CN110171815A - A kind of preparation method of the high-purity carbon nano-tube film of low cost - Google Patents
A kind of preparation method of the high-purity carbon nano-tube film of low cost Download PDFInfo
- Publication number
- CN110171815A CN110171815A CN201910530539.0A CN201910530539A CN110171815A CN 110171815 A CN110171815 A CN 110171815A CN 201910530539 A CN201910530539 A CN 201910530539A CN 110171815 A CN110171815 A CN 110171815A
- Authority
- CN
- China
- Prior art keywords
- carbon nano
- tube film
- film
- carbon
- tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/159—Carbon nanotubes single-walled
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/04—Nanotubes with a specific amount of walls
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/06—Multi-walled nanotubes
Abstract
The present invention relates to optoelectronic areas, mainly a kind of fast preparation method of high-purity carbon nano-tube film without any additive of low cost.This preparation method use feasible, easy and environmentally friendly operating method, after carbon nanotube is carried out ultrasonic disperse and mechanical stirring in dehydrated alcohol dispersing agent, by vacuum filtration, successfully prepared can large area remove carbon nano-tube film.By the way that carbon nanotube is removed from the large area on filter paper, carbon nano-tube film is transferred on other desired substrate.The carbon nano-tube film of method preparation has good compactness and electrical properties.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity carbon nano-tube film, more particularly to one kind are living without using other surfaces
The method that the controllable and efficient liquid phase of low cost, size of property agent prepares carbon nano-tube film.
Background technique
Carbon nanotube is a kind of typical one-dimensional material, since 1991 are found, carbon nanotube in photoelectron and
The application prospect in the fields such as bio-sensing causes extensive concern.Carbon nanotube can be divided into single according to its structure
Pipe, double-walled carbon nano-tube and multi-walled carbon nanotube.Carbon nanotube has very big specific surface area and excellent electric conductivity and heat
Stability.The carbon nano-tube film as made of carbon nanotube arrangement also has unique physics and chemical property, makes it in flexibility
Electrode, wearable device, touch screen and display etc. have broad application prospects.
Carbon nano-tube film can directly be grown to film by carbon source, can also by using carbon nanotube as raw material come
Film forming.Membrane formation process is directly grown by carbon source to the more demanding of equipment, the process conditions of preparation are also more harsh, are difficult to realize big
The preparation of batch.The technical process that film is prepared using carbon nanotube is then relatively easy, and the most common method is exactly that liquid phase is heavy
Area method.One kind property of can choose is referred in " a kind of preparation method of carbon nano-tube film " of application number 201510495655.5
The medium of carbon nanotube is adsorbed to form a film, however its preparation process not only used surfactant, there are also acidizations.Due to
Carbon nanotube is easy to reunite, it is not easy to disperses, thus many preparation methods all help to disperse using surfactant.Surface
Activating agent is difficult to completely remove, and remaining surfactant can have a huge impact its optical property, more furthermore
Acidization can also destroy the integrality of carbon nanotube chemical structure.Thus, it is badly in need of a kind of without using any surfactant
The preparation method of carbon nano-tube film." preparation method of carbon nano-tube film " of application number 200910309105.4 equally uses
The method of vacuum filtration prepares carbon nano-tube film, however the process for removing dispersion liquid is complicated, long period, in the process also
The chemical reagent such as strong acid have been used, pollution is easy and have destroyed carbon nanotube.In addition, when removing filter membrane, it be in acetone steam
1 h or more is kept, acetone is toxic gas, it is be easy to cause environmental pollution and insecurity factor, and the time for removing filter membrane is longer,
It is unfavorable for improving preparation efficiency.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of high-purity carbon nano-tube film that low cost is additive-free, lead to
It crosses and does not add any additive to carry out vacuum filtration film forming, carry out the integrality of the chemical structure of effective protection carbon nanotube, from
And the photoelectric characteristic for keeping carbon nanotube excellent.
The invention discloses a kind of high-purity carbon nano-tube film preparation methods of low cost, it is characterised in that carbon nanotube is put
Enter and carries out liquid phase ultrasonic disperse and mechanical stirring, the carbon nano tube dispersion liquid being evenly distributed, carbon nanotube in organic solvent
The concentration of dispersion liquid obtains being adhered to the carbon nano-tube film on filter paper by vacuum filtration in 0.05~0.1 mg/ml, leads to
The removing for carrying out large area to the carbon nano-tube film being adhered on filter paper is crossed, makes it easier to be transferred to other different substrates
On, to adapt to different application demands.
The described high-purity carbon nano-tube film preparation side of low cost, including uniform carbon nano tube dispersion liquid is obtained, carbon is received
The operating procedures such as the transfer of vacuum filtration and carbon nano-tube film of mitron dispersion liquid, feature are specific as follows:
Dispersing agent of the step (1) only with dehydrated alcohol as carbon nanotube, does not add other any surfactants, and carbon is received
The proportion of mitron and dehydrated alcohol is mg: 50-100 ml of 5-10, and carbon nanotube is scattered in dehydrated alcohol；
Step (2) is 30~36 min of dispersion liquid ultrasound of carbon nanotube and dehydrated alcohol, and then 2 h of mechanical stirring, stirring turn
Speed be 500 rpm, then 3~5 min of ultrasound after, be filtered by vacuum, film dried, can quickly obtain being adsorbed on filter paper
Carbon nano-tube film；
Step (3) takes the carbon nano-tube film after being dried, along the standardized circle notch in the edge of film, then being adhered on filter paper
Carbon nano-tube film is placed in the ethanol solution of 200~300 ml, pays attention to the side that make to have film downward, at 75 DEG C
Heating makes ethanol solution boil, and the tension overflowed outward using bubble can realize the quick separating of film and filter paper；
After step (4) carbon nano-tube film is separated with filter paper, filter paper is taken away, the carbon nano-tube film after peeling is placed in anhydrous second
In alcoholic solution, when being transferred on quartz substrate or other substrates, it need to only be picked up with quartz plate, carbon nano-tube film is allowed to be attached to
It on quartz plate or other substrates, then is dried, can successfully shift carbon nano-tube film.
Carbon nanotube in above-mentioned steps (1) is one or more of single wall, double-walled or multi-walled carbon nanotube.
In the present invention, in step (1) when obtaining the dispersion liquid of carbon nanotube, only with dehydrated alcohol, this one kind is organic
Solvent is as dispersing agent, and the film that dehydrated alcohol is conducive to make deposition to obtain is fine and close, and dehydrated alcohol highly volatile, after film forming
It can be completely removed by heating, high-purity carbon nano-tube film can be obtained；
The method for obtaining film using vacuum filtration in step (2), the equipment of use is simple and convenient, the time inner edge of 4 h can
Carbon nano-tube film is prepared, and can be prepared with mass, can be obtained not using various sizes of Suction filtration device simultaneously
With the carbon nano-tube film of size；The Suction filtration device is mainly made of glass sand core filter device, filter paper and vacuum pump, different
The Suction filtration device of size is primarily referred to as the glass sand core filter device and various sizes of filter paper of different size.Thus, pass through
Change the size of Suction filtration device to make various sizes of carbon nano-tube film.
In step (3) by the way of Bubbling method separating carbon nano-tube film and filter paper, used solution and carbon nanometer
The dispersing agent of pipe is consistent, has not only reduced costs but also will not introduce new impurity, in addition, not can cause environmental pollution also.And
The method can quickly be such that carbon nano-tube film and filter paper separates, and make it with impregnating by acidification or in the solution long-time
Isolated method is compared, and time cost has greatly been saved, and also avoids the secondary pollution of carbon nano-tube film, therefore, is had
High efficiency and high-purity property；
Step is placed in the carbon nano-tube film after peeling in ethanol solution in (4), can to avoid the curling of carbon nanotube,
Simultaneously convenient for being transferred on other substrates, the composite construction of carbon nanotube and other substrates or film can be readily available.
High-purity carbon nano-tube film prepared by the present invention, in the removing of vacuum filtration film forming procedure and carbon nano-tube film
It all only used a kind of volatile dehydrated alcohol reagent in the process.Impurity can generate very big shadow to the optical property of material
It rings, consequently only that high-purity carbon nano-tube film is just more suitable for for optoelectronic areas.
Technique effect and advantage of the invention:
1. overall technology route is innovated, high-purity carbon nanometer has successfully been prepared using easy, feasible and environmentally friendly mentality of designing
Pipe film, the chemical reagent used is all cheap cheap, nontoxic.
2. the method preparation process is easy, operation is feasible, only used dehydrated alcohol in preparation process and transfer process
This kind of volatile organic reagent, while maintaining carbon nanotube chemical structural intergrity, by making the carbon being prepared
Nano-tube film is free of other additives, has high purity, so as to be applied to field of optoelectronic devices well.
3. the size of the short preparation period of carbon nano-tube film, carbon nano-tube film is controllable.
Detailed description of the invention
Fig. 1 is the schematic diagram for preparing high-purity carbon nano-tube film preparation；1 dispersing agent in figure, 2 be CNT, 3 ultrasounds, 4 stirrings,
5 be CNT dispersion, 6 Suction filtration devices, 7 filter paper, 8 be carbon nanotube thin film, 9 dryings, 10 removings, 11 dehydrated alcohols, 12 transfer, 13 lining
Bottom.
Fig. 2 is the visible light figure for the carbon nano-tube film being prepared；
Fig. 3 is the I-V analysis result figure for the carbon nano-tube film being prepared；
Fig. 4 is the UV-Vis characterization spectrogram for the carbon nano-tube film being prepared.
Specific embodiment
Embodiment 1, as shown in Figs 1-4
It weighs 10 mg of double-walled carbon nano-tube to be put into beaker, 100 mL dehydrated alcohols is added, water bath sonicator handles 36 min, so
After carry out mechanical stirring, speed of agitator is 500 rpm, and mixing time is 2 h, 3 min of water bath sonicator again after the completion of stirring
Obtain the uniform dispersion of carbon nanotube.Carbon nano tube dispersion liquid is filtered by vacuum immediately, obtains being adhered on filter paper
Carbon nano-tube film.After his nano-tube film is dried, along the standardized circle notch in the edge of film, then it is placed in dehydrated alcohol
In, 75 DEG C are boiled 5~10 min, and carbon nano-tube film is just stripped down from filter paper.The carbon nano-tube film that will be stripped down
It is placed in dehydrated alcohol, when transfer, the transfer that carbon nanotube can be realized is picked up with required substrate.
As shown in Figure 1, be the schematic diagram of carbon nano-tube film preparation process, equipment is simple, concise in technology, manufacturing cycle
Less than 5 h, the carbon nano-tube film of preparation has high-purity.
As shown in Fig. 2, being the visible light figure of carbon nano-tube film, the carbon nanotube of preparation has good compactness.
As shown in figure 3, to talk the I-V analysis chart of nano-tube film, the resistance very little of carbon nano-tube film has good
Electric conductivity and uniformity.
As shown in figure 4, the UV-Visible absorption for carbon nano-tube film characterizes spectrogram, it can be seen that carbon nanotube is thin
Film has wide absorption spectrum.
The one or more steps that the present invention mentions is not repelled the combination step there is also other methods and was operated
Journey；It shall yet further be noted that the example is merely to illustrate feasibility of the invention, it is not intended to limit the scope of the invention.In addition to this, exist
In the case where without material alterations technology of preparing content, also when being considered as implementable scope of the invention.
Claims (3)
1. a kind of high-purity carbon nano-tube film preparation method of low cost, it is characterised in that carbon nanotube be put into organic solvent into
The concentration of row liquid phase ultrasonic disperse and mechanical stirring, the carbon nano tube dispersion liquid being evenly distributed, carbon nano tube dispersion liquid exists
0.05~0.1 mg/ml obtains being adhered to the carbon nano-tube film on filter paper by vacuum filtration, by being adhered to filter paper
On carbon nano-tube film carry out large area removing, make it easier to be transferred on other different substrates, it is different to adapt to
Application demand.
2. the high-purity carbon nano-tube film preparation side of low cost as claimed in claim 1, including obtain uniform carbon nanotube point
Dispersion liquid, the operating procedures such as transfer of vacuum filtration and carbon nano-tube film of carbon nano tube dispersion liquid, feature are specific as follows:
Dispersing agent of the step (1) only with dehydrated alcohol as carbon nanotube, does not add other any surfactants, and carbon is received
The proportion of mitron and dehydrated alcohol is mg: 50-100 ml of 5-10, and carbon nanotube is scattered in dehydrated alcohol；
Step (2) is 30~36 min of dispersion liquid ultrasound of carbon nanotube and dehydrated alcohol, and then 2 h of mechanical stirring, stirring turn
Speed be 500 rpm, then 3~5 min of ultrasound after, be filtered by vacuum, film dried, can quickly obtain being adsorbed on filter paper
Carbon nano-tube film；
Step (3) takes the carbon nano-tube film after being dried, along the standardized circle notch in the edge of film, then being adhered on filter paper
Carbon nano-tube film is placed in the ethanol solution of 200~300 ml, pays attention to the side that make to have film downward, at 75 DEG C
Heating makes ethanol solution boil, and the tension overflowed outward using bubble can realize the quick separating of film and filter paper；
After step (4) carbon nano-tube film is separated with filter paper, filter paper is taken away, the carbon nano-tube film after peeling is placed in anhydrous second
In alcoholic solution, when being transferred on quartz substrate or other substrates, it need to only be picked up with quartz plate, carbon nano-tube film is allowed to be attached to
It on quartz plate or other substrates, then is dried, can successfully shift carbon nano-tube film.
3. the high-purity carbon nano-tube film preparation method of low cost as claimed in claim 2, the carbon nanotube in step (1) is single
One or more of wall, double-walled or multi-walled carbon nanotube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910530539.0A CN110171815A (en) | 2019-06-19 | 2019-06-19 | A kind of preparation method of the high-purity carbon nano-tube film of low cost |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910530539.0A CN110171815A (en) | 2019-06-19 | 2019-06-19 | A kind of preparation method of the high-purity carbon nano-tube film of low cost |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110171815A true CN110171815A (en) | 2019-08-27 |
Family
ID=67697497
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910530539.0A Pending CN110171815A (en) | 2019-06-19 | 2019-06-19 | A kind of preparation method of the high-purity carbon nano-tube film of low cost |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110171815A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451484A (en) * | 2019-09-04 | 2019-11-15 | 北京华碳元芯电子科技有限责任公司 | A kind of preparation facilities and method of carbon nano-tube film |
| CN112897511A (en) * | 2021-02-05 | 2021-06-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Surface-cleaning single-walled carbon nanotube, and preparation method, system and application thereof |
| CN113675430A (en) * | 2021-08-09 | 2021-11-19 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Cooling water system of proton exchange membrane fuel cell test board |
| CN114149001A (en) * | 2021-12-22 | 2022-03-08 | 浙江大学 | Preparation, transfer and orientation determination method of self-assembled carbon nanotube array for terahertz |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691280A (en) * | 2009-10-30 | 2010-04-07 | 上海交通大学 | Method for preparing carbon nano tube film |
| CN106477548A (en) * | 2016-09-18 | 2017-03-08 | 北京华碳元芯电子科技有限责任公司 | A kind of preparation method of carbon nano-tube film |
-
2019
- 2019-06-19 CN CN201910530539.0A patent/CN110171815A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691280A (en) * | 2009-10-30 | 2010-04-07 | 上海交通大学 | Method for preparing carbon nano tube film |
| CN106477548A (en) * | 2016-09-18 | 2017-03-08 | 北京华碳元芯电子科技有限责任公司 | A kind of preparation method of carbon nano-tube film |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451484A (en) * | 2019-09-04 | 2019-11-15 | 北京华碳元芯电子科技有限责任公司 | A kind of preparation facilities and method of carbon nano-tube film |
| CN112897511A (en) * | 2021-02-05 | 2021-06-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Surface-cleaning single-walled carbon nanotube, and preparation method, system and application thereof |
| CN113675430A (en) * | 2021-08-09 | 2021-11-19 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Cooling water system of proton exchange membrane fuel cell test board |
| CN114149001A (en) * | 2021-12-22 | 2022-03-08 | 浙江大学 | Preparation, transfer and orientation determination method of self-assembled carbon nanotube array for terahertz |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110171815A (en) | A kind of preparation method of the high-purity carbon nano-tube film of low cost | |
| CN102877367B (en) | Carbon nanotube/short-fiber composited nano-carbon paper and continuous preparation method thereof | |
| CN103253659B (en) | A kind of ultrasonic wave peels off the method for preparing graphite alkene | |
| CN103058172B (en) | Preparation method of carbon nanometer tube-graphene composite material | |
| CN103449420B (en) | High-quality graphene dispersion method and film preparation method | |
| CN102173406B (en) | Preparation method for carbon nano tube or graphene extra-thin film | |
| US10472243B2 (en) | Industrial method for preparing large-sized graphene | |
| CN104445167A (en) | Preparation method of water-soluble graphene | |
| CN105536842B (en) | A kind of carbonitride/tungsten trioxide nano composite and its preparation method and application | |
| CN102580716B (en) | Method for synthesizing zinc oxide/graphene composite by solvothermal method | |
| CN105439133B (en) | A kind of preparation method of elecrtonegativity single-layer graphene | |
| CN111170864B (en) | Graphene dispersing agent and preparation method thereof, and preparation method of graphene | |
| CN102351165A (en) | Large-area freestanding carbon nanotube paper and preparation method thereof | |
| CN104959622B (en) | Synthesis method for copper nanowire with different length-diameter ratios | |
| WO2013106963A1 (en) | Process for preparing graphene dispersion | |
| CN107201689B (en) | A kind of preparation method of carbon nano tube electromagnetic shielding paper | |
| CN102832050A (en) | Method for preparing graphene/carbon nanotube hybrid in hierarchical structure | |
| CN105752970B (en) | A kind of preparation method of carbon nano tube/graphene compound | |
| CN105967172A (en) | Preparation method of foldable graphene thin film of large area | |
| CN104851515B (en) | A kind of preparation method of conductive film | |
| CN101913594A (en) | Method for preparing carbon nanotube film by removing residual dispersant by alkali treatment | |
| CN113772732A (en) | Method for preparing two-dimensional material nanosheet by DEET stripping | |
| CN109305675A (en) | A kind of method that quantum dot auxiliary prepares graphene dispersing solution | |
| CN113118002A (en) | Carbon nanotube/two-dimensional titanium carbide transparent electromagnetic shielding film and preparation method thereof | |
| CN100454474C (en) | Method for preparing field emission display cathode and ZnO nanowire cathode |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190827 |
|
| RJ01 | Rejection of invention patent application after publication |