CN108043345A - Arc discharge device and the method that boron nitride nano-tube is prepared using the device - Google Patents
Arc discharge device and the method that boron nitride nano-tube is prepared using the device Download PDFInfo
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- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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- B01J2219/0807—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 involving electrodes
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Abstract
The present invention relates to a kind of arc discharge devices, including the chamber that discharges, arranged on the indoor electric discharge cathode of discharge cavity, discharge anode, the indoor tungsten filament of the discharge cavity is stretched into loading hopper and one end, extraction valve and intake valve are provided on electric discharge chamber, discharging has gap between cathode and discharge anode, loading hopper is located at the top in gap, one end of electric discharge cathode is connected with the first conducting rod, one end of discharge anode is connected with the second conducting rod, first conducting rod or the second conducting rod are connected with driving mechanism, first conducting rod is connected with load resistance, load resistance is connected with the cathode of the first power supply, the other end of tungsten filament is connected with the cathode of second source, the anode of first power supply, the anode of second conducting rod and second source is connected to the ground.The invention further relates to a kind of methods for preparing boron nitride nano-tube.The present invention significantly increases the stability in arc discharge process, and the boron nitride nano-tube prepared more is concentrated than the product ruler footpath of traditional handicraft, and form is more perfect.
Description
Technical field
The present invention relates to hot plasma and technical field of nano material more particularly to a kind of arc discharge device and utilizations
The method that the device prepares boron nitride nano-tube.
Background technology
Since there is boron nitride nano-tube higher Young's modulus, stronger inoxidizability, higher hydrogen molecule to absorb energy
Good characteristics are waited, it is often applied to high intensity synthetic material and hydrogen storage field.Similar with carbon nanotubes, boron nitride nano-tube has
Several synthetic methods below：Synthetic method based on plasma technique, pulsed laser deposition method, chemical vapour deposition technique and machine
Tool ball milling annealing method.Synthetic method and pulsed laser deposition method based on plasma technique can produce the nitridation of better quality
Boron nanotube, thus become the emphasis of current research.In the synthetic method based on plasma technique, only near atmospheric pressure
DC arc discharge and atmospheric pressure/high-voltage radio-frequency plasma can synthesize larger boron nitride nano-tube combination.And from
From the perspective of practicality, the sharpest edges of arc process are that synthesis device is simple in structure, cost is relatively low.
There are mainly two types of traditional arc process synthesis boron nitride nanotube technologies：A kind of compound using boracic makees electricity
Pole is discharged in nitrogen protects gas；Another kind uses the electrode containing boron nitride composite, is put in helium
Electricity.Traditional preparation method has the defects of several more apparent：First, the boron nitride nano-tube synthesized using both approaches
It almost exists only in cathode deposition, yield is relatively low and its subsequent separation and purification are more difficult；Secondly, electric arc electric discharge
Cathode and anode all employ boron-containing compound, and this compound electrode prepares difficulty, boron nitride nano-tube will be significantly greatly increased
Production cost.
The content of the invention
The present invention overcomes the deficiencies in the prior art, provide a kind of electric arc electric discharge dress for reducing cost, improving work efficiency
The method put and boron nitride nano-tube is prepared using the device
In order to achieve the above objectives, the technical solution adopted by the present invention is：A kind of arc discharge device including electric discharge chamber, is arranged on
The indoor tungsten filament of the discharge cavity is stretched into indoor cathode, discharge anode, loading hopper and the one end of discharging of the discharge cavity, described
Extraction valve and intake valve are provided on electric discharge chamber, there is gap, the loading hopper between the electric discharge cathode and discharge anode
Positioned at the top in the gap, one end of the electric discharge cathode is connected with the first conducting rod, one end connection of the discharge anode
There is the second conducting rod, first conducting rod or the second conducting rod are connected with driving mechanism, and first conducting rod is connected with negative
Resistance is carried, the load resistance is connected with the cathode of the first power supply, the other end of the tungsten filament and the cathode phase of second source
Connection, the anode of the anode of first power supply, the second conducting rod and second source are connected to the ground.
A kind of method for preparing boron nitride nano-tube, using described device, comprises the following steps：
（1）Using tungsten as electric discharge cathode, boron is as discharge anode；
（2）Loading hopper is closed, and catalyst is filled into loading hopper；
（3）Closing electric discharge chamber, extraction electric discharge chamber air are passed through nitrogen, bleeding regulating valve and intake valve to base vacuum
So that discharge cavity room pressure maintains 3 × 104Pa -7×104Pa；
（4）Electric discharge cathode and discharge anode are contacted using driving mechanism, increases the electric current of the first power supply to 35-45A, to electric discharge
Cathode and discharge anode are heated；
（5）After heating 0.5-1.5min, separately discharge cathode and discharge anode, adjusts the voltage of second source to 2000-
2500V strikes sparks between tungsten filament and electric discharge cathode, discharge anode and excites the electric arc between electric discharge cathode and discharge anode, and the starting the arc is completed
Close second source immediately afterwards；
（6）In arc discharge process, loading hopper is opened, catalyst is allowed to enter between electric discharge cathode and discharge anode；
（7）After electric discharge product is formed in electric discharge cathode surface and electric discharge chamber inner wall.
In a preferred embodiment of the present invention, the method for preparing boron nitride nano-tube further comprises the step（1）In,
The cathode that discharges is cylinder, a diameter of 5-7mm, length 50-130mm.
In a preferred embodiment of the present invention, the method for preparing boron nitride nano-tube further comprises the step（1）In,
Discharge anode is cylinder, a diameter of 8-12mm, length 10-25mm.
In a preferred embodiment of the present invention, the method for preparing boron nitride nano-tube further comprises the step（2）In,
Catalyst includes cobalt powder and nickel powder, the cobalt powder and nickel powder in mass ratio 1：It is filled into after 1 uniform mixing in loading hopper.
In a preferred embodiment of the present invention, prepare boron nitride nano-tube method further comprise once filling it is described
Catalyst is 5-7g.
In a preferred embodiment of the present invention, the method for preparing boron nitride nano-tube further comprises the step（5）In,
A diameter of 0.4-0.8mm of tungsten filament, the vertical range between tungsten filament and discharge anode are 0.5-1mm.
In a preferred embodiment of the present invention, the method for preparing boron nitride nano-tube further comprises the step（6）In,
The ingress rate of catalyst is controlled in 40-60mg/s.
In a preferred embodiment of the present invention, the method for preparing boron nitride nano-tube further comprises the step（6）In,
The gap for maintaining discharge anode between the cathode that discharges by driving mechanism is in 1.5-2.5mm.
The present invention solves defect present in background technology, and the present invention, as discharge anode, is first passed through directly using boron
It discharges after cathode and discharge anode contact heating, external high voltage power supply is recycled to aid in the starting the arc, starting the arc efficiency has obtained significantly
It improves, in discharge process, catalyst is persistently added between electric discharge cathode and discharge anode using loading hopper, is dramatically increased
Stability in arc discharge process, the combined coefficient for improving boron nitride nano-tube are discharged after electric discharge and cathode surface and are put
Electric chamber inner wall has a large amount of grey wadding netted product generations, and the present invention can carry out the electric arc electric discharge of long-time stable, prepare
Boron nitride nano-tube more concentrated than the product ruler footpath of traditional handicraft, form is changeable and more perfect.
Description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is the structure diagram of the arc discharge device of the preferred embodiment of the present invention；
Fig. 2 be the present invention discharge process in arc voltage and arc current change with time figure；
Fig. 3 is the TEM for the single-walled boron nitride nanotubes that a preferred embodiment of the method for the present invention is prepared（Transmitted electron is shown
Micro mirror）Figure；
Fig. 4 is the TEM for the multi wall boron nitride nano-tube that a preferred embodiment of the method for the present invention is prepared（Transmitted electron is shown
Micro mirror）Figure；
Fig. 5 is the boron nitride nano-tube being grown in around nano particle that a preferred embodiment of the method for the present invention is prepared
TEM（Transmission electron microscope）Figure.
Specific embodiment
Presently in connection with drawings and examples, the present invention is described in further detail, these attached drawings are simplified signal
Figure only illustrates the basic structure of the present invention in a schematic way, therefore it only shows composition related to the present invention.
As shown in Figure 1, a kind of arc discharge device, including electric discharge chamber 2, the electric discharge cathode 4 in electric discharge chamber 2,
The tungsten filament 10 in electric discharge chamber 2 is stretched into discharge anode 6, loading hopper 8 and one end, and 12 He of extraction valve is provided on the chamber 2 that discharges
Intake valve 14, electric discharge cathode 4 are oppositely arranged with discharge anode 6, and discharging has gap 16 between cathode 4 and discharge anode 6, charging
Bucket 8 is located at the top in gap 16, and one end of electric discharge cathode 4 is connected with the first conducting rod 18, and one end of discharge anode 6 is connected with the
Two conducting rods 20, the first conducting rod 18 and the second conducting rod 20 partially pass through electric discharge chamber 2, consolidate on preferably the first conducting rod 18
Surely there is the first clamping member 22, the first clamping member 22 clamps electric discharge cathode 4, the second clamping piece 24 is fixed on the second conducting rod 20,
Second clamping piece 24 clamps discharge anode 6, and 22 and second clamping piece 24 of the first clamping member is using red copper material, but do not limit to
In red copper material, or aluminium or silver, the first conducting rod 18 and the second conducting rod 20 are stainless steel, but are not limited to
In stainless steel, or aluminium or silver, the second conducting rod 18 are connected with driving mechanism 26, and driving mechanism 26 is using generally in the art
Technology, such as the rack and pinion mechanism or cylinder of stepper motor connection, can drive 20 or so the retraction of the second conducting rod, make
The second conducting rod 20 closer or far from the first conducting rod 18, adjust electric discharge the distance between cathode 4 and discharge anode 6, but simultaneously
It is not limited to such mode or the first conducting rod 20 is connected with driving mechanism, the first conducting rod 18 is connected with load electricity
Resistance 28, load resistance 28 is connected with the cathode of the first power supply 30, and the other end of tungsten filament 10 is connected with the cathode of second source 32
It connects, the anode of the anode of the first power supply 30, the second conducting rod 20 and second source 32 is connected to the ground.It is preferred that the first power supply 30
For power source, further preferred first power supply 30 is the power source of 40V/70A, and preferably second source 32 is high-voltage DC power supply,
Further preferred second source is 3000V high-voltage DC power supplies, and preferably load resistance 28 is 1-10 Ω.It, will for the ease of pumping
Extraction valve 12 is connected with mechanical pump 34.For the ease of the discharged condition in observation electric discharge chamber 2, the preferred electric discharge chamber of the present invention
Watch window 36 is provided on 2.
A kind of method for preparing boron nitride nano-tube, using above device, comprises the following steps：
（1）Using tungsten as electric discharge cathode, electric discharge cathode is cylinder, a diameter of 5-7mm, length 50-130mm, boron conduct
Discharge anode, discharge anode is cylinder, a diameter of 8-12mm, length 10-25mm；
（2）Loading hopper is closed, and prepares catalyst, and catalyst includes cobalt powder and nickel powder, and cobalt powder and nickel powder are in mass ratio
1：It is filled into after 1 uniform mixing in loading hopper, the catalyst once filled is 5-7g；
（3）Closing electric discharge chamber opens mechanical pump, extraction electric discharge chamber air to base vacuum, base vacuum<1Pa is passed through
Nitrogen, bleeding regulating valve and intake valve cause discharge cavity room pressure to maintain 3 × 104Pa -7×104Pa；
（4）Electric discharge cathode and discharge anode are contacted using driving mechanism, increases the electric current of the first power supply to 35-45A, to electric discharge
Cathode and discharge anode are preheated；
（5）After preheating 0.5-1.5min, separately discharge cathode and discharge anode, adjusts the voltage of second source to 2000-
2500V, a diameter of 0.4-0.8mm of tungsten filament, the vertical range between tungsten filament and discharge anode are 0.5-1mm, tungsten filament and electric discharge
It strikes sparks between cathode, discharge anode and excites the electric arc between electric discharge cathode and discharge anode, close the second electricity after the completion of the starting the arc immediately
Source；
（6）In arc discharge process, the gap for maintaining discharge anode between the cathode that discharges by driving mechanism is in 1.5-
2.5mm opens loading hopper, and catalyst is allowed to enter between electric discharge cathode and discharge anode, and the ingress rate of catalyst is controlled in 40-
60mg/s；
（7）After electric discharge boron nitride nano-tube is formed in electric discharge cathode surface and electric discharge chamber inner wall.
Fig. 2-Fig. 5 is method using the present invention, is comprised the following steps：
（1）Using tungsten as electric discharge cathode, electric discharge cathode is cylinder, a diameter of 6mm, length 100mm, and boron is as electric discharge
Anode, discharge anode is cylinder, a diameter of 9mm, length 20mm；
（2）Loading hopper is closed, and prepares catalyst, and catalyst includes cobalt powder and nickel powder, and cobalt powder and nickel powder are in mass ratio
1：It is filled into after 1 uniform mixing in loading hopper, the catalyst once filled is 6g；
（3）Closing electric discharge chamber opens mechanical pump, extraction electric discharge chamber air to base vacuum, base vacuum<1Pa is passed through
Nitrogen, bleeding regulating valve and intake valve cause discharge cavity room pressure to maintain 5 × 104Pa ；
（4）Electric discharge cathode and discharge anode are contacted using driving mechanism, increases the electric current of the first power supply to 40A, it is cloudy to electric discharge
Pole and discharge anode are preheated；
（5）After preheating 1min, separately discharge cathode and discharge anode, adjusts the voltage of second source, increases the voltage of tungsten filament,
Voltage increases to 2300V, a diameter of 0.6mm of tungsten filament, and the vertical range between tungsten filament and discharge anode is 1mm, tungsten filament and electricity
Interpolar strikes sparks and excites the electric arc between electric discharge cathode and discharge anode, and second source is closed immediately after the completion of the starting the arc；
（6）In arc discharge process, the gap between discharge anode and the cathode that discharges is maintained in 2mm, opening by driving mechanism
Loading hopper allows catalyst to enter between electric discharge cathode and discharge anode, and the ingress rate of catalyst is controlled in 50mg/s；
（7）After electric discharge product is formed in electric discharge cathode surface and electric discharge chamber inner wall.
As seen from Figure 2, in discharge process, arc voltage is reduced to 25V by 40V, and arc current increases to 40A by 0,
In discharge process, due to the addition of catalyst, arc current fluctuation range is larger, changes between 30-50A.
Fig. 3-Fig. 5 is that the product of formation is characterized using TEM, and there are substantial amounts of single wall boron nitride in discovery product to receive
Mitron, double-walled boron nitride nano-tube and the boron nitride nano-tube being grown in around nano particle, along being deposited on electric discharge cathode
The unreacted anode material bunchy growth in surface, about 1-3 microns of average length.The electric arc discharge environment of the present invention is stablized, and can have
Effect improves the quality of boron nitride nano-tube.
Above desirable embodiment according to the invention is enlightenment, and by above-mentioned description, related personnel completely can be with
Without departing from the scope of the technological thought of the present invention', various changes and amendments are carried out.The technical scope of this invention
The content being not limited on specification, it is necessary to determine the technical scope according to the scope of the claims.
Claims (9)
1. a kind of arc discharge device, it is characterised in that：Including electric discharge chamber, arranged on the discharge cavity it is indoor electric discharge cathode,
The indoor tungsten filament of the discharge cavity is stretched into discharge anode, loading hopper and one end, be provided on the electric discharge chamber extraction valve and
Intake valve has gap between the electric discharge cathode and discharge anode, and the loading hopper is located at the top in the gap, described to put
One end of electric cathode is connected with the first conducting rod, and one end of the discharge anode is connected with the second conducting rod, and described first is conductive
Bar or the second conducting rod are connected with driving mechanism, and first conducting rod is connected with load resistance, the load resistance and first
The cathode of power supply is connected, and the other end of the tungsten filament is connected with the cathode of second source, the anode of first power supply,
The anode of two conducting rods and second source is connected to the ground.
A kind of 2. method for preparing boron nitride nano-tube, which is characterized in that device as described in claim 1 is utilized, including following
Step：
Using tungsten as electric discharge cathode, boron is as discharge anode；
Loading hopper is closed, and catalyst is filled into loading hopper；
Closing electric discharge chamber, extraction electric discharge chamber air are passed through nitrogen, bleeding regulating valve and intake valve cause to base vacuum
Discharge cavity room pressure maintains 3 × 104Pa -7×104Pa；
（4）Electric discharge cathode and discharge anode are contacted using driving mechanism, increases the electric current of the first power supply to 35-45A, to electric discharge
Cathode and discharge anode are heated；
（5）After heating 0.5-1.5min, separately discharge cathode and discharge anode, adjusts the voltage of second source to 2000-
2500V strikes sparks between tungsten filament and electric discharge cathode, discharge anode and excites the electric arc between electric discharge cathode and discharge anode, and the starting the arc is completed
Close second source immediately afterwards；
（6）In arc discharge process, loading hopper is opened, catalyst is allowed to enter between electric discharge cathode and discharge anode；
（7）After electric discharge product is formed in electric discharge cathode surface and electric discharge chamber inner wall.
3. the method according to claim 2 for preparing boron nitride nano-tube, which is characterized in that the step（1）In, electric discharge
Cathode is cylinder, a diameter of 5-7mm, length 50-130mm.
4. the method according to claim 2 for preparing boron nitride nano-tube, which is characterized in that the step（1）In, electric discharge
Anode is cylinder, a diameter of 8-12mm, length 10-25mm.
5. the method according to claim 2 for preparing boron nitride nano-tube, which is characterized in that the step（2）In, catalysis
Agent includes cobalt powder and nickel powder, the cobalt powder and nickel powder in mass ratio 1：It is filled into after 1 uniform mixing in loading hopper.
6. the method according to claim 5 for preparing boron nitride nano-tube, which is characterized in that the catalysis once filled
Agent is 5-7g.
7. the method according to claim 2 for preparing boron nitride nano-tube, which is characterized in that the step（5）In, tungsten filament
A diameter of 0.4-0.8mm, vertical range between tungsten filament and discharge anode is 0.5-1mm.
8. the method according to claim 2 for preparing boron nitride nano-tube, which is characterized in that the step（6）In, catalysis
The ingress rate of agent is controlled in 40-60mg/s.
9. the method according to claim 2 for preparing boron nitride nano-tube, which is characterized in that the step（6）In, pass through
The gap that driving mechanism maintains discharge anode between the cathode that discharges is in 1.5-2.5mm.
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