CN104787749B - A kind of preparation method of aligned carbon nanotube - Google Patents
A kind of preparation method of aligned carbon nanotube Download PDFInfo
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- CN104787749B CN104787749B CN201510218668.8A CN201510218668A CN104787749B CN 104787749 B CN104787749 B CN 104787749B CN 201510218668 A CN201510218668 A CN 201510218668A CN 104787749 B CN104787749 B CN 104787749B
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Abstract
The preparation method that the invention discloses a kind of aligned carbon nanotube, the method is: one, by clean for silicon chip ethanol purge post-drying, then adopts coater silicon chip surface plated film after the drying, and Coating Materials is FeNi powders；Two, the silicon chip after plated film is placed in oxidation furnace, oxidation processes 30min～60min under oxidizing atmosphere；Three, the silicon chip after oxidation processes is placed in tube furnace, pass into nitrogen and heat up, when furnace temperature rises to 600 DEG C～800 DEG C, nitrogen is changed into hydrogen, acetylene and hydrofluoric mixing gas, and under heat-retaining condition, pulsed magnetic field is applied to described tube furnace both sides, ventilation and heating is stopped after 10min～30min, simultaneously close off pulsed magnetic field, take out silicon chip after furnace cooling, obtain aligned carbon nanotube at silicon chip surface.Adopting carbon nano-tube oriented property prepared by the method for the present invention good, preparation speed is fast, and yield is high.
Description
Technical field
The invention belongs to carbon nanotube preparation technology field, the preparation method being specifically related to a kind of aligned carbon nanotube.
Background technology
CNT is curling and formed by single or multiple lift graphite flake, and its diameter is generally tens nanometers, a few to tens of microns of length, and unique microstructure determines its good electrical property, excellent heat conductivility and superpower comprehensive mechanical performance.The performance of these excellences makes CNT have many potential purposes.CNT can apply to the reinforcement of composite because of high specific strength, high length-diameter ratio, good electric conductivity makes it the good material of the probe of atomic force microscope and PSTM, and good characteristic of semiconductor makes CNT may be used for manufacturing the wire of diode, audion, unimolecular switch, mnemon and molecular circuit；The light transfer characteristic utilizing CNT can also manufacture solaode light and handy, cheap, efficient.The electron emission characteristic that CNT is very strong makes it may be used for manufacturing giant-screen, ultra-thin, fine definition, high brightness, energy-conservation, long-life flexible display screen.But, the CNT disordered arrangements prepared by the preparation method commonly used at present, and be mutually wound around, have impact on the CNT deep development in use above field and perfect.Therefore orientational alignment carbon nano-tube is the important prerequisite realizing its practical application, is also the main bugbear realizing its practical application.
The CNT tube bank aligned at present and the preparation method of array are essentially divided into two classes: a class is growth control methods, refer in preparation, growth course by controlling the distribution of catalyst, using the physical influence of template to make the growth of carbon pipe have directivity.Another kind of method is subsequent transformation method, it is exactly make the CNT prepared redirect arrangement in physical field (liquid or gas flowfield, the field of force, high-intensity magnetic field, electric field), owing to adopting the CNT prepared as precursor, in the process of preparation, CNT has created mutual winding, therefore the effect that the solution of CNT was twined and redirected arrangement by the processing method in later stage is adopted to be extremely limited, particularly that the effect of the relatively larger CNT of major diameter is more faint.Therefore the method for aligned carbon nanotube is prepared still with Growth Control method for major way.
The method realizing oriented growth of carbon nanometer tube at present mainly has following several diverse ways: hot CVD (ThermalCVD), microwave plasma enhanced MPECVD (MicrowavePlasma-enhancedCVD), back bias voltage strengthen hot filament NBECVD (NegativeBias-enhancedCVD) and electron cyclotron resonace ECRCVD (ElectronCyclotronResonanceCVD).These preparation methoies still have certain defect, first the carbon nano-tube oriented property that prepared by thermal cvd and MPECVD method is not obvious especially, and the sample of preparation still has obvious wrapping phenomena, and the directionality of NBECVD and ECRCVD is better, but preparation speed is relatively slow, and yield is relatively low.
Summary of the invention
The technical problem to be solved is in that for above-mentioned the deficiencies in the prior art, it is provided that the preparation method of a kind of aligned carbon nanotube.The method adopts silicon chip as supporting carrier, with FeNi powders for Coating Materials at silicon chip surface plated film, and the silicon chip after plated film is aoxidized, silicon chip surface major part ferrum is made to be oxidized to ferromagnetic ferroso-ferric oxide, thus improving the ability receiving pulsed magnetic field, nickel in FeNi powders can decompose the acetylene passing in tube furnace as catalyst, and the growth for CNT provides carbon source；In tube furnace, pass into hydrogen, acetylene and hydrofluoric mixing gas, owing to fluorine atom has stronger electronegativity, ligand can be formed with ferroso-ferric oxide, be formed in nickel catalyst surface sterically hindered, the direction of growth of restriction CNT；Apply pulsed magnetic field to tube furnace both sides simultaneously, it is possible to anti-blocking arbitrarily spread growth, thus ensureing the oriented growth of CNT and the uniform of caliber.
For solving above-mentioned technical problem, the technical solution used in the present invention is: the preparation method of a kind of aligned carbon nanotube, it is characterised in that comprise the following steps:
Step one, by clean for silicon chip ethanol purge post-drying, then adopting coater silicon chip surface plated film after the drying, Coating Materials is FeNi powders, and the temperature of plated film is 1000 DEG C～1200 DEG C, the pressure of plated film is 0.000001Pa～0.001Pa, and the time of plated film is 10min～30min；
Step 2, being placed in oxidation furnace by the silicon chip after plated film in step one, under oxidizing atmosphere, temperature is 300 DEG C～400 DEG C, oxidation processes 30min～60min when pressure is 1Pa～5Pa；Described oxidizing atmosphere is the mixing gas of oxygen and nitrogen, and wherein the volumn concentration of oxygen is 2%～5%；
Step 3, the silicon chip after oxidation processes in step 2 is placed in tube furnace, in described tube furnace, pass into nitrogen and tube furnace is heated up, when the furnace temperature of described tube furnace rises to 600 DEG C～800 DEG C, nitrogen is changed into hydrogen, acetylene and hydrofluoric mixing gas, and under heat-retaining condition, pulsed magnetic field is applied to described tube furnace both sides, ventilation and heating is stopped after 10min～30min, simultaneously close off pulsed magnetic field, take out silicon chip after furnace cooling, obtain aligned carbon nanotube at silicon chip surface；In described hydrogen, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 50%～80%, and hydrofluoric volumn concentration is 0.5%～1%.
The preparation method of above-mentioned a kind of aligned carbon nanotube, it is characterised in that in FeNi powders described in step one, the weight/mass percentage composition of nickel is 33.5%～41%.
The preparation method of above-mentioned a kind of aligned carbon nanotube, it is characterised in that the speed heated up described in step 3 is 5 DEG C/min～10 DEG C/min.
The preparation method of above-mentioned a kind of aligned carbon nanotube, it is characterised in that in hydrogen described in step 3, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 60%～70%, and hydrofluoric volumn concentration is 0.5%～1%.
The preparation method of above-mentioned a kind of aligned carbon nanotube, it is characterised in that the magnetic field intensity of pulsed magnetic field described in step 3 is 1.5T～2.5T, pulse frequency is 10Hz～1000Hz.
The present invention compared with prior art has the advantage that
1, the present invention adopts silicon chip as supporting carrier, with FeNi powders for Coating Materials at silicon chip surface plated film, and the silicon chip after plated film is aoxidized, silicon chip surface major part ferrum is made to be oxidized to ferromagnetic ferroso-ferric oxide, thus improving the ability receiving pulsed magnetic field, nickel in FeNi powders can decompose the acetylene passing in tube furnace as catalyst, and the growth for CNT provides carbon source.
2, the present invention passes into hydrogen, acetylene and hydrofluoric mixing gas in tube furnace, owing to fluorine atom has stronger electronegativity, can form ligand with ferroso-ferric oxide, be formed in nickel catalyst surface sterically hindered, the direction of growth of restriction CNT；Apply pulsed magnetic field to tube furnace both sides simultaneously, it is possible to anti-blocking arbitrarily spread growth, thus ensureing the oriented growth of CNT and the uniform of caliber.
3, adopting carbon nano-tube oriented property prepared by the method for the present invention good, preparation speed is fast, and yield is high.
By the examples below, technical scheme is described in further detail.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the aligned carbon nanotube of the embodiment of the present invention 1 preparation.
Fig. 2 is the SEM figure of CNT prepared by conventional method.
Detailed description of the invention
Embodiment 1
The preparation method of the present embodiment comprises the following steps:
Step one, by clean for silicon chip ethanol purge post-drying, then adopt coater silicon chip surface plated film after the drying, Coating Materials is FeNi powders, and the temperature of plated film is 1000 DEG C, and the pressure of plated film is 0.000001Pa, and the time of plated film is 30min；In described FeNi powders, the weight/mass percentage composition of nickel is 33.5%；
Step 2, being placed in oxidation furnace by the silicon chip after plated film in step one, under oxidizing atmosphere, temperature is 300 DEG C, oxidation processes 30min when pressure is 1Pa；Described oxidizing atmosphere is the mixing gas of oxygen and nitrogen, and wherein the volumn concentration of oxygen is 2%；
Step 3, the silicon chip after oxidation processes in step 2 is placed in tube furnace, in described tube furnace, pass into nitrogen and tube furnace is heated up, the speed heated up is 5 DEG C/min, when the furnace temperature of described tube furnace rises to 600 DEG C, nitrogen is changed into hydrogen, acetylene and hydrofluoric mixing gas, and under heat-retaining condition, pulsed magnetic field is applied to described tube furnace both sides, ventilation and heating is stopped after 10min, simultaneously close off pulsed magnetic field, take out silicon chip after furnace cooling, obtain aligned carbon nanotube at silicon chip surface；In described hydrogen, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 50%, and hydrofluoric volumn concentration is 0.5%, and surplus is acetylene；The magnetic field intensity of described pulsed magnetic field is 1.5T, and pulse frequency is 10Hz.
Comparison diagram 1 and Fig. 2 are it can be seen that adopt carbon nano tube growth direction prepared by conventional method disorderly and unsystematic, and are mutually wound around.And adopt CNT prepared by the method for the present embodiment to have good oriented growth, and mutually significantly it is not wound around.The average length of CNT prepared by the present embodiment 3.5 μm, twine rate is 7.5%.
Embodiment 2
The preparation method of the present embodiment comprises the following steps:
Step one, by clean for silicon chip ethanol purge post-drying, then adopt coater silicon chip surface plated film after the drying, Coating Materials is FeNi powders, and the temperature of plated film is 1050 DEG C, and the pressure of plated film is 0.00001Pa, and the time of plated film is 25min；In described FeNi powders, the weight/mass percentage composition of nickel is 35%；
Step 2, being placed in oxidation furnace by the silicon chip after plated film in step one, under oxidizing atmosphere, temperature is 320 DEG C, oxidation processes 35min when pressure is 2Pa；Described oxidizing atmosphere is the mixing gas of oxygen and nitrogen, and wherein the volumn concentration of oxygen is 2%；
Step 3, the silicon chip after oxidation processes in step 2 is placed in tube furnace, in described tube furnace, pass into nitrogen and tube furnace is heated up, the speed heated up is 10 DEG C/min, when the furnace temperature of described tube furnace rises to 650 DEG C, nitrogen is changed into hydrogen, acetylene and hydrofluoric mixing gas, and under heat-retaining condition, pulsed magnetic field is applied to described tube furnace both sides, ventilation and heating is stopped after 15min, simultaneously close off pulsed magnetic field, take out silicon chip after furnace cooling, obtain aligned carbon nanotube at silicon chip surface；In described hydrogen, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 60%, and hydrofluoric volumn concentration is 0.5%；The magnetic field intensity of described pulsed magnetic field is 1.7T, and pulse frequency is 100Hz.
The average length of CNT prepared by the present embodiment 4.7 μm, twine rate is 8.5%.
Embodiment 3
The preparation method of the present embodiment comprises the following steps:
Step one, by clean for silicon chip ethanol purge post-drying, then adopt coater silicon chip surface plated film after the drying, Coating Materials is FeNi powders, and the temperature of plated film is 1100 DEG C, and the pressure of plated film is 0.0001Pa, and the time of plated film is 20min；In described FeNi powders, the weight/mass percentage composition of nickel is 39%；
Step 2, being placed in oxidation furnace by the silicon chip after plated film in step one, under oxidizing atmosphere, temperature is 360 DEG C, oxidation processes 60min when pressure is 1Pa；Described oxidizing atmosphere is the mixing gas of oxygen and nitrogen, and wherein the volumn concentration of oxygen is 2%；
Step 3, the silicon chip after oxidation processes in step 2 is placed in tube furnace, in described tube furnace, pass into nitrogen and tube furnace is heated up, the speed heated up is 8 DEG C/min, when the furnace temperature of described tube furnace rises to 700 DEG C, nitrogen is changed into hydrogen, acetylene and hydrofluoric mixing gas, and under heat-retaining condition, pulsed magnetic field is applied to described tube furnace both sides, ventilation and heating is stopped after 25min, simultaneously close off pulsed magnetic field, take out silicon chip after furnace cooling, obtain aligned carbon nanotube at silicon chip surface；In described hydrogen, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 80%, and hydrofluoric volumn concentration is 1%；The magnetic field intensity of described pulsed magnetic field is 1.8T, and pulse frequency is 200Hz.
The average length of CNT prepared by the present embodiment 5.5 μm, twine rate is 8.1%.
Embodiment 4
The preparation method of the present embodiment comprises the following steps:
Step one, by clean for silicon chip ethanol purge post-drying, then adopt coater silicon chip surface plated film after the drying, Coating Materials is FeNi powders, and the temperature of plated film is 1150 DEG C, and the pressure of plated film is 0.001Pa, and the time of plated film is 15min；In described FeNi powders, the weight/mass percentage composition of nickel is 41%；
Step 2, being placed in oxidation furnace by the silicon chip after plated film in step one, under oxidizing atmosphere, temperature is 380 DEG C, oxidation processes 45min when pressure is 4Pa；Described oxidizing atmosphere is the mixing gas of oxygen and nitrogen, and wherein the volumn concentration of oxygen is 4%；
Step 3, the silicon chip after oxidation processes in step 2 is placed in tube furnace, in described tube furnace, pass into nitrogen and tube furnace is heated up, the speed heated up is 6 DEG C/min, when the furnace temperature of described tube furnace rises to 750 DEG C, nitrogen is changed into hydrogen, acetylene and hydrofluoric mixing gas, and under heat-retaining condition, pulsed magnetic field is applied to described tube furnace both sides, ventilation and heating is stopped after 28min, simultaneously close off pulsed magnetic field, take out silicon chip after furnace cooling, obtain aligned carbon nanotube at silicon chip surface；In described hydrogen, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 70%, and hydrofluoric volumn concentration is 1%；The magnetic field intensity of described pulsed magnetic field is 2.0T, and pulse frequency is 500Hz.
The average length of CNT prepared by the present embodiment 7.8 μm, twine rate is 8.5%.
Embodiment 5
The preparation method of the present embodiment comprises the following steps:
Step one, by clean for silicon chip ethanol purge post-drying, then adopt coater silicon chip surface plated film after the drying, Coating Materials is FeNi powders, and the temperature of plated film is 1200 DEG C, and the pressure of plated film is 0.001Pa, and the time of plated film is 10min；In described FeNi powders, the weight/mass percentage composition of nickel is 35%；
Step 2, being placed in oxidation furnace by the silicon chip after plated film in step one, under oxidizing atmosphere, temperature is 400 DEG C, oxidation processes 30min when pressure is 5Pa；Described oxidizing atmosphere is the mixing gas of oxygen and nitrogen, and wherein the volumn concentration of oxygen is 5%；
Step 3, the silicon chip after oxidation processes in step 2 is placed in tube furnace, in described tube furnace, pass into nitrogen and tube furnace is heated up, the speed heated up is 10 DEG C/min, when the furnace temperature of described tube furnace rises to 800 DEG C, nitrogen is changed into hydrogen, acetylene and hydrofluoric mixing gas, and under heat-retaining condition, pulsed magnetic field is applied to described tube furnace both sides, ventilation and heating is stopped after 30min, simultaneously close off pulsed magnetic field, take out silicon chip after furnace cooling, obtain aligned carbon nanotube at silicon chip surface；In described hydrogen, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 65%, and hydrofluoric volumn concentration is 0.8%；The magnetic field intensity of described pulsed magnetic field is 2.5T, and pulse frequency is 1000Hz.
The average length of CNT prepared by the present embodiment 11.8 μm, twine rate is 10.7%.
The above; it it is only presently preferred embodiments of the present invention; not the present invention is imposed any restrictions, every any simple modification, change and equivalent structure change above example made according to the technology of the present invention essence, all still fall within the protection domain of technical solution of the present invention.
Claims (5)
1. the preparation method of an aligned carbon nanotube, it is characterised in that comprise the following steps:
Step one, by clean for silicon chip ethanol purge post-drying, then adopting coater silicon chip surface plated film after the drying, Coating Materials is FeNi powders, and the temperature of plated film is 1000 DEG C～1200 DEG C, the pressure of plated film is 0.000001Pa～0.001Pa, and the time of plated film is 10min～30min；
Step 2, being placed in oxidation furnace by the silicon chip after plated film in step one, under oxidizing atmosphere, temperature is 300 DEG C～400 DEG C, oxidation processes 30min～60min when pressure is 1Pa～5Pa；Described oxidizing atmosphere is the mixing gas of oxygen and nitrogen, and wherein the volumn concentration of oxygen is 2%～5%；
Step 3, the silicon chip after oxidation processes in step 2 is placed in tube furnace, in described tube furnace, pass into nitrogen and tube furnace is heated up, when the furnace temperature of described tube furnace rises to 600 DEG C～800 DEG C, nitrogen is changed into hydrogen, acetylene and hydrofluoric mixing gas, and under heat-retaining condition, pulsed magnetic field is applied to described tube furnace both sides, ventilation and heating is stopped after 10min～30min, simultaneously close off pulsed magnetic field, take out silicon chip after furnace cooling, obtain aligned carbon nanotube at silicon chip surface；In described hydrogen, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 50%～80%, and hydrofluoric volumn concentration is 0.5%～1%.
2. the preparation method of a kind of aligned carbon nanotube according to claim 1, it is characterised in that in FeNi powders described in step one, the weight/mass percentage composition of nickel is 33.5%～41%.
3. the preparation method of a kind of aligned carbon nanotube according to claim 1, it is characterised in that the speed heated up described in step 3 is 5 DEG C/min～10 DEG C/min.
4. the preparation method of a kind of aligned carbon nanotube according to claim 1, it is characterized in that, in hydrogen described in step 3, acetylene and hydrofluoric mixing gas, the volumn concentration of hydrogen is 60%～70%, and hydrofluoric volumn concentration is 0.5%～1%.
5. the preparation method of a kind of aligned carbon nanotube according to claim 1, it is characterised in that the magnetic field intensity of pulsed magnetic field described in step 3 is 1.5T～2.5T, pulse frequency is 10Hz～1000Hz.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1547225A (en) * | 2003-12-11 | 2004-11-17 | 中国科学院山西煤炭化学研究所 | Technology and equipment for preparing magnetic carbon nanometer tube by plasma |
| CN1907845A (en) * | 2005-08-05 | 2007-02-07 | 鸿富锦精密工业（深圳）有限公司 | Carbon nano-tube preparation method and apparatus |
| CN1955113A (en) * | 2005-10-28 | 2007-05-02 | 鸿富锦精密工业（深圳）有限公司 | Preparation device and method of carbon nano-tube |
| CN104555989A (en) * | 2015-01-30 | 2015-04-29 | 西安科技大学 | Method for preparing carbon nanotubes by adopting coal tar |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1547225A (en) * | 2003-12-11 | 2004-11-17 | 中国科学院山西煤炭化学研究所 | Technology and equipment for preparing magnetic carbon nanometer tube by plasma |
| CN1907845A (en) * | 2005-08-05 | 2007-02-07 | 鸿富锦精密工业（深圳）有限公司 | Carbon nano-tube preparation method and apparatus |
| CN1955113A (en) * | 2005-10-28 | 2007-05-02 | 鸿富锦精密工业（深圳）有限公司 | Preparation device and method of carbon nano-tube |
| CN104555989A (en) * | 2015-01-30 | 2015-04-29 | 西安科技大学 | Method for preparing carbon nanotubes by adopting coal tar |
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