
Demand of the battery in aviation, military affairs and automobile industry is increasingly vigorous, and the capacity and energy density of battery urgently increase substantially.
Currently, commercial lithium-ion batteries are mainly negative as it using the modified natural graphite and artificial graphite with excellent cycling performance
Pole material, but because of its theoretical specific capacity (LiC6Vs.372mAh/g) lower, therefore people are for Novel high-specific capacity flexible, long circulating
Service life negative electrode material is placed high hopes.
In lithium ion battery negative material, silicon is one of most promising high-performance lithium ion negative electrode material.Because it has
Highest theoretical specific capacity (4200mAh/g) and lower removal lithium embedded voltage (< 0.5V), and highly-safe, abundance, valence
Lattice are cheap.However silicon in charge and discharge process there are serious bulk effect, lead to dusting and the active material of electrode material
It falls off, to seriously affect the cyclical stability of silicon electrode material.In addition, silicon have lower electronic conductivity and with routine
The compatibility of electrolyte is poor, all limits the practical application of silicon materials.
Nano-tube with hollow structure is very promising negative electrode material, because axial gap provides foot to it
Expansion of enough spaces for silicon particle in charge and discharge process can prevent the rupture of silicon and the deformation of SEI film.In addition, due to
It is both exposed in electrolyte for inside and outside two layers, and tube wall is very thin, highly shortened the diffusion path of lithium ion.Nano-tube tool
There are the reversible capacity and cyclical stability higher than general nanostructure, and nano-tube possesses very high specific surface area, therefore electricity
The current density of extremely upper unit area is also higher than nano silicon particles.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide one kind with aluminium oxide is
Carbon coating nano-tube of template and preparation method thereof is applied in lithium ion battery to improve battery head effect, capacity and follow
Ring performance.
To achieve the above object, the present invention is using following technical solution:
It is a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, include following steps:
(1) reducing agent is added after being sufficiently mixed silicon precursor and organic solvent, flow back 7-13h at 400 DEG C, and normal-butyl is then added
Lithium solution stirs 6-12h, and solvent is evaporated off in 120 DEG C of backspins, is eventually adding diluent, reduces solution viscosity, it is molten to obtain butyl silicon
Liquid；
(2) under room temperature, multiaperture pellumina is immersed in by 2- in butyl silicon solution prepared by step (1) using solution dipping method
8min, is then dried in vacuo 2-6h at 200 DEG C, repeated impregnations and drying process 3-5 times, obtains butyl silicon/alumina composite
Nanotube；
(3) composite nano tube obtained by step (2) is further made annealing treatment, is then removed with 3mol L-1 sodium hydroxide solution etching
Fall aluminium oxide, and eluted 2-5 times with ethyl alcohol or deionized water, is finally dried in vacuo 8-12h at 120 DEG C and obtains carbon-coated silicon
Nanotube.
As a preferred embodiment, the silicon precursor is silicon tetrachloride, in silicon bromide, silicon tetraiodide, silicon tetrahydride
It is one or more.
As a preferred embodiment, the organic solvent be glycol dimethyl ether, ethylene glycol diethyl ether, butyl glycol ether,
One of methylene chloride, chloroform, carbon tetrachloride are a variety of.
As a preferred embodiment, the reducing agent is one of liquefied ammonia sodium, sodium naphthalene, sodium alkoxide, sodium borohydride or a variety of.
As a preferred embodiment, the stirring is magnetic agitation or electric stirring, revolving speed 1000-15000rpm.
As a preferred embodiment, the diluent is acetone, n-butanol, n-hexane, pentamethylene, cyclohexanone, toluene, two
One of toluene, styrene are a variety of.
As a preferred embodiment, the multiaperture pellumina is with a thickness of 200-300nm.
As a preferred embodiment, the annealing condition is 1100 DEG C of annealing 3-6h in vacuum.
It is a kind of using aluminium oxide as the carbon coating nano-tube of template, use aforementioned a kind of using aluminium oxide as the carbon coating of template
The preparation method of nano-tube is made.
The present invention has obvious advantages and beneficial effects compared with the existing technology, specifically, by above-mentioned technical proposal
Known to:
The present invention by multiaperture pellumina template chemical deposition finally obtain carbon-coated nano-tube, nano-tube table
The thin carbon layer of face deposition reduces silicium cathode and contacts with the direct of electrolyte, improves coulombic efficiency for the first time, and enhance negative
The stability of pole material and electrolyte contacts interface promotes stably generating for SEI film under long circulating, in addition, carbon-coating is in hydrogen-oxygen
Change during sodium etching removes alumina formwork and plays the role of that nano-tube is protected not to be corroded.The silicon that the present invention designs is received
Nanotube structures are with higher than table, increase the contact area of negative electrode material and electrolyte, allow lithium ion from nanotube
Inside and outside two sides be embedded into silicium cathode, shorten lithium ion diffusion path, provide superior high rate performance for negative electrode material,
And nano tube structure has reserved biggish space, the carbon-coating of mating surface deposition can effectively buffer the body of silicon in charge and discharge process
Product bulking effect.
Specific embodiment
Present invention discloses a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, includes following step
It is rapid:
(1) reducing agent is added after being sufficiently mixed silicon precursor and organic solvent, flow back 7-13h at 400 DEG C, and normal-butyl is then added
Lithium solution stirs 6-12h, and solvent is evaporated off in 120 DEG C of backspins, is eventually adding diluent, reduces solution viscosity, it is molten to obtain butyl silicon
Liquid.The silicon precursor is one of silicon tetrachloride, silicon bromide, silicon tetraiodide, silicon tetrahydride or a variety of, the organic solvent
For glycol dimethyl ether, ethylene glycol diethyl ether, butyl glycol ether, one of methylene chloride, chloroform, carbon tetrachloride or more
Kind, the reducing agent is one of liquefied ammonia sodium, sodium naphthalene, sodium alkoxide, sodium borohydride or a variety of, and the stirring is magnetic agitation or electricity
Dynamic stirring, revolving speed 1000-15000rpm, the diluent be acetone, n-butanol, n-hexane, pentamethylene, cyclohexanone, toluene,
One of dimethylbenzene, styrene are a variety of.
(2) under room temperature, multiaperture pellumina is immersed in by butyl silicon solution prepared by step (1) using solution dipping method
Middle 2-8min, is then dried in vacuo 2-6h at 200 DEG C, repeated impregnations and drying process 3-5 times, obtains butyl silicon/aluminium oxide
Composite nano tube.The multiaperture pellumina is with a thickness of 200-300nm.
(3) composite nano tube obtained by step (2) is further made annealing treatment, is then carved with 3mol L-1 sodium hydroxide solution
Ablation falls aluminium oxide, and is eluted 2-5 times with ethyl alcohol or deionized water, is finally dried in vacuo 8-12h at 120 DEG C and obtains carbon coating
Nano-tube.The annealing condition is 1100 DEG C of annealing 3-6h in vacuum.
It is a kind of using aluminium oxide as the carbon coating nano-tube of template, use aforementioned a kind of using aluminium oxide as the carbon coating of template
The preparation method of nano-tube is made.
With multiple embodiments, invention is further described in detail below:
Embodiment 1:
It takes 30g silicon tetrachloride (99.999%), 200g glycol dimethyl ether, 100g sodium naphthalene is added after being sufficiently mixed, 400 DEG C next time
Flow 9h, then be added 80mL n-butyllithium solution (99%), open magnetic stirring apparatus, setting revolving speed be 2000rpm, time 8h,
Then excess of solvent is evaporated off in 120 DEG C of backspins and obtains Pale yellow viscous liquid butyl silicon solution, appropriate n-hexane, which is added, to be reduced
Solution viscosity.Under room temperature, multiaperture pellumina is immersed in 2min in butyl silicon solution, is then dried in vacuo 2h at 200 DEG C,
Repeated impregnations and drying process 3 times, obtain butyl silicon/alumina composite nanotube, and gained composite nano tube is put into annealing furnace
In, then the lower 1100 DEG C of annealings 3h of vacuum uses 3molL-1Sodium hydroxide solution etching processing 3h remove pellumina
And it is dried in vacuum overnight at washing 3 times, last 120 DEG C and obtains carbon-coated nano-tube.
Active material carbon coating nano-tube, carbon black, Kynoar (PVDF) are mixed for 75:12:13 in mass ratio,
Appropriate N-Methyl pyrrolidone (NMP) solution is added dropwise, agitation and dilution is homogeneous paste, is coated on copper sheet, and coating layer thickness is 30 μ
M forms negative electrode tab.Pole piece is placed in 130 DEG C of vacuum oven drying, with the pressure of 10MPa carries out tabletting on tablet press machine,
Pole piece is put into 120 DEG C of vacuum ovens dry 12h again.Pole piece after drying is transferred in glove box, is made with metal lithium sheet
To be assembled into 2016 type button cells in the glove box full of dry argon gas to electrode.Diaphragm is porous polypropylene film, electrolysis
Liquid is 1molL-1LiPF6/ (EC+DMC) solution.Through electro-chemical test under 0.2C multiplying power, first charge-discharge capacity difference
For 3279mAh/g and 3673mAh/g, coulombic efficiency reaches 89.3%, and under 1C multiplying power, capacity retention ratio is after 200 circulations
87%。
Embodiment 2:
It takes 50g silicon tetrachloride (99.999%) to be dissolved in 200mL carbon tetrachloride solution, 130mL liquefied ammonia sodium solution is added, at 400 DEG C
Flow back 7h, and 140mL n-butyllithium solution (99%) then is added, and opens electric stirring, and revolving speed is set as 1700rpm, after stirring 12h
Excess of solvent is evaporated off in 120 DEG C of backspins, and 30mL acetone reduction solution viscosity is added.Under room temperature, multiaperture pellumina is immersed
The 4min into the butyl silicon solution of above-mentioned preparation, is then dried in vacuo 3h at 200 DEG C, repeated impregnations and drying process 4 times, obtains
To butyl silicon/alumina composite nanotube, the further lower 1100 DEG C of annealings 3h of vacuum in the lehr by composite material, so
After use 3molL-1Sodium hydroxide solution etching processing 3h remove pellumina template and with ethanol elution 2 times, last 120 DEG C
Under be dried in vacuum overnight and obtain carbon-coated nano-tube.
Electrode preparation method, battery assembly and test condition are identical as previous embodiment 1.It is obtained by electro-chemical test
Under 0.2C multiplying power, first charge-discharge capacity is respectively 3089mAh/g and 3572mAh/g, and coulombic efficiency reaches 86.5%, in 3C and
Under 5C multiplying power, initial capacity is at 2500mAh/g or more, 1C multiplying power, and capacity retention ratio still has after 150 circulations
84.7%。
Embodiment 3:
It takes 130g silicon bromide (99.8%), 170mL ethylene glycol diethyl ether, 80g sodium alkoxide is added after mixing, flows back at 400 DEG C
Then 110mL n-butyllithium solution (99%) is added in 9h, open magnetic agitation, and revolving speed is set as 2000rpm, stirs after 6h 120
DEG C backspin, which is evaporated off excess of solvent and 45mL pentamethylene is added, reduces solution viscosity.Under room temperature, multiaperture pellumina is immersed in
2min in the butyl silicon solution of above-mentioned preparation, is then dried in vacuo 5h at 200 DEG C, repeated impregnations and drying process 3 times, obtains
Composite nano tube is put into annealing furnace by butyl silicon/alumina composite nanotube, then 1100 DEG C of annealing 3h in vacuum are used
3mol·L-1Sodium hydroxide solution etching processing 3h remove pellumina template and at ethanol elution 3 times, last 120 DEG C very
Sky, which is dried overnight, obtains carbon-coated nano-tube.
Electrode preparation method, battery assembly and test condition are identical as previous embodiment 1.It is obtained by electro-chemical test
Under 0.2C multiplying power, first charge-discharge capacity is respectively 2875mAh/g and 3417mAh/g, and coulombic efficiency reaches 84.1%, 1C multiplying power
Under, capacity retention ratio is 78.6% after 200 circulations.
Design focal point of the invention is: the present invention by multiaperture pellumina template chemical deposition finally obtain carbon
The nano-tube of cladding, the thin carbon layer of nano-tube surface deposition reduce silicium cathode and contact with the direct of electrolyte, improve
Coulombic efficiency for the first time, and the stability of negative electrode material Yu electrolyte contacts interface is enhanced, promote SEI film under long circulating
It stably generates, protects nano-tube not rotten in addition, carbon-coating plays during sodium hydroxide etches and removes alumina formwork
The effect of erosion.The nano-tube structure that the present invention designs is with higher than table, increases contact of the negative electrode material with electrolyte
Area is embedded into lithium ion in silicium cathode from the inside and outside two sides of nanotube, shortens lithium ion diffusion path, is cathode
Material provides superior high rate performance, and nano tube structure has reserved biggish space, and the carbon-coating of mating surface deposition can
The Volumetric expansion of silicon effectively in buffering charge and discharge process.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore any subtle modifications, equivalent variations and modifications to the above embodiments according to the technical essence of the invention, still
Belong in the range of technical solution of the present invention.
Claims (9)
1. a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, it is characterised in that: include following steps:
(1) reducing agent is added after being sufficiently mixed silicon precursor and organic solvent, flow back 7-13h at 400 DEG C, and normal-butyl is then added
Lithium solution stirs 6-12h, and solvent is evaporated off in 120 DEG C of backspins, is eventually adding diluent, reduces solution viscosity, it is molten to obtain butyl silicon
Liquid；
(2) under room temperature, multiaperture pellumina is immersed in by 2- in butyl silicon solution prepared by step (1) using solution dipping method
8min, is then dried in vacuo 2-6h at 200 DEG C, repeated impregnations and drying process 3-5 times, obtains butyl silicon/alumina composite
Nanotube；
(3) composite nano tube obtained by step (2) is further made annealing treatment, is then removed with 3mol L-1 sodium hydroxide solution etching
Fall aluminium oxide, and eluted 2-5 times with ethyl alcohol or deionized water, is finally dried in vacuo 8-12h at 120 DEG C and obtains carbon-coated silicon
Nanotube.
2. according to claim 1 a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, feature
Be: the silicon precursor is one of silicon tetrachloride, silicon bromide, silicon tetraiodide, silicon tetrahydride or a variety of.
3. according to claim 1 a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, feature
Be: the organic solvent is glycol dimethyl ether, ethylene glycol diethyl ether, butyl glycol ether, methylene chloride, chloroform, four
One of chlorination carbon is a variety of.
4. according to claim 1 a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, feature
Be: the reducing agent is one of liquefied ammonia sodium, sodium naphthalene, sodium alkoxide, sodium borohydride or a variety of.
5. according to claim 1 a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, feature
Be: the stirring is magnetic agitation or electric stirring, revolving speed 1000-15000rpm.
6. according to claim 1 a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, feature
Be: the diluent is one of acetone, n-butanol, n-hexane, pentamethylene, cyclohexanone, toluene, dimethylbenzene, styrene
Or it is a variety of.
7. according to claim 1 a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, feature
Be: the multiaperture pellumina is with a thickness of 200-300nm.
8. according to claim 1 a kind of using aluminium oxide as the preparation method of the carbon coating nano-tube of template, feature
Be: the annealing condition is 1100 DEG C of annealing 3-6h in vacuum.
9. a kind of using aluminium oxide as the carbon coating nano-tube of template, it is characterised in that: using such as any one of claim 1-8 institute
That states is a kind of obtained by the preparation method of the carbon coating nano-tube of template of aluminium oxide.
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Cited By (1)
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