CN108043345B - Arc discharge device and method for preparing boron nitride nanotube by using same - Google Patents
Arc discharge device and method for preparing boron nitride nanotube by using same Download PDFInfo
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- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0845—Details relating to the type of discharge
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
Abstract
The invention relates to an arc discharge device, which comprises a discharge chamber, a discharge cathode, a discharge anode, a feed hopper and a tungsten filament, wherein the discharge cathode, the discharge anode and the feed hopper are arranged in the discharge chamber, one end of the tungsten filament extends into the discharge chamber, an air suction valve and an air inlet valve are arranged on the discharge chamber, a gap is formed between the discharge cathode and the discharge anode, the feed hopper is positioned above the gap, one end of the discharge cathode is connected with a first conducting rod, one end of the discharge anode is connected with a second conducting rod, the first conducting rod or the second conducting rod is connected with a driving mechanism, the first conducting rod is connected with a load resistor, the load resistor is connected with the negative electrode of a first power supply, the other end of the tungsten filament is connected with the negative electrode of a second power supply, and the positive electrode of the first power supply, the. The invention also relates to a method for preparing the boron nitride nanotube. The invention obviously increases the stability in the arc discharge process, and the prepared boron nitride nanotube has more concentrated product size and more perfect shape compared with the product of the traditional process.
Description
Technical Field
The invention relates to the technical field of thermal plasma and nano materials, in particular to an arc discharge device and a method for preparing a boron nitride nanotube by using the same.
Background
The boron nitride nanotube has excellent characteristics of high Young's modulus, strong oxidation resistance, high hydrogen molecule absorption energy and the like, so that the boron nitride nanotube is often applied to the fields of high-strength synthetic materials and hydrogen storage. Similar to carbon nanotubes, boron nitride nanotubes have several synthetic methods: a plasma technology-based synthesis method, a laser sputtering deposition method, a chemical vapor deposition method and a mechanical ball milling annealing method. The plasma technology-based synthesis method and the laser sputtering deposition method can produce boron nitride nanotubes with higher quality, and thus become the focus of current research. In the synthesis method based on the plasma technology, only near-atmospheric pressure direct current arc discharge and atmospheric pressure/high-voltage radio frequency plasma can synthesize a larger boron nitride nanotube combination. From the practical point of view, the arc method has the greatest advantages of simple structure and low cost of the synthesis equipment.
The traditional arc method for synthesizing the boron nitride nanotube mainly comprises two processes: one method adopts boron-containing compound as electrode, and discharges in nitrogen protective gas; another uses an electrode containing boron nitride composite material and discharges in helium. The traditional preparation method has several obvious defects: firstly, the boron nitride nanotubes synthesized by the two methods almost only exist in cathode sediments, the yield is low, and the subsequent separation and purification are difficult; secondly, the arc discharge cathode and the arc discharge anode both adopt boron-containing compounds, and the preparation of the compound electrodes is difficult, so that the production cost of the boron nitride nanotube is greatly increased.
Disclosure of Invention
The invention overcomes the defects of the prior art, and provides the arc discharge device which reduces the cost and improves the working efficiency and the method for preparing the boron nitride nanotube by using the device
In order to achieve the purpose, the invention adopts the technical scheme that: the utility model provides an arc discharge device, includes the discharge chamber, locates discharge cathode, discharge anode, loading hopper and one end in the discharge chamber stretch into tungsten filament in the discharge chamber, be provided with bleeder valve and admission valve on the discharge chamber, discharge cathode and discharge have the clearance between the positive pole, the loading hopper is located the top in clearance, the one end of discharge cathode is connected with first conducting rod, the one end of discharge anode is connected with the second conducting rod, first conducting rod or second conducting rod are connected with actuating mechanism, first conducting rod is connected with load resistance, load resistance is connected with the negative pole of first power, the other end of tungsten filament is connected with the negative pole of second power, the positive pole of positive pole, second conducting rod and the second power of first power all is connected with ground.
A method of making boron nitride nanotubes using the apparatus, comprising the steps of:
(1) tungsten is used as a discharge cathode, and boron is used as a discharge anode;
(2) the loading hopper is in a closed state, and the catalyst is filled into the loading hopper;
(3) sealing the discharge chamber, pumping out air in the discharge chamber to background vacuum, introducing nitrogen, and regulating the air pumping valve and air inlet valve to maintain the air pressure in the discharge chamber at 3 × 104Pa -7×104Pa；
(4) The discharge cathode is contacted with the discharge anode by using a driving mechanism, the current of a first power supply is increased to 35-45A, and the discharge cathode and the discharge anode are heated;
(5) after heating for 0.5-1.5min, separating the discharge cathode and the discharge anode, adjusting the voltage of the second power supply to 2000-2500V, igniting the tungsten filament between the discharge cathode and the discharge anode and exciting an electric arc between the discharge cathode and the discharge anode, and immediately closing the second power supply after the arc striking is finished;
(6) in the arc discharge process, opening a charging hopper to allow a catalyst to enter between a discharge cathode and a discharge anode;
(7) and products are formed on the surface of the discharge cathode and the inner wall of the discharge cavity after the discharge is finished.
In a preferred embodiment of the present invention, the method for preparing boron nitride nanotubes further comprises the step (1) wherein the discharge cathode is cylindrical, has a diameter of 5-7mm and a length of 50-130 mm.
In a preferred embodiment of the present invention, the method for preparing boron nitride nanotubes further comprises the step (1) wherein the discharge anode is cylindrical, has a diameter of 8-12mm and a length of 10-25 mm.
In a preferred embodiment of the present invention, the method for preparing boron nitride nanotubes further comprises, in the step (2), a catalyst comprising cobalt powder and nickel powder, wherein the cobalt powder and the nickel powder are mixed in a mass ratio of 1: 1, uniformly mixing and then filling into a charging hopper.
In a preferred embodiment of the present invention, the method for preparing boron nitride nanotubes further comprises adding 5-7g of the catalyst at one time.
In a preferred embodiment of the present invention, the method for preparing boron nitride nanotubes further comprises the step (5), wherein the diameter of the tungsten filament is 0.4-0.8mm, and the vertical distance between the tungsten filament and the discharge anode is 0.5-1 mm.
In a preferred embodiment of the present invention, the method for preparing boron nitride nanotubes further comprises the step (6) of controlling the entry rate of the catalyst to 40-60 mg/s.
In a preferred embodiment of the present invention, the method for preparing boron nitride nanotubes further comprises the step (6) of maintaining the gap between the discharge anode and the discharge cathode at 1.5-2.5mm by a driving mechanism.
The invention solves the defects in the background technology, the invention directly adopts boron as the discharge anode, firstly, the boron is heated by the contact of the discharge cathode and the discharge anode, and then the arc striking is assisted by an external high-voltage power supply, the arc striking efficiency is obviously improved, in the discharge process, the catalyst is continuously added between the discharge cathode and the discharge anode by using the charging hopper, the stability in the arc discharge process is obviously improved, the synthesis efficiency of the boron nitride nanotube is improved, a large amount of gray flocculent net-shaped products are generated on the surface of the discharge cathode and the inner wall of the discharge chamber after the discharge, the invention can carry out the long-time stable arc discharge, and the prepared boron nitride nanotube has more concentrated, changeable and more perfect product size than the product of the traditional technology.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic structural view of an arc discharge device according to a preferred embodiment of the present invention;
FIG. 2 is a graph of arc voltage and arc current over time during a discharge process of the present invention;
FIG. 3 is a TEM (transmission electron microscope) image of a single-walled boron nitride nanotube prepared by a preferred embodiment of the method of the present invention;
FIG. 4 is a TEM (transmission electron microscope) image of a multi-walled boron nitride nanotube prepared by a preferred embodiment of the method of the present invention;
fig. 5 is a TEM (transmission electron microscope) image of boron nitride nanotubes grown around nanoparticles prepared by a preferred embodiment of the method of the present invention.
Detailed Description
The invention will now be described in further detail with reference to the accompanying drawings and examples, which are simplified schematic drawings and illustrate only the basic structure of the invention in a schematic manner, and thus show only the constituents relevant to the invention.
As shown in fig. 1, an arc discharge device comprises a discharge chamber 2, a discharge cathode 4 disposed in the discharge chamber 2, a discharge anode 6, a hopper 8, and a tungsten filament 10 with one end extending into the discharge chamber 2, the discharge chamber 2 is provided with an air exhaust valve 12 and an air intake valve 14, the discharge cathode 4 is disposed opposite to the discharge anode 6, a gap 16 is formed between the discharge cathode 4 and the discharge anode 6, the hopper 8 is disposed above the gap 16, one end of the discharge cathode 4 is connected with a first conductive rod 18, one end of the discharge anode 6 is connected with a second conductive rod 20, the first conductive rod 18 and the second conductive rod 20 both partially penetrate through the discharge chamber 2, preferably, a first clamping member 22 is fixed on the first conductive rod 18, the first clamping member 22 clamps the discharge cathode 4, a second clamping member 24 is fixed on the second conductive rod 20, the second clamping member 24 clamps the discharge anode 6, and both the first clamping member 22 and the second clamping member 24 are made of red copper, but not limited to red copper, aluminum or silver, the first conductive rod 18 and the second conductive rod 20 are both stainless steel, but not limited to stainless steel, and may be aluminum or silver, the second conductive rod 18 is connected to a driving mechanism 26, the driving mechanism 26 is a gear rack mechanism connected by a stepping motor, or the cylinder can drive the second conducting rod 20 to retract left and right, so that the second conducting rod 20 is close to or far away from the first conducting rod 18, the distance between the discharge cathode 4 and the discharge anode 6 is adjusted, however, the present invention is not limited to this embodiment, and the driving mechanism may be connected to the first conductive rod 20, the load resistor 28 may be connected to the first conductive rod 18, the load resistor 28 may be connected to the negative electrode of the first power source 30, the other end of the tungsten filament 10 may be connected to the negative electrode of the second power source 32, and the positive electrode of the first power source 30, the positive electrode of the second conductive rod 20, and the positive electrode of the second power source 32 may be connected to the ground. Preferably, the first power source 30 is a power source, more preferably, the first power source 30 is a power source of 40V/70A, more preferably, the second power source 32 is a high voltage DC power source, more preferably, the second power source is a 3000V high voltage DC power source, and more preferably, the load resistor 28 is 1-10 Ω. To facilitate air extraction, the extraction valve 12 is connected to a mechanical pump 34. In order to facilitate observation of the discharge condition in the discharge chamber 2, it is preferable that the discharge chamber 2 is provided with an observation window 36.
A method for preparing boron nitride nanotubes by using the device comprises the following steps:
(1) adopting tungsten as a discharge cathode, wherein the discharge cathode is cylindrical, the diameter is 5-7mm, the length is 50-130mm, boron is used as a discharge anode, and the discharge anode is cylindrical, the diameter is 8-12mm, and the length is 10-25 mm;
(2) the loading hopper is in a closed state, a catalyst is prepared, the catalyst comprises cobalt powder and nickel powder, and the cobalt powder and the nickel powder are mixed according to a mass ratio of 1: 1, uniformly mixing and then filling the mixture into a charging hopper, wherein the amount of the catalyst added at one time is 5-7 g;
(3) sealing the discharge chamber, starting the mechanical pump, and pumping out air in the discharge chamber to background vacuum<1Pa, introducing nitrogen, and adjusting an air extraction valve and an air inlet valve to maintain the air pressure in the discharge chamber at 3 x 104Pa -7×104Pa；
(4) The discharge cathode is contacted with the discharge anode by using a driving mechanism, the current of a first power supply is increased to 35-45A, and the discharge cathode and the discharge anode are preheated;
(5) after preheating for 0.5-1.5min, separating the discharge cathode and the discharge anode, adjusting the voltage of a second power supply to 2000-2500V, wherein the diameter of the tungsten wire is 0.4-0.8mm, the vertical distance between the tungsten wire and the discharge anode is 0.5-1mm, the tungsten wire, the discharge cathode and the discharge anode are ignited and excite the electric arc between the discharge cathode and the discharge anode, and the second power supply is immediately closed after the arc striking is finished;
(6) in the arc discharge process, a driving mechanism is used for maintaining the gap between a discharge anode and a discharge cathode to be 1.5-2.5mm, a loading hopper is opened, a catalyst enters between the discharge cathode and the discharge anode, and the entering speed of the catalyst is controlled to be 40-60 mg/s;
(7) and after the discharge is finished, forming boron nitride nanotubes on the surface of the discharge cathode and the inner wall of the discharge cavity.
Fig. 2-5 are methods of using the present invention, comprising the steps of:
(1) adopting tungsten as a discharge cathode, wherein the discharge cathode is cylindrical, the diameter of the discharge cathode is 6mm, the length of the discharge cathode is 100mm, boron is used as a discharge anode, and the discharge anode is cylindrical, the diameter of the discharge anode is 9mm, and the length of the discharge anode is 20 mm;
(2) the loading hopper is in a closed state, a catalyst is prepared, the catalyst comprises cobalt powder and nickel powder, and the cobalt powder and the nickel powder are mixed according to a mass ratio of 1: 1, uniformly mixing, and then filling into a charging hopper, wherein the amount of the catalyst added at one time is 6 g;
(3) sealing the discharge chamber, starting the mechanical pump, and pumping out air in the discharge chamber to background vacuum<1Pa, introducing nitrogen, and adjusting an air extraction valve and an air inlet valve to maintain the air pressure in the discharge chamber at 5X 104Pa ；
(4) The discharge cathode is contacted with the discharge anode by using a driving mechanism, the current of a first power supply is increased to 40A, and the discharge cathode and the discharge anode are preheated;
(5) after preheating for 1min, separating a discharge cathode and a discharge anode, adjusting the voltage of a second power supply, increasing the voltage of a tungsten filament to 2300V when the voltage is increased, wherein the diameter of the tungsten filament is 0.6mm, the vertical distance between the tungsten filament and the discharge anode is 1mm, igniting between the tungsten filament and the electrodes and exciting an electric arc between the discharge cathode and the discharge anode, and immediately closing the second power supply after the electric arc is started;
(6) in the arc discharge process, a driving mechanism is used for maintaining the gap between a discharge anode and a discharge cathode to be 2mm, a loading hopper is opened, a catalyst enters between the discharge cathode and the discharge anode, and the entering speed of the catalyst is controlled to be 50 mg/s;
(7) and products are formed on the surface of the discharge cathode and the inner wall of the discharge cavity after the discharge is finished.
As can be seen from FIG. 2, during the discharge, the arc voltage is reduced from 40V to 25V, the arc current is increased from 0 to 40A, and during the discharge, the fluctuation range of the arc current is large and varies from 30A to 50A due to the addition of the catalyst.
Fig. 3-5 are TEM representations of the resulting product and found to have significant amounts of single-walled boron nitride nanotubes, double-walled boron nitride nanotubes, and boron nitride nanotubes grown around the nanoparticles, grown in bundles with an average length of about 1-3 microns along the unreacted anode material deposited on the surface of the discharge cathode. The invention has stable arc discharge environment and can effectively improve the quality of the boron nitride nanotube.
In light of the foregoing description of the preferred embodiment of the present invention, it is to be understood that various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (8)
1. The method for preparing the boron nitride nanotube is characterized in that an arc discharge device is utilized, the arc discharge device comprises a discharge chamber, a discharge cathode, a discharge anode, a feed hopper and a tungsten filament, wherein the discharge cathode, the discharge anode, the feed hopper and the tungsten filament are arranged in the discharge chamber, one end of the tungsten filament extends into the discharge chamber, an air suction valve and an air inlet valve are arranged on the discharge chamber, a gap is formed between the discharge cathode and the discharge anode, the feed hopper is positioned above the gap, one end of the discharge cathode is connected with a first conducting rod, one end of the discharge anode is connected with a second conducting rod, the first conducting rod or the second conducting rod is connected with a driving mechanism, the first conducting rod is connected with a load resistor, the load resistor is connected with the negative pole of a first power supply, the other end of the tungsten filament is connected with the negative pole of a second power supply, the positive pole, The second conducting rod and the positive pole of the second power supply are both connected with the ground, and the method comprises the following steps:
(1) tungsten is used as a discharge cathode, and boron is used as a discharge anode;
(2) the loading hopper is in a closed state, and the catalyst is filled into the loading hopper;
(3) sealing the discharge chamber, pumping out air in the discharge chamber to background vacuum<1Pa, introducing nitrogen, and adjusting an air extraction valve and an air inlet valve to maintain the air pressure in the discharge chamber at 3 x 104Pa -7×104Pa；
(4) The discharge cathode is contacted with the discharge anode by using a driving mechanism, the current of a first power supply is increased to 35-45A, and the discharge cathode and the discharge anode are heated;
(5) after heating for 0.5-1.5min, separating the discharge cathode and the discharge anode, adjusting the voltage of the second power supply to 2000-2500V, igniting the tungsten filament between the discharge cathode and the discharge anode and exciting an electric arc between the discharge cathode and the discharge anode, and immediately closing the second power supply after the arc striking is finished;
(6) in the arc discharge process, opening a charging hopper to allow a catalyst to enter between a discharge cathode and a discharge anode;
(7) and products are formed on the surface of the discharge cathode and the inner wall of the discharge cavity after the discharge is finished.
2. The method for preparing boron nitride nanotubes according to claim 1, wherein in step (1), the discharge cathode has a cylindrical shape with a diameter of 5-7mm and a length of 50-130 mm.
3. The method for preparing boron nitride nanotubes according to claim 1, wherein in step (1), the discharge anode has a cylindrical shape with a diameter of 8-12mm and a length of 10-25 mm.
4. The method for preparing boron nitride nanotubes according to claim 1, wherein in the step (2), the catalyst comprises cobalt powder and nickel powder, and the mass ratio of the cobalt powder to the nickel powder is 1: 1, uniformly mixing and then filling into a charging hopper.
5. The method for preparing boron nitride nanotubes as claimed in claim 4, wherein the amount of the catalyst added at one time is 5-7 g.
6. The method for preparing boron nitride nanotubes of claim 1, wherein in step (5), the diameter of the tungsten filament is 0.4-0.8mm, and the vertical distance between the tungsten filament and the discharge anode is 0.5-1 mm.
7. The method for producing boron nitride nanotubes according to claim 1, wherein in the step (6), the entry rate of the catalyst is controlled to 40 to 60 mg/s.
8. The method for preparing boron nitride nanotubes of claim 1, wherein in step (6), the gap between the discharge anode and the discharge cathode is maintained at 1.5-2.5mm by a driving mechanism.
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| JPH06333535A (en) * | 1993-05-18 | 1994-12-02 | Showa Denko Kk | Metallic vapor discharge lamp coated with boron nitride film |
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