CN102070139A - V-shaped flame burner and method for synthesizing carbon nanotube array - Google Patents
V-shaped flame burner and method for synthesizing carbon nanotube array Download PDFInfo
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- CN102070139A CN102070139A CN2010105724196A CN201010572419A CN102070139A CN 102070139 A CN102070139 A CN 102070139A CN 2010105724196 A CN2010105724196 A CN 2010105724196A CN 201010572419 A CN201010572419 A CN 201010572419A CN 102070139 A CN102070139 A CN 102070139A
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Abstract
The invention discloses a V-shaped flame burner and a method for synthesizing a carbon nanotube array, belonging to the technical field of carbon nanotube synthesis. In the invention, reactive gas passes through a central tube of the V-shaped burner to enter a reaction zone of a V-shaped port with inert gas, a sampling substrate sputtered with a catalyst coating layer is put at an outlet of the V-shaped burner, and after being heated for 3 minutes-5 minutes, the carbon nanotube array can be obtained on the sampling substrate. In the invention, the used equipment is simple, the operation is simple and easy, flame is directly adopted for heating in atmosphere, the energy utilization ratio is high, and a continuous conveying belt sampling mechanism is adopted, so that the carbon nanotube array with high efficiency, continuous batch and a low cost is prepared.
Description
Technical field
The invention belongs to the carbon nanotube synthesis technical field, be specifically related to the method for a kind of V-flame burner and synthesizing carbon nanotubes array thereof.
Background technology
Carbon nanotube (Carbon Nanotube, CNT) by one deck or multilayer graphite curl according to certain helix angle form, diameter is nano level tubular nanometer material.The accurate 1-dimention nano new carbon of carbon nanotube has unique electricity, chemistry and mechanical property.The intensity that studies show that CNT is about 100 times of steel, and density has only the sixth of steel.The resistance of CNT is 4.2～190k Ω/μ m, and its axial thermal conductivity is up to 6600W/ (mK), exceeds 1 order of magnitude than the thermal conductivity of metal, with thermal conductivity best material diamond is suitable up to now; CNT has the electronic structure of enriching, and is one of most promising components and parts of microelectronics of future generation.But disorderly and unsystematic, the mutual winding of free growing carbon nanotube has limited the application and development of carbon nanotube, particularly the application aspect device.And aspects such as directional carbon nanotube array emission on the scene, electrode materials, super capacitor, transmitter have shown preferable performance, are the gordian techniquies of making based on the Field Emission Display of carbon nanotube.Therefore, realize efficient, the continuous batch of carbon nano pipe array, the low-cost carbon nanotube key in application that becomes.
Synthesis method representative studies for carbon nano pipe array mainly contains more following at present:
Separate and think to wait deeply (Li W Z, Xie S S, Qian L X, et al.Science, 1996,274:1701～1703) to propose to utilize the method for duct restriction CNT orientation to prepare carbon nano pipe array.They are by adopting the method for collosol and gel, in the gel that the iron catalyst particles dispersed is formed to teos hydrolysis, feed acetylene gas then, and the employing controlled temperature is 700 ℃ a chemical vapor deposition processes, it is spacing to be dispersed in nano level iron catalyst particle in the duct catalytic synthesis of C nanotube and passing hole channel in a suitable temperature window, make the CNT oriented growth, thereby obtain the very big carbon nano pipe array of length-to-diameter ratio.(Ren Z F such as Ren, HuangZ P, Xu JW, et al.Science, 1998,282 (5391): 1105～1107) method of the Ti Chuing nickel film of sputter last layer 15nm～60nm on glass substrate at first, the etching through ammonia obtains the dispersed catalyst particle again, be that carbon source is passed through plasma enhanced chemical vapor deposition then with acetylene, under 660 ℃, prepare directed array of multi-walled carbon nanotubes perpendicular to glass surface.Isoionicly induce oriented growth to play promoter action to CNT.(Melechko A V such as Fan Shoushan, MerkulovV I, McKnightT E, et al.Journalof Applied Physics, 2005,97 (4): 104～130) utilize the film catalytic coking to learn vapour deposition first and successfully prepared array of multi-walled carbon nanotubes, this method at first obtains porous silicon with the galvanic corrosion monocrystalline silicon piece, obtain the iron catalyst film of 5nm then by electron beam evaporation plating at porous silicon surface, after air atmosphere annealing forms granules of catalyst, with acetylene is carbon source, and temperature of reaction is 700 ℃, has grown the array of multi-walled carbon nanotubes perpendicular to substrate surface in the thermal chemical vapor deposition stove.
But the method for above synthesizing carbon nanotubes array mostly adopts chemical gaseous phase depositing process, and institute's employing equipment is all comparatively expensive, and reactions steps is comparatively complicated.Up to now, the mode that does not still have efficient, continuous batch, low-cost synthesizing carbon nanotubes array.The present invention protects the people, the Zhao Huifu (patent No.: PNCN1830770-A) provide a kind of novel method of V-flame synthesizing carbon nanotubes array on the burner of V-type of Ti Chuing and pyramid type pyrolysis flame synthesizing carbon nanotubes and the synthetic method basis grandson in 2006.
Summary of the invention
The object of the present invention is to provide a kind of V-flame burner.
The object of the present invention is to provide a kind of method of V-flame synthesizing carbon nanotubes array.
A kind of V-flame burner is characterized in that, described burner mainly is made up of V-type isosceles body 1, rectangular centre pipe 2, external flame spout 3, sampling substrate 4; V-type isosceles body 1 both sides are set to opening, and bottom and rectangular centre pipe 2 join; External flame spout 3 and the parallel placement in rectangular centre pipe 2 left and right sides; Sampling substrate (4) places V-type isosceles body central authorities by the direction perpendicular to rectangular centre pipe (2).
Described sampling substrate (4) is made of polishing monocrystalline silicon piece or the quartz plate of coating buffer coating and catalyst coat in the mode of magnetron sputtering successively.
Described buffer coating is that pure aluminum, catalyst coat are fe, elemental nickel or simple substance cobalt.
A kind of method of V-flame synthesizing carbon nanotubes array is characterized in that, may further comprise the steps:
(1) at first, with the igniting of V-type burner, flammable premixed gas is from the ejection of V-type external body flame jet, and stable burning, and the V-type mouth is heated, and the synthetic high temperature heat source that provides of carbon nano pipe array is provided;
(2) secondly, feed the reactant mixed gas, comprise reactant gases, assist gas and rare gas element, the synthetic carbon source that provides of carbon nano pipe array is provided to the rectangular centre pipe;
(3) last, the sampling substrate is put in the V-type exit of burner, take off behind heating 3～5min, obtain carbon nano pipe array.
The premix gas that described flammable premixed gas is geseous fuel and air or oxygen.
Described geseous fuel is acetylene, ethene or methane gas.
Described reactant gases is carbon monoxide, methane or acetylene, and assist gas is a hydrogen, and rare gas element is argon, helium or nitrogen.
Fire the severe degree that oxygen is recently regulated flame by regulating, thereby change V-type mouth sampling area temperature.
Beneficial effect of the present invention: 1, the present invention directly adopts flame as thermal source, has improved the heating rate and the capacity usage ratio of reaction, has reduced reaction times and energy consumption.2, owing to be open reactive, the present invention can adopt the continuous conveyor sampling mechanism, realizes that carbon nano-pipe array is listed in the continuous growth on the substrate, accomplishes that continuous batch prepares carbon nano pipe array.3, the V-flame that provides of present method flame heating and carbon nanotube building-up process separately, thereby avoided the carbon source of the affluence in the fuel to cause the generation of a large amount of carbon blacks and Nano capsule, can synthesize higher-quality carbon nano pipe array efficiently.4, all price is cheap for equipment of the present invention, carbon source, thermal source, catalyzer etc., and operation is simple, and the capacity usage ratio height can be realized the large-scale industrial production carbon nano pipe array.
Description of drawings
Fig. 1 is a V-flame burner tomograph of the present invention;
Fig. 2 is a V-flame burner principle schematic of the present invention;
Number in the figure: 1-V type isosceles body; 2-rectangular centre pipe; 3-external flame spout; The 4-substrate of taking a sample; 5-flame; The flammable premixed gas of 6-; 7-reactant mixed gas;
Fig. 3 is the scanning electron microscope picture of the carbon nano pipe array that adopts the inventive method and obtain, and magnification is 10000 times;
Fig. 4 is the scanning electron microscope picture of the carbon nano pipe array that adopts the inventive method and obtain, and magnification is 20000 times.
Embodiment
Below in conjunction with the drawings and specific embodiments the specific embodiment of the present invention is further described:
Embodiment 1:
A kind of V-flame burner of the present invention mainly is made up of V-type isosceles body 1, rectangular centre pipe 2, external flame spout 3, sampling substrate 4; V-type isosceles body 1 both sides are set to opening, and bottom and rectangular centre pipe 2 join; External flame spout 3 and the parallel placement in rectangular centre pipe 2 left and right sides (Fig. 1, Fig. 2); Pass through magnetron sputtering at polishing monocrystalline silicon piece or quartz plate surface, plate the aluminium Al of one deck 20～50nm and the iron Fe of 5～10nm successively, make the sampling substrate; The substrate (4) of will taking a sample places V-type isosceles body central authorities by the direction perpendicular to rectangular centre pipe (2).
The present invention utilizes said burner synthesizing carbon nanotubes array, and operation steps is:
(1) at first, with the igniting of V-type burner, the flammable premixed gas that acetylene and oxygen are formed is from the ejection of V-type external body flame jet, and stable burning, and the V-type mouth is heated, and the synthetic high temperature heat source that provides of carbon nano pipe array is provided; Fire the severe degree that oxygen is recently regulated flame by regulating, thereby change V-type mouth sampling area temperature (550～700 ℃);
(2) secondly, feed methane, hydrogen and nitrogen, the synthetic carbon source that provides of carbon nano pipe array is provided to the rectangular centre pipe;
(3) last, the sampling substrate is put in the V-type exit of burner, take off behind heating 3～5min, obtain carbon nano pipe array.
The carbon nano pipe array ultrastructure that this product is made as shown in Figure 3 and Figure 4.
Claims (8)
1. a V-flame burner is characterized in that, described burner mainly is made up of V-type isosceles body (1), rectangular centre pipe (2), external flame spout (3), sampling substrate (4); V-type isosceles body (1) both sides are set to opening, and bottom and rectangular centre pipe (2) join; External flame spout (3) and the parallel placement in rectangular centre pipe (2) left and right side; Sampling substrate (4) places V-type isosceles body central authorities by the direction perpendicular to rectangular centre pipe (2).
2. according to the described a kind of V-flame burner of claim 1, it is characterized in that described sampling substrate (4) is made of polishing monocrystalline silicon piece or the quartz plate of coating buffer coating and catalyst coat in the mode of magnetron sputtering successively.
3. according to the described a kind of V-flame burner of claim 2, it is characterized in that described buffer coating is that pure aluminum, catalyst coat are fe, elemental nickel or simple substance cobalt.
4. the method for a V-flame synthesizing carbon nanotubes array is characterized in that, may further comprise the steps:
(1) at first, with the igniting of V-type burner, flammable premixed gas is from the ejection of V-type external body flame jet, and stable burning, and the V-type mouth is heated, and the synthetic high temperature heat source that provides of carbon nano pipe array is provided;
(2) secondly, feed the reactant mixed gas, comprise reactant gases, assist gas and rare gas element, the synthetic carbon source that provides of carbon nano pipe array is provided to the rectangular centre pipe;
(3) last, the sampling substrate is put in the V-type exit of burner, take off behind heating 3～5min, obtain carbon nano pipe array.
5. according to the method for the described a kind of V-flame synthesizing carbon nanotubes array of claim 4, it is characterized in that the premix gas that described flammable premixed gas is geseous fuel and air or oxygen.
6. according to the method for the described a kind of V-flame synthesizing carbon nanotubes array of claim 5, it is characterized in that described geseous fuel is acetylene, ethene or methane gas.
7. according to the method for the described a kind of V-flame synthesizing carbon nanotubes array of claim 4, it is characterized in that described reactant gases is carbon monoxide, methane or acetylene, assist gas is a hydrogen, and rare gas element is argon, helium or nitrogen.
8. according to the method for the described a kind of V-flame synthesizing carbon nanotubes array of claim 5, it is characterized in that, fire the severe degree that oxygen is recently regulated flame, thereby change V-type mouth sampling area temperature by regulating.
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| CN110219052A (en) * | 2019-05-31 | 2019-09-10 | 南京理工大学 | A kind of ultra thin single crystalline Zn3(OH)4(NO3)2Hydroxyl zinc nitrate nanometer sheet of structure and preparation method thereof |
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| CN110219052A (en) * | 2019-05-31 | 2019-09-10 | 南京理工大学 | A kind of ultra thin single crystalline Zn3(OH)4(NO3)2Hydroxyl zinc nitrate nanometer sheet of structure and preparation method thereof |
| CN110219052B (en) * | 2019-05-31 | 2021-09-03 | 南京理工大学 | Ultrathin single crystal Zn3(OH)4(NO3)2Hydroxyl zinc nitrate nanosheet with structure and preparation method thereof |
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Application publication date: 20110525 |