CN1887702A - Process of preparing carbon nanotube - Google Patents
Process of preparing carbon nanotube Download PDFInfo
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- CN1887702A CN1887702A CNA2006100290067A CN200610029006A CN1887702A CN 1887702 A CN1887702 A CN 1887702A CN A2006100290067 A CNA2006100290067 A CN A2006100290067A CN 200610029006 A CN200610029006 A CN 200610029006A CN 1887702 A CN1887702 A CN 1887702A
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- carbon nanotube
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Abstract
The present invention discloses process of preparing carbon nanotube. The base plate material is first acid etched in acid solution and then burnt in flame of organic solvent, and the black powdered burnt product is collected as the carbon nanotube. The said process needs no expensive equipment, has simple operation and low cost, and is easy to use in industrial production.
Description
Technical field
The present invention relates to prepare the method for carbon nano fiber and carbon nanotube, particularly prepare the method for carbon nanotube by phase carbon source.
Technical background
Carbon nanotube belongs to richness and reins in carbon system, is the seamless nano level tubular structure material that is curled and formed by the single or multiple lift graphite flake, is called single wall or multiple-wall carbon nanotube (SWCNTs or MWCNTs).Since the Iijima of Japanese NEC produces in the world first CNT (carbon nano-tube), CNT (carbon nano-tube) is just with the characteristic of its many novelties, as high tensile strength, both can be conductor, semi-conductor, and can be machinery, conductivities such as isolator again and caused the researchist's of each subject such as material, physics, chemistry very big concern.
The early stage method for preparing carbon nanotube mainly contains laser evaporation synthesis method and arc process, and people had developed chemical Vapor deposition process (CVD), diffusion flame method, low temperature solid state heat solution, polymer manufacture method, hydrothermal synthesis method etc. again afterwards.Traditional method needs strict reaction conditions, as higher temperature of reaction or vacuum tightness, and needs to use expensive equipment.
Chemical physics wall bulletin (Chemical Physics Letters 323.2000.217-223) has reported that R.L.Vander Wal uses diffusion flame method synthesizing carbon nanotubes the earliest, and he utilizes the method that is blown into granules of catalyst in acetylene and ethene flame to make.The Dr.Kozo Saito of department of mechanical engineering of engineering college of Kentucky, United States university professor's research group has also synthesized carbon nanotube with the diffusion flame method subsequently.Professor Pan Chunxu of Wuhan University with the diffusion flame method with ethanol, the methyl alcohol carbon nanotube that has been feedstock production.But the existing remarkable defective of aforesaid method is to need expensive device, complicated operation, cost height, can't realize suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing carbon nanotube, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
At first baseplate material is put into acid solution and carry out acid etching, place the flame of organic solvent to burn the baseplate material of handling well then, collect the black powder shape product after burning, be carbon nanotube.The long 0.5-2.5 μ of carbon nanotube m, external diameter is 30-50nm, internal diameter is 5-8nm.
Said baseplate material is the pure nickel tinsel, and thickness is 0.2～1mm;
Said acid solution is that weight concentration is that nitric acid or the weight concentration of 65-68% is 36-38% hydrochloric acid;
Baseplate material carries out acid etching in acid solution time is 2～5 minutes;
Said organic solvent is selected from the monohydroxy-alcohol of C1～C6 or the alkane of C1～C6, preferred n-propyl alcohol or normal hexane;
Baseplate material combustion time in organic solvent flame is 10～15 minutes.
Adopt method of the present invention to prepare carbon nanotube, need not expensive device, simple to operate, with low cost, be easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is the electromicroscopic photograph of embodiment 1 product.
Fig. 2 is the electromicroscopic photograph of embodiment 2 products.
Fig. 3 is for adopting JSM-5600LV type scanning electronic microscope to embodiment 2 product observationss.
Fig. 4 is embodiment 2 product Raman spectrums.
Fig. 5 is the electromicroscopic photograph of embodiment 3 products.
Fig. 6 is for adopting JSM-5600LV type scanning electronic microscope to embodiment 3 product observationss.
Embodiment
Adopting thickness is that the pure nickel sheet of 0.4mm is made baseplate material, corrodes 5 minutes in weight concentration is 37% hydrochloric acid, and burning is 15 minutes in n-propyl alcohol flame, collects the product after the burning, obtains carbon nanotube.The long 2.5 μ m of carbon nanotube, external diameter is 35nm, internal diameter is 5nm.Black powder shape product of the present invention is scattered in the ethanol, behind the ultra-sonic dispersion, drops in sample preparation on the copper mesh, adopt JEM-100CXII type transmission electron microscope observing sample topography then, pattern such as Fig. 1, bar=50nm.
Embodiment 2
Adopting thickness is that the pure nickel sheet of 0.2mm is made baseplate material, corrodes 5 minutes in weight concentration is 67% nitric acid, and burning is 15 minutes in n-propyl alcohol flame, collects the product after the burning, obtains carbon nanotube.The long 0.5 μ m of carbon nanotube, external diameter is 50nm, internal diameter is 8nm.Black powder shape product of the present invention is scattered in the ethanol, behind the ultra-sonic dispersion, drops in sample preparation on the copper mesh, adopt JEM-100CXII type transmission electron microscope observing sample topography then, pattern as shown in Figure 2, bar=100nm.
Adopt JSM-5600LV type scanning electronic microscope that products of combustion is observed, scanned photograph as shown in Figure 3.
Adopt French LabRam-1B type laser Raman spectrometer that products of combustion is characterized, product as shown in Figure 4, there is being the G mould (graphite band) that characterizes the active mould of the graphited Raman of carbon pipe high order that the D peak, unordered peak that characterizes carbon tubular construction defective is being arranged near the 1336cm-1 place near the 1596cm-1 place, strength ratio ID/IG is about 1.083, shows that the carbon nanotube of method preparation of the present invention has the intact graphite-structure of formation.
Embodiment 3
Adopting thickness is that the pure nickel sheet of 0.4mm is made baseplate material, corrodes 5 minutes in weight concentration is 65% nitric acid, and burning is 15 minutes in normal hexane flame, collects product, obtains carbon nanotube.The long 5 μ m of carbon nanotube, external diameter is 20nm, internal diameter is 4nm.Black powder shape product of the present invention is scattered in the ethanol, behind the ultra-sonic dispersion, drops in sample preparation on the copper mesh, adopt JEM-100CXII type transmission electron microscope observing sample topography then, pattern as shown in Figure 5, bar=100nm.
Adopt JSM-5600LV type scanning electronic microscope that products of combustion is observed, except that common pattern carbon nanotube, also have a small amount of helicoidal structure in scanned photograph (as accompanying drawing 6) the demonstration products of combustion.
Claims (8)
1. method for preparing carbon nanotube, it is characterized in that, comprise the steps: that at first baseplate material being put into acid solution carries out acid etching, place the flame of organic solvent to burn the baseplate material of handling well then, collect the black powder shape product after burning, be carbon nanotube.
2. method according to claim 1 is characterized in that, said baseplate material is the pure nickel tinsel.
3. method according to claim 2 is characterized in that, baseplate material thickness is 0.2～1mm.
4. method according to claim 1 is characterized in that, said acid solution is that weight concentration is that nitric acid or the weight concentration of 65-68% is 36-38% hydrochloric acid.
5. method according to claim 1 is characterized in that, baseplate material carries out acid etching in acid solution time is 2～5 minutes.
6. method according to claim 1 is characterized in that, baseplate material combustion time in organic solvent flame is 10～15 minutes.
7. method according to claim 1 is characterized in that, said organic solvent is selected from the monohydroxy-alcohol of C1～C6 or the alkane of C1～C6.
8. according to each described method of claim 1～7, it is characterized in that, the long 0.5-2.5 μ of carbon nanotube m, external diameter is 30-50nm, internal diameter is 5-8nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100290067A CN1887702A (en) | 2006-07-17 | 2006-07-17 | Process of preparing carbon nanotube |
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| CNA2006100290067A CN1887702A (en) | 2006-07-17 | 2006-07-17 | Process of preparing carbon nanotube |
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| CN1887702A true CN1887702A (en) | 2007-01-03 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807205A (en) * | 2012-09-07 | 2012-12-05 | 天津大学 | Self-assembling method for low-fiber carbon nanometer material |
| CN104961120A (en) * | 2015-06-11 | 2015-10-07 | 中国工程物理研究院化工材料研究所 | Preparation method of carbon nanotube |
| CN107619036A (en) * | 2017-11-02 | 2018-01-23 | 北京化工大学 | The method that burning is oriented to quick preparation structure ordered carbon nanotube array |
| CN112191239A (en) * | 2020-10-12 | 2021-01-08 | 中国科学技术大学 | In-situ grown self-supporting nickel-oxygen co-doped carbon nanotube catalyst and preparation and application thereof |
-
2006
- 2006-07-17 CN CNA2006100290067A patent/CN1887702A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807205A (en) * | 2012-09-07 | 2012-12-05 | 天津大学 | Self-assembling method for low-fiber carbon nanometer material |
| CN104961120A (en) * | 2015-06-11 | 2015-10-07 | 中国工程物理研究院化工材料研究所 | Preparation method of carbon nanotube |
| CN107619036A (en) * | 2017-11-02 | 2018-01-23 | 北京化工大学 | The method that burning is oriented to quick preparation structure ordered carbon nanotube array |
| CN112191239A (en) * | 2020-10-12 | 2021-01-08 | 中国科学技术大学 | In-situ grown self-supporting nickel-oxygen co-doped carbon nanotube catalyst and preparation and application thereof |
| CN112191239B (en) * | 2020-10-12 | 2021-10-01 | 中国科学技术大学 | In-situ grown self-supporting nickel-oxygen co-doped carbon nanotube catalyst and preparation and application thereof |
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