CN106219516B - A kind of method that solution left standstill method prepares oriented alignment single-walled carbon nanotube - Google Patents
A kind of method that solution left standstill method prepares oriented alignment single-walled carbon nanotube Download PDFInfo
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- CN106219516B CN106219516B CN201610604496.2A CN201610604496A CN106219516B CN 106219516 B CN106219516 B CN 106219516B CN 201610604496 A CN201610604496 A CN 201610604496A CN 106219516 B CN106219516 B CN 106219516B
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Abstract
The invention discloses a kind of methods that solution left standstill method prepares oriented alignment single-walled carbon nanotube, it is rested in the colloidal liquid that single-walled carbon nanotube, deionized water, surfactant, organic polymer are mixed to prepare by the substrate inclination by surface with parallel pole, since parallel pole enables carbon nanotube oriented alignment parallel pole to the dimensional effect of carbon nanotube.This method prepares the aligned carbon nanotube of vertical arrangement compared to traditional chemical vapour deposition technique, easy to operate, is prepared for the carbon nanotube of horizontal orientation arrangement, can be applied in scene effect pipe, field emission device and chemical sensor.
Description
Technical field
The present invention relates to function film preparation methods, belong to nano film material field and field of nanometer devices, specifically relate to
A kind of and method that novel solution left standstill method prepares oriented alignment single-walled carbon nanotube.
Background technique
For carbon nano-tube material as a kind of new functional material paid close attention in recent years by various countries, it has good current-carrying
The features such as transport factor and electric current transport ability, good mechanical property, good optical property, makes its scene effect pipe, field hair
Has good application prospect in the devices such as emitter, semiconductor probe, chemical sensor.
For many years, single-walled carbon nanotube is seen as that silicon substrate can be replaced due to its good electric property and ultra-thin structure
The new material of TFT.The method for preparing single-walled carbon nanotube TFT is divided into two kinds: chemical vapour deposition technique and solution filtration method.
Chuan Wang in 2009 etc. is prepared for high performance single-walled carbon nanotube TFT using solution filtration method method, and current density reaches
10uA/ μm, on-off ratio is greater than 104.(Chuan Wang etc Wafer~Scale Fabrication of Separated
Carbon Nanotube Thin~Film Transistors for Display Applications, Nano Letters,
2009,Vol.9,No.12)。
S.J Wind in 2002 etc. is prepared for single-walled carbon nanotube TFT using chemical vapour deposition technique, and current density reaches
2100 uA/um.(S.J Wind etc Vertical scaling of carbon nanotube field~effect
transistors using top gate electrodes, Applied physics Letters,2002,Vol.80,
No.20) but the carbon nanotube TFT of these methods preparation is since the density of carbon nanotube is low and non-directional characteristic, electrical property
Application demand can be not achieved.In order to solve problem above, Hyunhyub Ko etc. proposes that one kind can allow carbon nano-tube oriented alignment
Method.And when using solution filtration method, the polymer solution of carbon nanotube is fixed in certain area coverage in film forming,
And by self-assembled film Parallel Growth on silicon wafer, in silicon wafer, plated film, carbon nanotube can be since dimensional effect be in directional trend arrangement again
(since the spacing of self-assembled film is less than the length of carbon nanotube).(Hyunhyub Ko etc Liquid~Crystalline
Processing of Highly Oriented Carbon Nanotube Arrays for Thin~Film
Transistors, Nano Letters, 2006, Vol.6, No.7) but this method due to obtaining the film that aligns
Plated electrode again afterwards, may have residue when removing self-assembled film, influence structural behaviour, and be not easy to determine the carbon nanotube of orientation
Region, it is complicated for operation, it is not easy to intact device be made.
Summary of the invention
The purpose of the present invention is how to overcome, preparation carbon nanotube cost is excessively high, preparation is complicated, carbon nanotube concentration is too low
And there is no the disadvantages of directionality, electric property is poor, improve existing carbon nanotube the preparation method, simplify preparation method, obtain
High performance carbon nanotube.
Technical problem proposed by the invention solves in this way: providing a kind of novel solution left standstill method preparation orientation row
The method of cloth single-walled carbon nanotube, which is characterized in that have follow steps:
(1) single-walled carbon nanotube, deionized water, surfactant are uniformly mixed, obtain solution 1;
(2) organic polymer is added into solution 1, is uniformly mixed, obtains black colloidal liquid, ie in solution 2;
(3) the substrate inclination with parallel pole is rested in solution 2, prepares wet film；
(4) make the film spontaneous nucleation in step (3) under room temperature, in normal atmospheric conditions, be formed in parallel with substrate orientation
The single-walled carbon nanotube figure of arrangement；
(5) photoetching removes extra part, obtains complete aligned carbon nanotube figure.
Further, the mass ratio of the single-walled carbon nanotube and surfactant is 1:5~10.
Further, the mass ratio of the single-walled carbon nanotube and organic polymer is 1:10~20.
Further, the surfactant and organic polymer can allow single-walled carbon nanotube to be suspended in solution surface.
The environment for preparing is general room environment, the requirement such as inert free gas protection, adiabatic drying.
The surfactant is dodecyl trimethyl ammonium bromide, cetyl trimethylammonium bromide, dodecyl
One of benzene sulfonic acid sodium salt, cetyl benzenesulfonic acid sodium are a variety of, preferably neopelex；
The organic polymer is polypeptide or protein, such as Polystyrene Sulronate, polyvinyl alcohol, polyvinylpyrrolidine
Ketone etc., preferably polyvinylpyrrolidone.
Further, the thickness of the substrate does not have particular/special requirement, is provided with 300~500nm insulating layer above it, absolutely
The metal layer of 100~300nm is provided in edge layer, metal layer lithography goes out parallel pole.
Preferably, the insulating layer is SiO2Insulating layer, the length of the parallel pole are 0.1~5mm, electrode
Between spacing be 3~30 μm.Parallel pole figure can play orientation to the carbon nanotube of distribution between the electrodes.
Further, inclination standing refers to that being in 3~20 ° for substrate favours the culture equipped with solution 2 in the step (3)
In ware, and make the long side of parallel pole horizontal by 3~20 ° of angles, time of repose is 24~72 small in the step (3)
When.
Further, the mixing in the step (1) and step (2) is all made of ultrasonic mixing.
Preferably, the step (1) or step (2) can be combined with magnetic agitation while using ultrasonic mixing,
The magnetic agitation temperature of the step (1) is 60~80 DEG C, and the time is 3~6 hours, the magnetic agitation temperature of the step (2)
It is 60~80 DEG C for temperature, the time is 10~30min.
The carbon nanotube prepared using method of the present invention, is had the advantage that
A. orientating products are good, stable electrical properties, stable structure, uniform, smooth；
B. interdigital electrode is first carried out, recycles interdigital electrode to the orientation of carbon nanotube, entire technological operation is simple；
C. normal-temperature reaction, and to environment without particular/special requirement, equipment requirement is low, needs small investment, product cost low；
D. reactant is nontoxic, does not pollute the environment and influences human health.
Detailed description of the invention
Fig. 1 is the method for the present invention flow chart；
The orientation SEM of Fig. 2 single-walled carbon nanotube between 1 products obtained therefrom parallel pole of embodiment schemes；
Fig. 3 is the non-directional SEM figure of the outer single-walled carbon nanotube of 1 products obtained therefrom parallel pole of embodiment；
Fig. 4 is the method for the present invention schematic diagram (section)；
Wherein, 1 it is substrate, 2 is SiO2Insulating layer, 3 be parallel pole, 4 be oriented alignment single-walled carbon nanotube.
Specific embodiment
The present invention is done below with reference to embodiment and attached drawing and is further described:
A kind of embodiment 1: method that solution left standstill method prepares oriented alignment single-walled carbon nanotube, comprising the following steps:
(1) it takes 20mL deionized water to be fitted into beaker, weighs carbon nanotube 15mg, weigh neopelex
100mg is added in beaker, and magnet rotor is put into beaker, beaker is put into magnetic stirrer, and adjusting temperature is 70 DEG C, and revolving speed is
12rad/s, magnetic agitation 3 hours, while ultrasonic mixing is carried out, it is dispersed in neopelex and carbon nanotube
In deionized water, solution 1 is obtained；
(2) polyvinylpyrrolidone 150mg is taken to be added in solution 1, adjusting temperature is 70 DEG C, revolving speed 12rad/s, magnetic
Power stirs 10 minutes, while carrying out ultrasonic mixing, obtains black colloidal liquid, ie in solution 2；
(3) wet film is prepared using solution left standstill method, the substrate with parallel pole is rested in solution 2 with 5 ° of overturning angles
Wet film is prepared, 24 hours is stood and crystallizes；
(4) excess carbon nanotubes outside channel are fallen in photoetching, obtain product.
Product is tested using field emission scanning electron microscope (SEM), obtains Fig. 2, Fig. 3, by Fig. 2, Fig. 3 comparison it is found that
Orientating products performance is good, and structure is uniform, smooth, stable.
A kind of embodiment 2: method that solution left standstill method prepares oriented alignment single-walled carbon nanotube, comprising the following steps:
(1) it takes 20mL deionized water to be fitted into beaker, weighs carbon nanotube 15mg, weigh dodecyl trimethyl ammonium bromide
75mg, cetyl trimethylammonium bromide 75mg be added beaker in, ultrasonic mixing, make ten behenyl ammonium bromides,
Cetyl trimethylammonium bromide and carbon nanotube are evenly dispersed in deionized water, obtain solution 1；
(2) it takes Polystyrene Sulronate 150mg, polyvinyl alcohol 150mg to be added in solution 1, is obtained after ultrasonic mixing is uniform black
Color colloidal liquid, ie in solution 2；
(3) wet film is prepared using solution left standstill method, the substrate with parallel pole is rested in solution 2 with 2 ° of overturning angles
Wet film is prepared, 72 hours is stood and crystallizes；
(4) excess carbon nanotubes outside channel are fallen in photoetching, obtain product.
A kind of embodiment 3: method that solution left standstill method prepares oriented alignment single-walled carbon nanotube, comprising the following steps:
(1) it takes 20mL deionized water to be fitted into beaker, weighs carbon nanotube 15mg, weigh cetyl trimethylammonium bromide
40mg, neopelex 60mg are added in beaker, and magnet rotor is put into beaker, beaker is put into magnetic stirrer,
Adjusting temperature is 80 DEG C, revolving speed 12rad/s, magnetic agitation 5 hours, while carrying out ultrasonic mixing, makes dodecyl benzene sulfonic acid
Sodium and carbon nanotube are evenly dispersed in deionized water, obtain solution 1；
(2) polyvinyl alcohol 200mg is taken to be added in solution 1, adjusting temperature is 80 DEG C, revolving speed 12rad/s, magnetic agitation 20
Minute, while ultrasonic mixing is carried out, obtain black colloidal liquid, ie in solution 2；
(3) wet film is prepared using solution left standstill method, the substrate with parallel pole is rested on into solution 2 with 30 ° of overturning angles
In prepare wet film, stand 48 hours crystallize；
(4) excess carbon nanotubes outside channel are fallen in photoetching, obtain product.
A kind of embodiment 4: method that solution left standstill method prepares oriented alignment single-walled carbon nanotube, comprising the following steps:
(1) it takes 20mL deionized water to be fitted into beaker, weighs carbon nanotube 15mg, weigh neopelex
75mg is added in beaker, and magnet rotor is put into beaker, beaker is put into magnetic stirrer, and adjusting temperature is 60 DEG C, and revolving speed is
12rad/s, magnetic agitation 6 hours, while ultrasonic mixing is carried out, it is dispersed in neopelex and carbon nanotube
In deionized water, solution 1 is obtained；
(2) it takes the protein 300mg that single-walled carbon nanotube can be allowed to be suspended in solution surface to be added in solution 1, adjusts temperature
Degree is 60 DEG C, revolving speed 12rad/s, magnetic agitation 30 minutes, while carrying out ultrasonic mixing, obtains black colloidal liquid, ie in solution
2；
(3) wet film is prepared using solution left standstill method, the substrate with parallel pole is rested in solution 2 with 5 ° of overturning angles
Wet film is prepared, 72 hours is stood and crystallizes；
(4) excess carbon nanotubes outside channel are fallen in photoetching, obtain product.
A kind of embodiment 5: method that solution left standstill method prepares oriented alignment single-walled carbon nanotube, comprising the following steps:
(1) it takes 20mL deionized water to be fitted into beaker, weighs carbon nanotube 15mg, weigh neopelex
80mg is added in beaker, carries out ultrasonic mixing, keeps neopelex and carbon nanotube evenly dispersed in deionized water,
Obtain solution 1；
(2) the polypeptides matter 250mg that single-walled carbon nanotube can be allowed to be suspended in solution surface is taken to be added in solution 1, into
Row ultrasonic mixing obtains black colloidal liquid, ie in solution 2；
(3) wet film is prepared using solution left standstill method, the substrate with parallel pole is rested on into solution 2 with 12 ° of overturning angles
In prepare wet film, stand 36 hours crystallize；
(4) excess carbon nanotubes outside channel are fallen in photoetching, obtain product.
As described above, only present pre-ferred embodiments, thus appoint it is all without departing from this programme technology contents, according to this hair
Bright technical spirit makes any simple change, equivalent variations and modification to above embodiments, still falls within the technology of the present invention
The range of scheme.
Claims (8)
1. a kind of method that solution left standstill method prepares oriented alignment single-walled carbon nanotube, which comprises the following steps:
(1) single-walled carbon nanotube, deionized water, surfactant are uniformly mixed, obtain solution 1；
(2) organic polymer is added into solution 1, is uniformly mixed, obtains black colloidal liquid, ie in solution 2；
(3) the substrate inclination with parallel pole is rested in solution 2, prepares wet film；
(4) make the film spontaneous nucleation in step (3) under room temperature, in normal atmospheric conditions, be formed in parallel with substrate and align
Single-walled carbon nanotube figure；
(5) photoetching removes extra part, obtains complete aligned carbon nanotube figure；
Inclination, which is stood, in the step (3) refers to that being in 3~20 ° for substrate favours in the culture dish equipped with solution 2, and makes
For the long side of parallel pole horizontal by 3~20 ° of angles, time of repose is 24~72 hours；Single in the step (2)
Pipe is 1:10~20 with organic polymer mass ratio.
2. the method that a kind of solution left standstill method according to claim 1 prepares oriented alignment single-walled carbon nanotube, feature
Be: the mass ratio of single-walled carbon nanotube and surfactant is 1:5~10 in the step (1).
3. the according to claim 1, method that a kind of 2 any solution left standstill methods prepare oriented alignment single-walled carbon nanotube,
It is characterized by: the surfactant and organic polymer can allow single-walled carbon nanotube to float on solution surface.
4. the method that a kind of solution left standstill method according to claim 3 prepares oriented alignment single-walled carbon nanotube, feature
Be: the surfactant is dodecyl trimethyl ammonium bromide, cetyl trimethylammonium bromide, detergent alkylate sulphur
One of sour sodium, cetyl benzenesulfonic acid sodium are a variety of；The organic polymer is polypeptide or protein.
5. the method that a kind of solution left standstill method prepares oriented alignment single-walled carbon nanotube according to claim 1, special
Sign is: being provided with the insulating layer of 300~500nm above the substrate, the metal of 100~300nm is provided on insulating layer
Layer, metal layer lithography go out parallel pole figure.
6. the method that a kind of solution left standstill method according to claim 5 prepares oriented alignment single-walled carbon nanotube, feature
Be: the insulating layer be SiO2 insulating layer, the parallel pole length be 0.1~5mm, interelectrode spacing be 3~
30 µm。
7. the method that a kind of solution left standstill method according to claim 1 prepares oriented alignment single-walled carbon nanotube, feature
Be: the mixing in the step (1) and step (2) is using ultrasonic mixing.
8. the method that a kind of solution left standstill method according to claim 1 prepares oriented alignment single-walled carbon nanotube, feature
Be: the step (1) or step (2) can be combined with magnetic agitation while using ultrasonic mixing, the step (1)
Magnetic agitation temperature is 60~80 DEG C, and the time is 3~6 hours, and it is 60~80 that the magnetic agitation temperature of the step (2), which is temperature,
DEG C, the time is 10~30min.
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| CN106904598A (en) * | 2017-04-20 | 2017-06-30 | 国家纳米科学中心 | A kind of CNT magnet and its preparation method and application |
| CN109534317B (en) * | 2017-09-21 | 2021-11-23 | 中国科学院物理研究所 | Preparation method of carbon nanotube film |
| CN109761222A (en) * | 2017-11-09 | 2019-05-17 | 北京华碳元芯电子科技有限责任公司 | The method for removing carbon nano tube surface dispersing agent using being evaporated in vacuo |
| CN110282974B (en) * | 2019-06-28 | 2020-12-29 | 华南理工大学 | Oriented magnetic carbon fiber graphene composite membrane and preparation method and application thereof |
| CN114149001B (en) * | 2021-12-22 | 2023-04-25 | 浙江大学 | Self-assembled carbon nano tube array preparation, transfer and orientation determination method for terahertz |
| CN115340085B (en) * | 2022-05-12 | 2024-04-26 | 中山大学 | Carbon nanotube film with controllable areal density and preparation method and application thereof |
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