CN105731480A - Method for preparing boron nano material through arc discharge - Google Patents
Method for preparing boron nano material through arc discharge Download PDFInfo
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- CN105731480A CN105731480A CN201610296932.4A CN201610296932A CN105731480A CN 105731480 A CN105731480 A CN 105731480A CN 201610296932 A CN201610296932 A CN 201610296932A CN 105731480 A CN105731480 A CN 105731480A
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- arc discharge
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/023—Boron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a method for preparing a boron nano material through arc discharge, and belongs to a method for preparing a nano material. The invention mainly aims to solve the technical problems of poor product purity, low preparation efficiency and low production of the existing method for preparing a nano material through arc discharge. The technical scheme of the invention is that the method for preparing the boron nano material through arc discharge comprises the following steps: (1) mixing boron powder and high-boiling-point metal powder according to a volume ratio of (1-10):1 to prepare a powder mixture; (2) installing a pure tungsten negative electrode and a mixed positive electrode in a reaction cavity of an arc discharge device, wherein the mixed positive electrode and the pure tungsten negative electrode are connected with a power supply, and the mixed positive electrode is a mixed electrode prepared from a powder mixture and a tungsten crucible; (3) performing evacuation on the reaction cavity, and then introducing a working gas; (4) switching on a power supply to perform arc discharge, and keeping the discharge current and the voltage stable during discharge; and (5) after discharge, collecting a product in the reaction cavity under the protection of argon gas.
Description
Technical field
The present invention relates to a kind of method that arc discharge prepares boron nano material, it belongs to a kind of method preparing nano material.
Background technology
Arc discharge is a kind of method of conventional preparation nano material.Relative to laser ablation and chemical deposition, it is with low cost, is suitable for a large amount of production, has become as the prefered method of preparation nano material.At present, it is widely used to prepare high boiling carbon nanomaterial, including fullerene, metal fullerene, CNT etc..Prepare in the technique of carbon nanomaterial at arc discharge, adopt the graphite electrode conducted electricity or admixed graphite electrode as carbon source.In arc discharge, graphite electrode deposits in high temperature gasified produced by electric arc as consumable anode, generates carbon nanomaterial.
But, for being high boiling boron material (boiling point 3927 DEG C) equally, do not deposit the pure boron material of conduction due to nature, it is impossible to directly make pure boron simple substance consumable anode, thus cannot by with carbons like method prepare boron nano material.On the other hand, the chemical gaseous phase depositing process primary raw material when preparing boron nano material is highly toxic borane gas, and the special handling of this high-air-tightness needing equipment and reaction end gas encounters huge difficulty in technique, is rarely employed at present.Therefore, arc discharge method remains the prefered method preparing a large amount of boron nano materials.
In order to enable boron material to prepare nano material by arc discharge, ZL201510146897.3 discloses " a kind of method utilizing arc discharge to prepare boron nitride nanometer fiber ", the method adopts and hollows out in the middle of graphite electrode, and a small amount of boron material (boron nitride) is embedded the nano material preparing boron in graphite electrode.Although this method can produce boron nano material, but it can generate a large amount of carbon nanomaterial while producing boron nano material, causes that required boron nano material is mixed in material with carbon element, it is difficult to separating-purifying.It addition, a small amount of required boron material can only be put in each graphite electrode center, preparation efficiency is low.On the other hand, it is possible to the method taking to add conductive agent in boron powder, common conductive agent is such as added: white carbon black, nikel powder etc..But these conductive agents can evaporate equally in course of reaction and become gas, even form compound with boron element, generate a large amount of impurity composition in the product.
Summary of the invention
Present invention aim to address that existing arc discharge prepares the technical problem that method also exists product purity difference, preparation efficiency is low and yield is few of nano material, it is provided that a kind of arc discharge prepares the method for boron nano material.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
A kind of arc discharge prepares the method for boron nano material, and it comprises the following steps:
(1) prepare mixture of powders: be that 1～10:1 mixes by volume boron powder and high boiling point metal dust, prepare mixture of powders；
(2) in the reaction chamber of arc discharge device, pure tungsten negative electrode is installed and multilayer anode, described multilayer anode and pure tungsten negative electrode are all connected with power supply；The mixed electrode that described multilayer anode is mixture of powders and tungsten crucible is made；
(3) described reaction chamber is bled, make the air pressure in reaction chamber lower than 0.0001Pa, then pass to working gas；
(4) switch on power and carry out arc discharge, first initial current is regulated to 10 amperes, then the distance of pure tungsten negative electrode and multilayer anode is regulated, when making pure tungsten negative electrode and multilayer anode 8～12mm apart, continue to regulate electric current to 160～175 amperes, voltage remains 50 volts, keeps discharge current and voltage stabilization in discharge process；
(5), after end to be discharged, under argon gas is protected, in reaction chamber, product is collected.
Further, described high boiling point metal dust is any one in tungsten, tantalum or rhenium powder.
The present invention adopts technique scheme, make consumable anode and pure tungsten negative electrode heavy-current discharge under the conduction of metal dust, the high temperature generated causes that boron powder progressively melts and gasifies, finally deposition generates the nano material of boron, and high boiling metal does not gasify substantially, it is retained in crucible, solves existing arc discharge and prepare the technical problem that method also exists product purity difference, preparation efficiency is low and yield is few of nano material.Therefore, compared with background technology, the present invention has that technical process is simple, product purity is high and produces big advantage.
Accompanying drawing explanation
Fig. 1 is the structural representation of arc discharge device of the present invention；
In figure, 1, mixture of powders, 2, tungsten crucible, 3, anode conducting plate, 4, pure tungsten negative electrode, 5, reaction chamber, 6, cooling water system, 7, argon air valve, 8, vacuum valve, 9, negative electrode step-by-step system.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps:
(1) prepare mixture of powders: boron powder and tungsten powder powder are mixed for 4:1 by volume, prepare mixture of powders；
(2) in the reaction chamber of arc discharge device, pure tungsten negative electrode is installed and multilayer anode, described multilayer anode and pure tungsten negative electrode are all connected with power supply；The mixture of powders of preparation in step (1) is loaded tungsten crucible, and with the mixed electrode that tablet machine compacting is made；
(3) described reaction chamber is bled, make the air pressure in reaction chamber lower than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, first initial current is regulated to 10 amperes, then the distance of pure tungsten negative electrode and multilayer anode is regulated, when making pure tungsten negative electrode and multilayer anode 8mm apart, continue to regulate electric current to 160 amperes, voltage is 50 volts, keeps discharge current and voltage stabilization in discharge process；
(5), after end to be discharged, under argon gas is protected, in reaction chamber, collect product namely obtain boron nano material.
Specifically, 40 grams of boron powder and 80 grams of tungsten powder ground and mixed uniformly being obtained boron powder and tungsten powder mixture of powders 1, now boron powder is about 4:1 with the volume ratio of tungsten powder.Above-mentioned mixture of powders 1 being loaded tungsten crucible 2 (diameter 50mm height 20mm), and with the mixed electrode that tablet machine compacting is made, the resistance measuring tungsten crucible surface and mixture of powders surface is 1.67m Ω；Tungsten crucible mixed electrode is placed on the anode conducting plate 3 in the reaction chamber 5 of arc discharge device, closes reaction chamber 5, the pure tungsten negative electrode 4 being arranged on above the reaction chamber 5 of arc discharge device is directed at tungsten crucible mixed electrode center and fits tightly.Open vacuum pump, open the vacuum valve 8 that reaction chamber 5 is connected with vacuum pump, reaction chamber is carried out evacuation.When air pressure is lower than 4Pa, open cooling water system 6, open molecular pump, continue evacuation, when air pressure is lower than 0.0001Pa, close the vacuum valve 8 that reaction chamber 5 is connected with vacuum pump, stop evacuation.Slowly open argon air valve 7, in reaction chamber, be filled with certain argon.Switching on power, regulate current knob, increase initial current to 10 amperes, regulate the height of pure tungsten negative electrode by negative electrode step-by-step system 9, make mixed electrode and pure tungsten negative electrode disengage, distance is about 8mm.Now produce some arc sparks between mixed electrode and tungsten cathode.Continuing to regulate electric current and reach 160 amperes, voltage is 50 volts, now defines powerful electric field between mixed electrode and pure tungsten negative electrode and produces electric discharge, makes temperature reach more than 4000 DEG C.The local temperature of mixed electrode constantly raises so that boron powder and tungsten powder melt in succession, and temperature continues to raise, and boron gas is flown out by evaporation, and the volume of tungsten liquid constantly increases, and the boron of larger area is evaporated.Finally, only remaining tungsten liquid residue is in tungsten crucible, and boron pruinescence is evaporated to gas completely, is scattered in the reactor chamber.After discharge off, treat that electric arc reaction chamber cools down, open argon valve 7, pass into argon to normal pressure, under argon shield, collect the flue dust of boron nano material.Finally obtain about 34.6 grams of boron ashes.
Embodiment 2
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps:
(1) prepare mixture of powders: boron powder and tungsten powder powder are mixed for 1:1 by volume, prepare mixture of powders；
(2) in the reaction chamber of arc discharge device, pure tungsten negative electrode is installed and multilayer anode, described multilayer anode and pure tungsten negative electrode are all connected with power supply；The mixture of powders of preparation in step (1) is loaded tungsten crucible, and with the mixed electrode that tablet machine compacting is made；
(3) described reaction chamber is bled, make the air pressure in reaction chamber lower than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, first initial current is regulated to 10 amperes, then the distance of pure tungsten negative electrode and multilayer anode is regulated, when making pure tungsten negative electrode and multilayer anode 10mm apart, continue to regulate electric current to 170 amperes, voltage is 50 volts, keeps discharge current and voltage stabilization in discharge process；
(5), after end to be discharged, under argon gas is protected, in reaction chamber, collect product namely obtain boron nano material.
Embodiment 3
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps:
(1) prepare mixture of powders: boron powder and tungsten powder powder are mixed for 10:1 by volume, prepare mixture of powders；
(2) in the reaction chamber of arc discharge device, pure tungsten negative electrode is installed and multilayer anode, described multilayer anode and pure tungsten negative electrode are all connected with power supply；The mixture of powders of preparation in step (1) is loaded tungsten crucible, and with the mixed electrode that tablet machine compacting is made；
(3) described reaction chamber is bled, make the air pressure in reaction chamber lower than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, first initial current is regulated to 10 amperes, then the distance of pure tungsten negative electrode and multilayer anode is regulated, when making pure tungsten negative electrode and multilayer anode 12mm apart, continue to regulate electric current to 175 amperes, voltage is 50 volts, keeps discharge current and voltage stabilization in discharge process；
(5), after end to be discharged, under argon gas is protected, in reaction chamber, collect product namely obtain boron nano material.
Embodiment 4
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps:
(1) prepare mixture of powders: boron powder and tantalum powder powder are mixed for 4:1 by volume, prepare mixture of powders；
(2) in the reaction chamber of arc discharge device, pure tungsten negative electrode is installed and multilayer anode, described multilayer anode and pure tungsten negative electrode are all connected with power supply；The mixture of powders of preparation in step (1) is loaded tungsten crucible, and with the mixed electrode that tablet machine compacting is made；
(3) described reaction chamber is bled, make the air pressure in reaction chamber lower than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, first initial current is regulated to 10 amperes, then the distance of pure tungsten negative electrode and multilayer anode is regulated, when making pure tungsten negative electrode and multilayer anode 8mm apart, continue to regulate electric current to 160 amperes, voltage is 50 volts, keeps discharge current and voltage stabilization in discharge process；
(5), after end to be discharged, under argon gas is protected, in reaction chamber, collect product namely obtain boron nano material.
Specifically, take 40 grams of boron powder and 80 grams of tantalum powder carry out Homogeneous phase mixing, prepare mixture of powders, now the volume ratio of boron powder and tantalum powder is about 4:1, mixture of powders is loaded tungsten crucible (diameter 50mm height 20mm), and uses tablet machine compacting, make boron powder and the mixed electrode of tantalum powder.Carry out arc discharge according to the method in embodiment 1, be made for boron nano material 35.7 grams.
Embodiment 5
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps:
(1) prepare mixture of powders: boron powder and rhenium powder powder are mixed for 4:1 by volume, prepare mixture of powders；
(2) in the reaction chamber of arc discharge device, pure tungsten negative electrode is installed and multilayer anode, described multilayer anode and pure tungsten negative electrode are all connected with power supply；The mixture of powders of preparation in step (1) is loaded tungsten crucible, and with the mixed electrode that tablet machine compacting is made；
(3) described reaction chamber is bled, make the air pressure in reaction chamber lower than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, first initial current is regulated to 10 amperes, then the distance of pure tungsten negative electrode and multilayer anode is regulated, when making pure tungsten negative electrode and multilayer anode 8mm apart, continue to regulate electric current to 160 amperes, voltage is 50 volts, keeps discharge current and voltage stabilization in discharge process；
(5), after end to be discharged, under argon gas is protected, in reaction chamber, collect product namely obtain boron nano material.
Specifically, take 80 grams of rhenium powder of 40 grams of boron powder and carry out Homogeneous phase mixing, prepare mixture of powders, the volume ratio of boron powder and rhenium powder is about 4:1, mixture of powders is loaded tungsten crucible (diameter 50mm height 20mm), and uses tablet machine compacting, make boron powder and the mixed electrode of rhenium powder.According to embodiment 1 method carry out arc discharge, be made for boron nano material 33.6 grams.
Tungsten powder in above-described embodiment can replace with any one in tantalum or rhenium powder.
Boron powder and high boiling point metal dust in above-described embodiment can also be that 1～10:1 mixes by volume, prepare mixture of powders.
Claims (2)
1. the method that an arc discharge prepares boron nano material, it is characterised in that comprise the following steps:
(1) prepare mixture of powders: be that 1～10:1 mixes by volume boron powder and high boiling point metal dust, prepare mixture of powders；
(2) in the reaction chamber of arc discharge device, pure tungsten negative electrode is installed and multilayer anode, described multilayer anode and pure tungsten negative electrode are all connected with power supply；The mixed electrode that described multilayer anode is mixture of powders and tungsten crucible is made；
(3) described reaction chamber is bled, make the air pressure in reaction chamber lower than 0.0001Pa, then pass to working gas；
(4) switch on power and carry out arc discharge, first initial current is regulated to 10 amperes, then the distance of pure tungsten negative electrode and multilayer anode is regulated, when making pure tungsten negative electrode and multilayer anode 8～12mm apart, continue to regulate electric current to 160～175 amperes, voltage remains 50 volts, keeps discharge current and voltage stabilization in discharge process；
(5), after end to be discharged, under argon gas is protected, in reaction chamber, product is collected.
2. the method that a kind of arc discharge according to claim 1 prepares boron nano material, it is characterised in that: described high boiling point metal dust is any one in tungsten, tantalum or rhenium powder.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107511487A (en) * | 2017-08-22 | 2017-12-26 | 西北工业大学 | The preparation method of multi-principal elements alloy nano particle |
| CN108043345A (en) * | 2017-12-29 | 2018-05-18 | 苏州大学 | Arc discharge device and the method that boron nitride nano-tube is prepared using the device |
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| KR101193818B1 (en) * | 2011-08-31 | 2012-10-23 | 한국기계연구원 | Method for fabricating amorphous boron powder by plasma arc discharge |
| CN102849752A (en) * | 2012-08-28 | 2013-01-02 | 浙江大学 | Preparation method of boron nano-particles |
| CN104743530A (en) * | 2015-03-31 | 2015-07-01 | 盐城工学院 | Method for preparing boron nitride nano-fibres by virtue of arc discharge |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101193818B1 (en) * | 2011-08-31 | 2012-10-23 | 한국기계연구원 | Method for fabricating amorphous boron powder by plasma arc discharge |
| CN102849752A (en) * | 2012-08-28 | 2013-01-02 | 浙江大学 | Preparation method of boron nano-particles |
| CN104743530A (en) * | 2015-03-31 | 2015-07-01 | 盐城工学院 | Method for preparing boron nitride nano-fibres by virtue of arc discharge |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107511487A (en) * | 2017-08-22 | 2017-12-26 | 西北工业大学 | The preparation method of multi-principal elements alloy nano particle |
| CN108043345A (en) * | 2017-12-29 | 2018-05-18 | 苏州大学 | Arc discharge device and the method that boron nitride nano-tube is prepared using the device |
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