CN101723355B - Amorphous carbon coated single-walled carbon nano tube line and preparation method thereof - Google Patents
Amorphous carbon coated single-walled carbon nano tube line and preparation method thereof Download PDFInfo
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- CN101723355B CN101723355B CN2009103104463A CN200910310446A CN101723355B CN 101723355 B CN101723355 B CN 101723355B CN 2009103104463 A CN2009103104463 A CN 2009103104463A CN 200910310446 A CN200910310446 A CN 200910310446A CN 101723355 B CN101723355 B CN 101723355B
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- amorphous carbon
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- walled carbon
- carbon nanotube
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- 239000002109 single walled nanotube Substances 0.000 title claims abstract description 37
- 229910003481 amorphous carbon Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000010439 graphite Substances 0.000 claims abstract description 14
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000010891 electric arc Methods 0.000 claims abstract description 5
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 3
- 150000003624 transition metals Chemical class 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002041 carbon nanotube Substances 0.000 description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000011280 coal tar Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000001241 arc-discharge method Methods 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 3
- 239000010977 jade Substances 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
一种纳米材料技术领域的非晶碳包裹单壁碳纳米管线及其制备方法；该非晶碳包裹单壁碳纳米管线由无定形碳构成的外壳和包裹在该外壳中的单壁碳纳米管组成；其制备方法包括如下步骤：步骤一，将催化剂与石墨粉混合，制备石墨棒；所述催化剂为过渡金属中的一种或几种的混合；步骤二，在缓冲气体氛围中，以步骤一所得石墨棒为阳极，在电弧室中发生电弧放电，得到非晶碳包裹单壁碳纳米管线。本发明的方法工艺简单，制备的非晶碳包裹单壁碳纳米管线纯度高，表面光滑，长径比可达10～100。
An amorphous carbon-wrapped single-wall carbon nanotube wire in the technical field of nanomaterials and a preparation method thereof; the amorphous carbon-wrapped single-wall carbon nanotube wire consists of a shell made of amorphous carbon and a single-wall carbon nanotube wrapped in the shell Composition; its preparation method comprises the following steps: Step 1, catalyst and graphite powder are mixed, prepare graphite rod; Described catalyst is the mixing of one or several kinds of transition metals; Step 2, in buffer gas atmosphere, with step The obtained graphite rod is used as an anode, and an arc discharge occurs in an arc chamber to obtain single-walled carbon nanotubes wrapped in amorphous carbon. The method of the invention has simple process, and the prepared amorphous carbon-wrapped single-wall carbon nanotube line has high purity, smooth surface, and the length-to-diameter ratio can reach 10-100.
Description
Technical field
The present invention relates to Single Walled Carbon Nanotube line of a kind of technical field of nano material and preparation method thereof, specifically is a kind of amorphous carbon coated single-walled carbon nano tube line and preparation method thereof.
Background technology
Carbon nanotube (Carbon nanotubes; CNT) after being found in 1991, just caused the extensive concern of scientific circles.Because it has unique accurate one-dimentional structure and excellent electric property and mechanical property, and be widely used in nanometer electronic device, a lift-off technology, biological medicine carrying, hydrogen storage technology or the like numerous areas tool.Carbon nanotube can be divided into single ancient piece of jade, round, flat and with a hole in its centre carbon nanotube (SWNT), two ancient piece of jade, round, flat and with a hole in its centre carbon nanotube (DWNT), multi-walled carbon nano-tubes (MWNT).Wherein single ancient piece of jade, round, flat and with a hole in its centre carbon nanotube is as good monodimension nanometer material, be used as nanometer electronic devices such as making field-effect transistor, thin film transistor because of it has higher carrier mobility, be expected to replace silicon materials and the critical material that becomes microelectronic device of future generation.The main technology of preparing of current preparation carbon nanotube is arc discharge method (DC arc discharge), chemical Vapor deposition process (CVD) and laser ablation method.Wherein arc discharge method (Takikawa, H.Journal of the Vacuum Society of Japan, 2008, Vol.51, P.240～244) is the main method for preparing the high quality Single Walled Carbon Nanotube at present.Arc discharge method is meant in the reaction cavity that is filled with certain gas (rare gas element or contain the mixed gas of activated gas), two over against between Graphite Electrodes (wherein containing catalyzer in the graphite anode rod) arc-over take place under certain voltage, carbon atom is reset under high temperature and catalyst action and is formed hollow tubular product, i.e. carbon nanotube.Since carbon nanotube was found, a lot of scientists had carried out big quantity research, carbon nano tube growth mechanism especially along its length to the growth mechanism of carbon nanotube.The growth model of relatively generally acknowledging is gas-liquid-solid (VLS) model at present, be to be in the gasiform carbon atom under the high temperature to form eutectic with the melted catalyst effect, oversaturated carbon atom is separated out on the liquid phase surface of eutectic, and then cooling back nucleation (solid phase), thereby grow into carbon nanotube, but lack research along the growth mechanism on the diametric(al) for carbon nanotube.
Find through literature search, do not find the report relevant as yet with amorphous carbon coated single-walled carbon nano tube line of the present invention and preparation method thereof to prior art.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of amorphous carbon coated single-walled carbon nano tube line and preparation method thereof is provided.Method technology of the present invention is simple, the amorphous carbon coated single-walled carbon nano tube line purity height of preparation, and smooth surface, length-to-diameter ratio can reach 10～100.
The present invention realizes by following technical scheme,
The present invention relates to a kind of amorphous carbon coated single-walled carbon nano tube line, form by decolorizing carbon shell that constitutes and the Single Walled Carbon Nanotube that is wrapped in this shell.
Described Single Walled Carbon Nanotube is one or more.
The preparation method of described amorphous carbon coated single-walled carbon nano tube line comprises the steps:
Step 1 is mixed catalyzer with Graphite Powder 99, the preparation graphite rod;
Described catalyzer is one or more the mixing in the transition metal;
Step 2 in the buffer gas atmosphere, is an anode with step 1 gained graphite rod, and arc-over takes place in arc chamber, obtains amorphous carbon coated single-walled carbon nano tube line.
In the step 1, the molar content 1%～6% of catalyzer in the described graphite rod.
In the step 1, described catalyzer is one or more the mixing in the following combination: iron, cobalt, nickel and yttrium.
In the step 2, in the described arc-over, the anodic diameter is (1～5) with the ratio of the diameter of negative electrode: 1.
In the step 2, described buffer gas is one or more the mixing in the following combination: helium, argon and hydrogen.
In the step 2, the air pressure of described buffer gas is 20～80KPa.
In the step 2, described arc-over is specially: voltage is 40～80V, electric current 60～120A.
Compared with prior art, the present invention has following beneficial effect: method technology of the present invention is simple, the amorphous carbon coated single-walled carbon nano tube line purity height of preparation, and smooth surface, length-to-diameter ratio can reach 10～100.
Description of drawings
Fig. 1 is the structural representation of amorphous carbon coated single-walled carbon nano tube line;
Fig. 2 is scanning electron microscope (SEM) photo of the amorphous carbon coated single-walled carbon nano tube line of embodiment 1 preparation;
Fig. 3 is projection Electronic Speculum (TEM) photo of the amorphous carbon coated single-walled carbon nano tube line of embodiment 1 preparation;
Fig. 4 is the Raman spectrogram of the amorphous carbon coated single-walled carbon nano tube line of embodiment 1 preparation.
Embodiment
Following example will the invention will be further described in conjunction with the accompanying drawings.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1
Step 1 is that 94.8: 4.2: 1 ratio is got following material: high purity graphite powder, Ni powder and Y according to the mol ratio of C: Ni: Y
2O
3Powder is dosed into 25wt% coal tar after mixing, it is the rod of 40mm that extrusion becomes diameter; Then rod is put into the High Temperature Furnaces Heating Apparatus of nitrogen protection and handled 3 hours for 900 ℃, promptly make graphite rod;
Step 2, arc-over carries out in the arc chamber that is connected with the 80KPa helium, and the negative electrode diameter is 8mm, and discharging current is 60～70A, and voltage is 40～50V, be 30 minutes discharge time, makes about 0.2g amorphous carbon coated single-walled carbon nano tube line.
Fig. 2, Fig. 3 are respectively SEM, the TEM photo of prepared product, and as can be seen from the figure the diameter of amorphous carbon coated single-walled carbon nano tube line is at 30～50nm, smooth surface.Can find out that from TEM figure carbon nano tube surface wrapped up by decolorizing carbon, its structural representation as shown in Figure 1.Fig. 4 is the Raman spectrogram of prepared product, as can be seen from the figure is positioned at 1340cm
-1Near D peak almost disappears, and illustrates that prepared amorphous carbon coated single-walled carbon nano tube line purity is higher.
Embodiment 2
Step 1 is that 99: 1 ratio is got following material according to the mol ratio of C: Fe: high purity graphite powder, Fe powder, dose into 25wt% coal tar after mixing, and it is the rod of 20mm that extrusion becomes diameter; Then rod is put into the High Temperature Furnaces Heating Apparatus of nitrogen protection and handled 3 hours for 900 ℃, promptly make graphite rod;
Step 2, arc-over carries out in the arc chamber that is connected with 12KPa hydrogen and 18KPa argon gas, and the negative electrode diameter is 8mm, and discharging current is 70～80A, and voltage is 40～50V, be 30 minutes discharge time, makes about 0.25g amorphous carbon coated single-walled carbon nano tube line.
Embodiment 3
Step 1, be 94: 4: 1 according to the mol ratio of C: Ni: Co: Fe: 1 ratio is got following material: high purity graphite powder, Ni powder, Co powder, Fe powder, dose into 25wt% coal tar after mixing, it is the rod of 35mm that extrusion becomes diameter; Then rod is put into the High Temperature Furnaces Heating Apparatus of nitrogen protection and handled 3 hours for 900 ℃, promptly make graphite rod;
Step 2, arc-over carries out in the arc chamber that is connected with 24KPa hydrogen and 36KPa argon gas, and the negative electrode diameter is 8mm, and discharging current is 110～120A, and voltage is 70～80V, be 50 minutes discharge time, makes about 0.5g amorphous carbon coated single-walled carbon nano tube line.
Embodiment 4
Step 1 is that 94.8: 4.2: 1 ratio is got following material: high purity graphite powder, Ni powder, Y according to the mol ratio of C: Ni: Y
2O
3Powder is dosed into 25wt% coal tar after mixing, it is the rod of 8mm that extrusion becomes diameter; Then rod is put into the High Temperature Furnaces Heating Apparatus of nitrogen protection and handled 3 hours for 900 ℃, promptly make graphite rod;
Step 2, arc-over carries out in the arc chamber that is connected with the 20KPa helium, and the negative electrode diameter is 8mm, and discharging current is 80～90A, and voltage is 60～70V, be 20 minutes discharge time, makes about 0.15g amorphous carbon coated single-walled carbon nano tube line.
Claims (4)
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