CN107352544A - A kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube - Google Patents
A kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube Download PDFInfo
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- CN107352544A CN107352544A CN201710684828.7A CN201710684828A CN107352544A CN 107352544 A CN107352544 A CN 107352544A CN 201710684828 A CN201710684828 A CN 201710684828A CN 107352544 A CN107352544 A CN 107352544A
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- C—CHEMISTRY; METALLURGY
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- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/00—Particle morphology
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Abstract
The invention discloses a kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube, first by silicon source, template, dispersant, catalyst, solvent at a temperature of 20 35 DEG C magnetic agitation 12 24 hours, centrifugation, dry, obtain mesoporous silicon dioxide nano rod；Then it is mesoporous silicon dioxide nano rod is scattered in a solvent, surfactant of the addition with surface protection effect and etching action, it is heated to 90 150 DEG C; magnetic agitation 2 12 hours, 28 hours are stood, centrifugation; cleaning, is dried under vacuum to constant weight, obtains Silica Nanotube；Silica Nanotube in tube furnace is finally calcined into 2 4h under the protection of 640 670 DEG C of argon gas with reducing agent, nano-tube is made.The present invention has the characteristics of can solve silicon and make existing Volumetric expansion during lithium ion battery negative material discharge and recharge, can effectively controlling nano-tube draw ratio and thickness.
Description
Technical field
The present invention relates to a kind of synthetic method of nano-tube, particularly one kind to receive for lithium-ion electric pool size controllable silicon
The synthetic method of mitron.
Background technology
Since synthesizing carbon nanotubes, because nanotube has specific surface area big, the features such as being cavity structure, turn into already
The study hotspot of researcher, and have many grind in biology sensor, pharmaceutical carrier, lithium ion battery negative material etc.
Study carefully and apply.Silicon is lithium ion battery negative material ideal at present.With higher theoretical specific capacity and relatively low embedding lithium
Current potential.Silicon is sp3 hydridization, is not easy to form tubular structure, and tends to form wire solid construction.Then preparing silicon nano material
Shi Rongyi forms silicon nanowires.
The method of current synthesis nano-tube mainly has template, hydro-thermal method etc., but there are problems that：Template is
Unordered accumulation of the silicon atom in template, the characteristic of nano-tube can not be embodied well when making negative material, it is impossible to very well
Solution silicon make existing Volumetric expansion during lithium ion battery negative material discharge and recharge, hydro-thermal method is more difficult to accomplish
The controllability of size is synthesized, for example draw ratio and thickness are more difficult to get effective control.
The content of the invention
It is an object of the present invention to develop a kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube.This
Invention, which has, can solve silicon and makees Volumetric expansion present in lithium ion battery negative material charge and discharge process, can be with
The characteristics of effectively controlling nano-tube draw ratio and thickness.
Technical scheme：A kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube, including such as
Lower step：
（1）Prepare mesoporous silicon dioxide nano rod：By silicon source, template, dispersant, catalyst, solvent at a temperature of 20-35 DEG C
Magnetic agitation 12-24 hours, centrifuge, dry, obtain mesoporous silicon dioxide nano rod；
（2）Mesoporous silicon dioxide nano rod is etched into pipe：Mesoporous silicon dioxide nano rod is scattered in a solvent, and addition has table
Face protective effect and the surfactant of etching action, 90-150 DEG C is heated to, magnetic agitation 2-12 hours, stands 2-8 hours,
Centrifugation, cleaning, is dried under vacuum to constant weight, obtains Silica Nanotube；
（3）Silica Nanotube is reduced into nano-tube：By Silica Nanotube reducing agent in tube furnace 640-670
The lower calcining 2-4h of DEG C argon gas protection, is made nano-tube.
The synthetic method of lithium-ion electric pool size controllable silicon nanotube is previously described for, the silicon source, template, is disperseed
Agent, catalyst, solvent in parts by mass, respectively silicon source 2-10 parts, template 0.5-2 parts, dispersant 0.1-0.3 parts, catalysis
Agent 3-10 parts, solvent 90-95 parts.
The synthetic method of lithium-ion electric pool size controllable silicon nanotube is previously described for, the silicon source is tetraethyl orthosilicate.
The synthetic method of lithium-ion electric pool size controllable silicon nanotube is previously described for, the template is cetyl three
Methyl bromide ammonium.
Be previously described for the synthetic method of lithium-ion electric pool size controllable silicon nanotube, the dispersant be polyethylene glycol-
4000 or polyoxyethylene poly-oxygen propylene aether block copolymer（That is poloxamer）.
The synthetic method of lithium-ion electric pool size controllable silicon nanotube is previously described for, the catalyst is ammoniacal liquor.
The synthetic method of lithium-ion electric pool size controllable silicon nanotube is previously described for, the solvent is pure water.
It is previously described for the synthetic method of lithium-ion electric pool size controllable silicon nanotube, the mesoporous silicon dioxide nano rod
Diameter is in 200-500nm, length in 1-4um.
It is previously described for the synthetic method of lithium-ion electric pool size controllable silicon nanotube, the step（2）In, surface-active
Agent is polyethyleneimine, and in parts by mass, wherein polyethyleneimine is 0.4-1 parts, and mesoporous silicon dioxide nano rod is 1-3 parts,
Solvent is 95-98 parts.
It is previously described for the synthetic method of lithium-ion electric pool size controllable silicon nanotube, the reducing agent is magnesium powder, dioxy
The mass ratio of SiClx nanotube and reducing agent is 5:1-3.
Beneficial effects of the present invention：
1st, the nano-tube that the present invention finally synthesizes is not that the unordered accumulation of silicon atom is formed, and is had to Volumetric expansion bright
It is aobvious to improve, efficiently solve silicon and make existing Volumetric expansion during lithium ion battery negative material discharge and recharge.
2nd, the length and diameter of the invention by controlling presoma mesoporous silicon dioxide nano rod, can reach finally to silicon
Nanotube length and the purpose of controlled diameter synthesis.
3rd, the present invention is by the polyethyleneimine with surface protection and etching action, by changing polyethyleneimine
Concentration, etching period, etch temperature can regulate and control the wall thickness of mesoporous silicon dioxide nano pipe, then by Silica Nanotube magnesium
Nano-tube is heat reduced to, is finally reached the purpose of regulation and control nano-tube wall thickness.
Experimental example：
1st, by changing reaction condition, the mesoporous silicon dioxide nano rod of preparation as shown in accompanying drawing 1, accompanying drawing 2, contrasts accompanying drawing respectively
1 and accompanying drawing 2 can be seen that the mesoporous silicon dioxide nano rod prepared has different length and diameter, then can reach final
The purpose synthesized to nano-tube length and controlled diameter.It can be seen that the silicon dioxide nano rod of preparation is with hole from accompanying drawing 3
The mesoporous silicon dioxide nano rod of road structure.
2nd, to take silicon dioxide nano rod quality be 0.2g, polyethyleneimine 0.2g, 90 DEG C of 95ml pure water, 150r/
Min rotating speed stirring 2h, the Silica Nanotube that 90 DEG C of standing 8h are obtained is as shown in Figure 4；Take silicon dioxide nano rod matter
Measure and obtained for 0.2g, polyethyleneimine 0.2g, in 90 DEG C of 95ml pure water, 150r/min rotating speed stirring 2h, 90 DEG C of standing 4h
Silica Nanotube as shown in Figure 5.From accompanying drawing 4 and accompanying drawing 5 as can be seen that by changing parameter, can effectively change
Become the wall thickness of mesoporous silicon dioxide nano pipe, be finally reached the purpose of the wall thickness of regulation and control nano-tube.
Brief description of the drawings
The scanning electron microscope (SEM) photograph for the mesoporous silicon dioxide nano rod that accompanying drawing 1 is prepared for the present invention；
The scanning electron microscope (SEM) photograph for the mesoporous silicon dioxide nano rod that accompanying drawing 2 is prepared for the present invention；
The transmission electron microscope picture for the mesoporous silicon dioxide nano rod that accompanying drawing 3 is prepared for the present invention；
Accompanying drawing 4 is the transmission electron microscope picture through mesoporous silicon dioxide nano pipe produced by the present invention；
Accompanying drawing 5 is the transmission electron microscope picture through mesoporous silicon dioxide nano pipe produced by the present invention.
Embodiment
With reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiments of the invention
Embodiment 1：A kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube, comprise the following steps：
（1）Prepare mesoporous silicon dioxide nano rod：By 6 parts of tetraethyl orthosilicate, 1.3 parts of cetyl trimethylammonium bromide, poly- second
0.2 part of glycol -4000,6 parts of ammoniacal liquor, 92.5 parts of pure water magnetic agitation 18 hours at a temperature of 28 DEG C, centrifuge, dry, obtain straight
Footpath 200-500nm, length 1-4um mesoporous silicon dioxide nano rod；
（2）Mesoporous silicon dioxide nano rod is etched into pipe：The mesoporous silicon dioxide nano rod that mass parts are 2 parts is dispersed in quality
Part is the polyethyleneimine with surface protection effect and etching action that in 96.5 parts of pure water, addition mass parts are 0.7 part,
120 DEG C are heated to, magnetic agitation 5 hours, stands 4h；Centrifugation, cleaning, is dried under vacuum to constant weight, obtains Silica Nanotube；
（3）Silica Nanotube is reduced into nano-tube：Silica Nanotube and magnesium powder are pressed 5:1 mass ratio is put into pipe
Argon gas is passed through in formula stove, 3h is calcined at 650 DEG C, obtains nano-tube.
Embodiment 2：A kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube, comprise the following steps：
（1）Prepare mesoporous silicon dioxide nano rod：By 2 parts of tetraethyl orthosilicate, 0.5 part of cetyl trimethylammonium bromide, polyoxy
0.1 part of ethene polyoxypropylene ether block copolymers, 3 parts of ammoniacal liquor, 90 parts of pure water magnetic agitation 24 hours at a temperature of 20 DEG C, from
The heart, dry, obtain diameter 200-500nm, length 1-4um mesoporous silicon dioxide nano rod；
（2）Mesoporous silicon dioxide nano rod is etched into pipe：The mesoporous silicon dioxide nano rod that mass parts are 1 part is dispersed in quality
Part is the polyethyleneimine with surface protection effect and etching action that in 95 parts of pure water, addition mass parts are 1 part, is heated
To 90 DEG C, magnetic agitation 2 hours, 2h is stood；Centrifugation, cleaning, is dried under vacuum to constant weight, obtains Silica Nanotube；
（3）Silica Nanotube is reduced into nano-tube：Magnesium powder is pressed 5:1 mass ratio, which is put into tube furnace, is passed through argon gas,
2h is calcined at 640 DEG C, obtains nano-tube.
Embodiment 3：A kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube, comprise the following steps：
（1）Prepare mesoporous silicon dioxide nano rod：By 4 parts of tetraethyl orthosilicate, 0.9 part of cetyl trimethylammonium bromide, poly- second
0.15 part of glycol -4000,5 parts of ammoniacal liquor, 91.5 parts of pure water magnetic agitation 24 hours at a temperature of 25 DEG C, centrifuge, dry, obtain
Diameter 200-500nm, length 1-4um mesoporous silicon dioxide nano rod；
（2）Mesoporous silicon dioxide nano rod is etched into pipe：The mesoporous silicon dioxide nano rod that mass parts are 1.5 parts is dispersed in matter
Measure in the pure water that part is 96 parts, the polyethyleneimine with surface protection effect and etching action that addition mass parts are 0.6 part,
110 DEG C are heated to, magnetic agitation 12 hours, stands 8h；Centrifugation, cleaning, is dried under vacuum to constant weight, obtains Silica Nanotube；
（3）Silica Nanotube is reduced into nano-tube：Silica Nanotube and magnesium powder are pressed 5:2 mass ratio is put into pipe
Argon gas is passed through in formula stove, 4h is calcined at 670 DEG C, obtains nano-tube.
Embodiment 4：A kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube, comprise the following steps：
（1）Prepare mesoporous silicon dioxide nano rod：Will be by 8 parts of tetraethyl orthosilicate, 1.7 parts of cetyl trimethylammonium bromide, poly-
0.25 part of oxygen ethene polyoxypropylene ether block copolymers, 8 parts of ammoniacal liquor, 94 parts of pure water magnetic agitation 15 hours at a temperature of 31 DEG C,
Centrifugation, dry, obtain diameter 200-500nm, length 1-4um mesoporous silicon dioxide nano rod；
（2）Mesoporous silicon dioxide nano rod is etched into pipe：The mesoporous silicon dioxide nano rod that mass parts are 2.5 parts is dispersed in matter
Measure in the pure water that part is 97 parts, the polyethyleneimine with surface protection effect and etching action that addition mass parts are 0.8 part,
135 DEG C are heated to, magnetic agitation 6 hours, stands 3h；Centrifugation, cleaning, is dried under vacuum to constant weight, obtains Silica Nanotube；
（3）Silica Nanotube is reduced into nano-tube：Silica Nanotube and magnesium powder are pressed 5:2 mass ratio is put into pipe
Argon gas is passed through in formula stove, 3h is calcined at 650 DEG C, obtains nano-tube.
Embodiment 5：A kind of synthetic method for lithium-ion electric pool size controllable silicon nanotube, comprise the following steps：
（1）Prepare mesoporous silicon dioxide nano rod：Will be by 10 parts of tetraethyl orthosilicate, 2 parts of cetyl trimethylammonium bromide, poly- second
0.3 part of glycol -4000,10 parts of ammoniacal liquor, 95 parts of pure water magnetic agitation 12 hours at a temperature of 35 DEG C, centrifuge, dry, obtain straight
Footpath 200-500nm, length 1-4um mesoporous silicon dioxide nano rod；
（2）Mesoporous silicon dioxide nano rod is etched into pipe：The mesoporous silicon dioxide nano rod that mass parts are 3 parts is dispersed in quality
Part is the polyethyleneimine with surface protection effect and etching action that in 98 parts of pure water, addition mass parts are 1 part, is heated
To 150 DEG C, magnetic agitation 2 hours, 3h is stood；Centrifugation, cleaning, is dried under vacuum to constant weight, obtains Silica Nanotube；
（3）Silica Nanotube is reduced into nano-tube：Silica Nanotube and magnesium powder are pressed 5:3 mass ratio is put into pipe
Argon gas is passed through in formula stove, 3h is calcined at 650 DEG C, obtains nano-tube.
Claims (10)
- A kind of 1. synthetic method for lithium-ion electric pool size controllable silicon nanotube, it is characterised in that：Comprise the following steps：（1）Prepare mesoporous silicon dioxide nano rod：By silicon source, template, dispersant, catalyst, solvent at a temperature of 20-35 DEG C Magnetic agitation 12-24 hours, centrifuge, dry, obtain mesoporous silicon dioxide nano rod；（2）Mesoporous silicon dioxide nano rod is etched into pipe：Mesoporous silicon dioxide nano rod is scattered in a solvent, and addition has table Face protective effect and the surfactant of etching action, 90-150 DEG C is heated to, magnetic agitation 2-12 hours, stands 2-8 hours, Centrifugation, cleaning, is dried under vacuum to constant weight, obtains Silica Nanotube；（3）Silica Nanotube is reduced into nano-tube：By Silica Nanotube reducing agent in tube furnace 640-670 The lower calcining 2-4h of DEG C argon gas protection, is made nano-tube.
- 2. the synthetic method according to claim 1 for lithium-ion electric pool size controllable silicon nanotube, it is characterised in that： The silicon source, template, dispersant, catalyst, solvent in parts by mass, respectively silicon source 2-10 parts, template 0.5-2 parts, Dispersant 0.1-0.3 parts, catalyst 3-10 parts, solvent 90-95 parts.
- 3. the synthetic method according to claim 1 or 2 for lithium-ion electric pool size controllable silicon nanotube, its feature exists In：The silicon source is tetraethyl orthosilicate.
- 4. the synthetic method according to claim 1 or 2 for lithium-ion electric pool size controllable silicon nanotube, its feature exists In：The template is cetyl trimethylammonium bromide.
- 5. the synthetic method according to claim 1 or 2 for lithium-ion electric pool size controllable silicon nanotube, its feature exists In：The dispersant is PEG-4000 or polyoxyethylene poly-oxygen propylene aether block copolymer.
- 6. the synthetic method according to claim 1 or 2 for lithium-ion electric pool size controllable silicon nanotube, its feature exists In：The catalyst is ammoniacal liquor.
- 7. the synthetic method according to claim 1 or 2 for lithium-ion electric pool size controllable silicon nanotube, its feature exists In：The solvent is pure water.
- 8. the synthetic method according to claim 1 for lithium-ion electric pool size controllable silicon nanotube, it is characterised in that： The mesoporous silicon dioxide nano rod diameter is in 200-500nm, length in 1-4um.
- 9. the synthetic method according to claim 1 for lithium-ion electric pool size controllable silicon nanotube, it is characterised in that： The step（2）In, surfactant is polyethyleneimine, and in parts by mass, wherein polyethyleneimine is 0.4-1 parts, mesoporous Silicon dioxide nano rod is 1-3 parts, and solvent is 95-98 parts.
- 10. the synthetic method according to claim 1 for lithium-ion electric pool size controllable silicon nanotube, its feature exists In：The reducing agent is magnesium powder, and the mass ratio of Silica Nanotube and reducing agent is 5:1-3.
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Cited By (3)
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| CN110065947A (en) * | 2019-04-02 | 2019-07-30 | 贵州大学 | A kind of wet chemical preparation method of Silica Nanotube |
| CN110562985A (en) * | 2019-09-23 | 2019-12-13 | 北京化工大学 | preparation method and application of porous silicon nanowire |
| CN111807810A (en) * | 2019-04-12 | 2020-10-23 | 北京化工大学 | Preparation method of nanowire/silicon-aluminum aerogel composite material |
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