CN105731480B - A kind of method that arc discharge prepares boron nano material - Google Patents
A kind of method that arc discharge prepares boron nano material Download PDFInfo
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- CN105731480B CN105731480B CN201610296932.4A CN201610296932A CN105731480B CN 105731480 B CN105731480 B CN 105731480B CN 201610296932 A CN201610296932 A CN 201610296932A CN 105731480 B CN105731480 B CN 105731480B
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- arc discharge
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- nano material
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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 present invention relates to a kind of method that arc discharge prepares boron nano material, and it belongs to a kind of method for preparing nano material.There is the technical problem that product purity is poor, preparation efficiency is low and yield is few for the method for the invention for mainly solving existing arc discharge preparation nano material.The technical scheme is that：A kind of method that arc discharge prepares boron nano material, it comprises the following steps：(1) it is 1~10 by volume boron powder and higher boiling metal dust:1 is mixed, and mixture of powders is made；(2) pure tungsten negative electrode is installed in the reaction chamber of arc discharge device and multilayer anode, multilayer anode and the pure tungsten negative electrode is connected with power supply；The multilayer anode is mixed electrode made of mixture of powders and tungsten crucible；(3) to the reaction chamber pumping, working gas is then passed to；(4) switch on power and carry out arc discharge, discharge current and voltage stabilization are kept in discharge process；(5) after end to be discharged, product is collected in reaction chamber under argon gas protection.
Description
Technical field
The present invention relates to a kind of method that arc discharge prepares boron nano material, and it belongs to a kind of side for preparing nano material
Method.
Background technology
Arc discharge is a kind of method of conventional preparation nano material.Relative to laser ablation and chemical deposition,
Its cost is cheap, is adapted to a large amount of productions, has become the prefered method for preparing nano material.At present, it is widely used to make
Standby high boiling carbon nanomaterial, including fullerene, metal fullerene, CNT etc..Carbon nanometer material is prepared in arc discharge
In the technique of material, using the graphite electrode or admixed graphite electrode of conduction as carbon source.In arc discharge, graphite electrode conduct
Consumable anode vapor deposition at a high temperature of produced by electric arc, generate carbon nanomaterial.
But for being equally high boiling boron material (3927 DEG C of boiling point), because nature does not deposit the pure boron of conduction
Material, the consumable anode of pure boron simple substance can not be directly made, thus can not be by preparing boron nano material with method as carbons.
On the other hand, primary raw material of the chemical gaseous phase depositing process when preparing boron nano material is highly toxic boronation hydrogen, this
The specially treated of the high-air-tightness and reaction end gas of equipment is needed, huge difficulty is encountered in technique, is rarely employed at present.
Therefore, arc discharge method is still the prefered method for preparing a large amount of boron nano materials.
In order that boron material can prepare nano material by arc discharge, ZL201510146897.3 discloses " a kind of
The method that boron nitride nanometer fiber is prepared using arc discharge ", this method is used being hollowed out among graphite electrode, by a small amount of boron material
The nano material of boron is prepared in the embedded graphite electrode of material (boron nitride).Although this method can produce boron nano material,
But it can generate a large amount of carbon nanomaterials while boron nano material is produced, and cause required boron nano material to be mixed in carbon
In material, it is difficult to separating-purifying.In addition, each graphite electrode center can only put a small amount of required boron material, preparation efficiency is low.
On the other hand, the method that conductive agent is added in boron powder can be taken, for example adds common conductive agent：Carbon black, nickel powder etc..But
It is that these conductive agents can equally evaporate become gas during the course of the reaction, or even compound is formed with boron element, gives birth in the product
Into a large amount of impurity compositions.
The content of the invention
Present invention aim to address existing arc discharge prepare nano material method there is product purity it is poor, preparation
Efficiency is low and the few technical problem of yield, there is provided a kind of method that arc discharge prepares boron nano material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of method that arc discharge prepares boron nano material, it comprises the following steps：
(1) mixture of powders is prepared：It is 1~10 by volume boron powder and higher boiling metal dust:1 is mixed, system
Obtain mixture of powders；
(2) pure tungsten negative electrode and multilayer anode, the multilayer anode and pure tungsten are installed in the reaction chamber of arc discharge device
Negative electrode is connected with power supply；The multilayer anode is mixed electrode made of mixture of powders and tungsten crucible；
(3) to the reaction chamber pumping, the air pressure in reaction chamber is less than 0.0001Pa, then pass to working gas；
(4) switch on power and carry out arc discharge, adjust initial current first to 10 amperes, then adjust pure tungsten negative electrode with mixing
The distance of Heyang pole, when making pure tungsten negative electrode with multilayer anode at a distance of 8~12mm, continue to adjust electric current to 160~175 amperes, electricity
Pressure remains 50 volts, and discharge current and voltage stabilization are kept in discharge process；
(5) after end to be discharged, product is collected in reaction chamber under argon gas protection.
Further, the higher boiling metal dust is any one in tungsten, tantalum or rhenium powder.
The present invention uses above-mentioned technical proposal, and making consumable anode, the high current under the conduction of metal dust is put with pure tungsten negative electrode
Electricity, the high temperature of generation cause boron powder progressively to melt and gasify, the nano material of finally deposition generation boron, and high boiling Metal Substrate
This does not gasify, and is retained in crucible, solve existing arc discharge prepare the method for nano material there is product purity it is poor, make
Standby efficiency is low and the few technical problem of yield.Therefore, compared with background technology, the present invention has that technical process is simple, product is pure
Degree is high and produces the advantages of big.
Brief description of the drawings
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 gas air valve, 8, vacuum valve, 9, negative electrode step-by-step system.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
Embodiment 1
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps：
(1) mixture of powders is prepared：It is 4 by volume boron powder and tungsten powder powder:1 is mixed, and powder mixing is made
Thing；
(2) pure tungsten negative electrode and multilayer anode, the multilayer anode and pure tungsten are installed in the reaction chamber of arc discharge device
Negative electrode is connected with power supply；The mixture of powders prepared in step (1) is loaded into tungsten crucible, and mixed made of tablet press machine is compacted
Composite electrode；
(3) to the reaction chamber pumping, the air pressure in reaction chamber is less than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, adjust initial current first to 10 amperes, then adjust pure tungsten negative electrode with mixing
The distance of Heyang pole, when making pure tungsten negative electrode with multilayer anode at a distance of 8mm, continue to adjust electric current to 160 amperes, voltage is 50 volts
Spy, discharge current and voltage stabilization are kept in discharge process；
(5) after end to be discharged, collection product produces boron nano material in reaction chamber under argon gas protection.
Specifically, 40 grams of boron powder and 80 grams of tungsten powder ground and mixeds are uniformly obtained boron powder and tungsten powder mixture of powders 1, now
The volume ratio of boron powder and tungsten powder is about 4:1.Above-mentioned mixture of powders 1 is loaded tungsten crucible 2 (the high 20mm of diameter 50mm), and with pressure
Mixed electrode made of the compacting of piece machine, the resistance on measurement tungsten crucible surface and mixture of powders surface is 1.67m Ω；By tungsten crucible
Mixed electrode is placed on the anode conducting plate 3 in the reaction chamber 5 of arc discharge device, reaction chamber 5 is closed, being arranged on electric arc
The pure tungsten negative electrode 4 of the top of reaction chamber 5 of electric discharge device is directed at tungsten crucible mixed electrode center and is brought into close contact.Open vavuum pump,
The vacuum valve 8 that reaction chamber 5 is connected with vavuum pump is opened, reaction chamber is vacuumized.When air pressure is less than 4Pa, open cold
But water system 6, molecular pump is opened, continues to vacuumize, when air pressure is less than 0.0001Pa, closed reaction chamber 5 and be connected with vavuum pump
Vacuum valve 8, stop vacuumizing.Argon gas air valve 7 is slowly opened, certain argon gas is filled with into reaction chamber.Switch on power, adjust
Current knob, increase initial current adjust the height of pure tungsten negative electrode with negative electrode step-by-step system 9, make mixed electrode to 10 amperes
Disengaged with pure tungsten negative electrode, distance about 8mm.Some arc sparks are now produced between mixed electrode and tungsten cathode.Continue
Regulation electric current reaches 160 amperes, and voltage is 50 volts, now form powerful electric field between mixed electrode and pure tungsten negative electrode and
Electric discharge is produced, temperature is reached more than 4000 DEG C.The local temperature of mixed electrode constantly raises so that boron powder and tungsten powder melt in succession
Change, temperature continues to raise, and boron gas, which is evaporated, to be flown out, and the volume of tungsten liquid constantly increases, and the boron in bigger region is evaporated.
Finally, only in tungsten crucible, boron powder is vaporized completely as gas remaining tungsten liquid residue, is scattered in the reactor chamber.Discharge off
Afterwards, treat that electric arc reaction chamber cools down, open argon gas valve 7, be passed through argon gas to normal pressure, boron nano material is collected under argon gas protection
Cigarette ash.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) mixture of powders is prepared：It is 1 by volume boron powder and tungsten powder powder:1 is mixed, and powder mixing is made
Thing；
(2) pure tungsten negative electrode and multilayer anode, the multilayer anode and pure tungsten are installed in the reaction chamber of arc discharge device
Negative electrode is connected with power supply；The mixture of powders prepared in step (1) is loaded into tungsten crucible, and mixed made of tablet press machine is compacted
Composite electrode；
(3) to the reaction chamber pumping, the air pressure in reaction chamber is less than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, adjust initial current first to 10 amperes, then adjust pure tungsten negative electrode with mixing
The distance of Heyang pole, when making pure tungsten negative electrode with multilayer anode at a distance of 10mm, continue to adjust electric current to 170 amperes, voltage is 50 volts
Spy, discharge current and voltage stabilization are kept in discharge process；
(5) after end to be discharged, collection product produces boron nano material in reaction chamber under argon gas protection.
Embodiment 3
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps：
(1) mixture of powders is prepared：It is 10 by volume boron powder and tungsten powder powder:1 is mixed, and powder mixing is made
Thing；
(2) pure tungsten negative electrode and multilayer anode, the multilayer anode and pure tungsten are installed in the reaction chamber of arc discharge device
Negative electrode is connected with power supply；The mixture of powders prepared in step (1) is loaded into tungsten crucible, and mixed made of tablet press machine is compacted
Composite electrode；
(3) to the reaction chamber pumping, the air pressure in reaction chamber is less than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, adjust initial current first to 10 amperes, then adjust pure tungsten negative electrode with mixing
The distance of Heyang pole, when making pure tungsten negative electrode with multilayer anode at a distance of 12mm, continue to adjust electric current to 175 amperes, voltage is 50 volts
Spy, discharge current and voltage stabilization are kept in discharge process；
(5) after end to be discharged, collection product produces boron nano material in reaction chamber under argon gas protection.
Embodiment 4
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps：
(1) mixture of powders is prepared：It is 4 by volume boron powder and tantalum powder powder:1 is mixed, and powder mixing is made
Thing；
(2) pure tungsten negative electrode and multilayer anode, the multilayer anode and pure tungsten are installed in the reaction chamber of arc discharge device
Negative electrode is connected with power supply；The mixture of powders prepared in step (1) is loaded into tungsten crucible, and mixed made of tablet press machine is compacted
Composite electrode；
(3) to the reaction chamber pumping, the air pressure in reaction chamber is less than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, adjust initial current first to 10 amperes, then adjust pure tungsten negative electrode with mixing
The distance of Heyang pole, when making pure tungsten negative electrode with multilayer anode at a distance of 8mm, continue to adjust electric current to 160 amperes, voltage is 50 volts
Spy, discharge current and voltage stabilization are kept in discharge process；
(5) after end to be discharged, collection product produces boron nano material in reaction chamber under argon gas protection.
Specifically, take 40 grams of boron powder and 80 grams of tantalum powders uniformly to be mixed, mixture of powders is made, now boron powder and tantalum powder
Volume ratio be about 4:1, mixture of powders is loaded into tungsten crucible (the high 20mm of diameter 50mm), and be compacted with tablet press machine, boron is made
The mixed electrode of powder and tantalum powder.Arc discharge is carried out according to the method in embodiment 1,35.7 grams of boron nano material has been made.
Embodiment 5
The method that a kind of arc discharge in the present embodiment prepares boron nano material, it comprises the following steps：
(1) mixture of powders is prepared：It is 4 by volume boron powder and rhenium powder powder:1 is mixed, and powder mixing is made
Thing；
(2) pure tungsten negative electrode and multilayer anode, the multilayer anode and pure tungsten are installed in the reaction chamber of arc discharge device
Negative electrode is connected with power supply；The mixture of powders prepared in step (1) is loaded into tungsten crucible, and mixed made of tablet press machine is compacted
Composite electrode；
(3) to the reaction chamber pumping, the air pressure in reaction chamber is less than 0.0001Pa, then pass to argon gas；
(4) switch on power and carry out arc discharge, adjust initial current first to 10 amperes, then adjust pure tungsten negative electrode with mixing
The distance of Heyang pole, when making pure tungsten negative electrode with multilayer anode at a distance of 8mm, continue to adjust electric current to 160 amperes, voltage is 50 volts
Spy, discharge current and voltage stabilization are kept in discharge process；
(5) after end to be discharged, collection product produces boron nano material in reaction chamber under argon gas protection.
Specifically, take 40 grams of boron powder, 80 grams of rhenium powder uniformly to be mixed, the volume of mixture of powders, boron powder and rhenium powder is made
Than being about 4:1, mixture of powders is loaded into tungsten crucible (the high 20mm of diameter 50mm), and be compacted with tablet press machine, boron powder and rhenium is made
The mixed electrode of powder.According to embodiment 1 method carry out arc discharge, 33.6 grams of boron nano material has been made.
Tungsten powder in above-described embodiment can be replaced with any one in tantalum or rhenium powder.
Boron powder and higher boiling metal dust in above-described embodiment can also be 1~10 by volume:1 is mixed, system
Obtain mixture of powders.
Claims (2)
1. a kind of method that arc discharge prepares boron nano material, it is characterised in that comprise the following steps：
(1) mixture of powders is prepared：It is 1~10 by volume boron powder and higher boiling metal dust:1 is mixed, and powder is made
Last mixture；
(2) pure tungsten negative electrode and multilayer anode, multilayer anode and the pure tungsten negative electrode are installed in the reaction chamber of arc discharge device
It is connected with power supply；The multilayer anode is mixed electrode made of mixture of powders and tungsten crucible；
(3) to the reaction chamber pumping, the air pressure in reaction chamber is less than 0.0001Pa, then pass to working gas；
(4) switch on power and carry out arc discharge, adjust initial current first to 10 amperes, then adjust pure tungsten negative electrode with mixing sun
The distance of pole, when making pure tungsten negative electrode with multilayer anode at a distance of 8~12mm, continue to adjust electric current to 160~175 amperes, voltage is protected
Hold as 50 volts, discharge current and voltage stabilization are kept in discharge process；
(5) after end to be discharged, product is collected in reaction chamber under argon gas protection.
2. the method that a kind of arc discharge according to claim 1 prepares boron nano material, it is characterised in that：The height boiling
Point metal dust is any one in tungsten, tantalum or rhenium powder.
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| CN107511487B (en) * | 2017-08-22 | 2019-05-17 | 西北工业大学 | The preparation method of multi-principal elements alloy nano particle |
| CN108043345B (en) * | 2017-12-29 | 2020-04-21 | 苏州大学 | Arc discharge device and method for preparing boron nitride nanotube by using same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| A review on the methods of preparation of elemental boron;Jiaojiao Zhou,et al.;《ASIA-PACIFIC JOURNAL OF CHEMICAL ENGINEERING》;20150420;第10卷;325–338 * |
| Plasma arc Synthesis of Nano-Boron Towards the Synthesis of MgB2 Superconductors;B.B. Sinha,et al.;《J Supercond Nov Magn》;20121230;第26卷;1503–1506 * |
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