CN1943924A - Method for preparing nano particle by flash gasifying metal wire - Google Patents
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- CN1943924A CN1943924A CN 200510100256 CN200510100256A CN1943924A CN 1943924 A CN1943924 A CN 1943924A CN 200510100256 CN200510100256 CN 200510100256 CN 200510100256 A CN200510100256 A CN 200510100256A CN 1943924 A CN1943924 A CN 1943924A
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Abstract
The lightning gasifying method of preparing nanometer particle with metal wire is that inside a container with filled protecting gas, high voltage discharge produces lightning to gasify metal wire and to form nanometer particle through solidification. The said method may be used widely in continuous preparation of nanometer particle of metal, especially some noble metal and high smelting point metal, and in preparation of nanometer particle of metal alloy, intermetallic compound, metal oxide and metal nitride, in different industries. The prepared nanometer particle has homogeneous size distribution, high yield, no pollution and spherical shape.
Description
Technical field
The present invention relates to the preparation method of a kind of nano material and nano-powder.
Background technology
Nano material becomes the focus of world research and concern because of character such as its unusual electricity, magnetic, heat, power, optics, and the production in enormous quantities of nano powder focus, emphasis and difficult point especially.At present the method for the nano-powder of preparation metal and alloy thereof etc. has been said physical method and chemical method from big aspect, and physical method is as mechanical alloying method, sputtering method, plasma method, preparation such as laser composite algorithm metal nano powder.Said method productivity ratio is low, and output is little, and product purity is low, and size distribution is inhomogeneous, and the kind of producing metal nano powder is single, can not be as required the composite nano metallic material of production multiple components simultaneously in proportion at any time.Chemical method is as electrolysis, micro emulsion method, chemical plating reducing process, carbonyl thermal decomposition method etc., and the shortcoming of chemical method is to yield poorly, and the technology controlling and process complexity is produced difficulty in batches, and certain contaminative etc. is arranged.Therefore the method that develop that a kind of output is big, favorable repeatability, control simply prepares metal nano powder seems extremely important.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing high pressure to produce preparing nano particle by flash gasifying metal wire, to obtain the nano particle of even particle size distribution.
The present invention realizes above-mentioned purpose like this:
A kind of method of preparing nano particle by flash gasifying metal wire is characterized in that utilizing in being filled with the container of protective gas lightning that electrion produces that the wire after coagulation that gasifies is obtained nano particle.
The processing step of this method is:
A. adorn silk: suitable wire is sent in the reaction system, and selected suitable high-tension electricity voltage;
B. charge into protective gas: at first reaction system is vacuumized, then protective gas is charged in the reaction system, to the atmospheric pressure value of setting;
C. prepare nano particle: start reaction system, form high pressure between battery lead plate and the wire and produce lightning, the wire gasification is also solidified the formation nano particle in protective gas, and nano particle enters into gatherer with protective gas and collects;
D. passivation nano particle: unload gatherer, and put it in the passivation case that is filled with protective gas.
Wherein related relevant parameter is 10-35KV for high-tension electricity voltage, and wire diameter is 0.1-0.8mm, and wire length is 3-12cm, and the air pressure of protective gas is 1 * 10
5-1 * 10
6Pa.
In addition, described protective gas is inert gas or inert gas and oxygen mix body or inert gas and ammonia mixture.
The invention has the beneficial effects as follows: this method can realize the continuity preparation to various extending nano particles for thread metal, the particularly preparation of the nano particle of some noble metal and high-melting point metal, simultaneously can realize metal alloy, intermetallic compound, metal oxide, the nano particle preparation of metal nitride.Realize using different metal to prepare the corresponding metal nano powder, adopt the related process parameter that sets of the present invention, the granularity of the nano particle that is obtained is less and distribution is more even, and productive rate height, particle are the zero defect sphere; Adopt different protective gas can obtain the very high nano particle of purity according to different metals in addition, and adding oxygen can directly use metal simple-substance to prepare the very high metal oxide nanoparticles of purity in the inert gas.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples:
Fig. 1 is the structural representation of reaction system involved in the present invention;
Fig. 2 is the connection diagram of circuit control system of the present invention;
Fig. 3 is the transmission electron microscope photo of the prepared aluminium oxide nano particle of the present invention;
Fig. 4 is the transmission electron microscope photo of the prepared nickel nano particle of the present invention.
The specific embodiment
A kind of method of preparing nano particle by flash gasifying metal wire, the lightning that utilizes high pressure to spark in being filled with the container of protective gas to be produced obtains nano particle with the wire after coagulation that gasifies.
With reference to Fig. 1, Fig. 2, the reaction system that the method for preparing nano particle by flash gasifying metal wire is related comprises reative cell 1, protective gas system 2, circulating collection system 3, advances a system 4, air-conditioning system 5 and circuit control system 6.Wherein protective gas system 2 comprises vacuum system 21 and gas charging system 22; vacuum system 21 is connected with circulating collection system 3 respectively with gas charging system 22; because the atmosphere of course of reaction will have influence on the purity that obtains nano particle, utilize vacuum system 21 to charge into protective gas by gas charging system 22 as required with after the purifying of circulating collection system 3 and reative cell 1.Circulating collection system 3 can be divided into the circulatory system 31 and gatherer 32, and circulating collection system 3 is connected with reative cell 1, and the circulatory system 31 is sent protective gas to reative cell 1, the nano particle of reaction acquisition is sent into gatherer 32 collect.Enter a system 4 and wire is sent into constantly continuity prepares nano particle in the reactor 1.Air-conditioning system 5 is operating temperature and the humidity that is used to the equipment that guarantees.The circuit loop that circuit control system 6 is in turn connected to form for 1 wire in power supply 61, gauge tap 62, high pressure generator 63, current transformer 64, high-voltage capacitance 65, battery lead plate 66, the reative cell etc.
The processing step of preparing nano particle by flash gasifying metal wire is as follows:
E. adorn silk.The metal nanoparticle that obtains is selected the wire of suitable material as required, and its length is that 3-12cm, diameter are 0.1-0.8mm.If the metal filament length is long, diameter range is excessive, disposable gained nano particle is too much, easily reunites, and is too short, yields poorly; On the contrary,, can cause yielding poorly, therefore be chosen in and to satisfy the littler nano particle of preparation size in this scope and guarantee output if wire length and diameter are too small.Wire is installed on an into system 4, and sends in the reative cell 1.Regulate that wire is aimed at battery lead plate 66 and wire and battery lead plate 66 between distance, enclosed reaction chamber 1, and adjusting high-tension electricity voltage.Because the fusing point difference of different metal silk, according to the granularity of selected wire kind and needs acquisition nano particle, selecting high-tension electricity voltage is 10-35KV, and the nano particle yardstick that obtains in this voltage range like this is littler.
F. charge into protective gas.The vacuum system of at first opening in the protective gas system 2 21 vacuumizes, and to the vacuum of setting, closes vacuum system then, opens gas charging system 22, and protective gas is imported in circulating collection system 3 and the reative cell 1.Described as required protective gas can be inert gas, inert gas and oxygen mix body, inert gas and ammonia mixture.Because the air pressure of protective gas also can have influence on the nano particle granularity: air pressure is excessive, and the nano particle of preparation is easily collecting not, but granularity is less relatively; Reverse pressure is too small, and the nano particle of formation is easily reunited, and therefore works as protective gas pressure and reaches 1 * 10
5-1 * 10
6Close gas charging system 22 behind the Pa.Start air-conditioning system 5, to guarantee the operating temperature and the humidity of equipment.
G. prepare nano particle.Open the circulatory system 31; allow protective gas circulation in circulating collection system 3 and reative cell 1; open circuit control system 6; between battery lead plate and wire, produce high pressure and produce lightning; with wire gasification and solidify the formation nano particle in protective gas, nano particle enters into gatherer 32 with protective gas and collects.
H. passivation nano particle.Unload gatherer 32, and put it in the passivation case that is filled with protective gas.
With specific embodiment technological parameter of the present invention is elaborated below.
Embodiment one: with diameter is that the high-purity aluminium wire of 0.35mm places in the system 4, and regulating the aluminium wire respective length is 8cm, and charging into protective gas is inert gas and oxygen mix body, and pressure is 4 * 10
5Pa, operating voltage is 10KV, the high pressure lightning of generation makes aluminium wire gasification, and the aluminium nano particle generates the preparation of aluminium oxide realization to nano particle with oxygen reaction.Nano particle is collected behind the cooling passivation of protective gas, circulation classification can obtain aluminium oxide nano micro mist product.With reference to Fig. 3, be the transmission electron microscope photo of the prepared aluminium oxide nano particle of present embodiment.
Embodiment two: with diameter is that the high-purity titanium silk of 0.38mm places in the system 4, and regulating titanium silk respective length is 6cm, and charging into protective gas is inert gas and ammonia mixture, and pressure is 2 * 10
5Pa, operating voltage is 15KV, the high pressure lightning of generation makes the gasification of titanium silk, realizes the preparation to nano particle.Nano particle is collected behind the cooling passivation of protective gas, circulation classification can obtain titanium nitride nano micro mist product.
Embodiment three: with diameter is that the high-purity copper wire of 0.38mm places in the system 4, and regulating the copper wire respective length is 7cm, and charging into protective gas is inert gas, and pressure is 7 * 10
5Pa, operating voltage is 20KV, the high pressure lightning of generation makes the copper wire gasification, realizes the preparation to nano particle.Nano particle is collected behind the cooling passivation of protective gas, circulation classification can obtain copper nano powder product.
Embodiment four: with diameter is that the high-purity filamentary silver of 0.7mm places in the system 4, and regulating the filamentary silver respective length is 12cm, and charging into protective gas is inert gas, and pressure is 5 * 10
5Pa, operating voltage is 30KV, the high pressure lightning of generation makes the filamentary silver gasification, realizes the preparation to nano particle.Nano particle is collected behind the cooling passivation of protective gas, circulation classification can obtain silver-colored nano powder product.
Embodiment five: with diameter is that the high-purity nickel wire of 0.38mm places in the system 4, and regulating the nickel wire respective length is 8cm, and charging into protective gas is inert gas, and pressure is 3 * 10
5Pa, operating voltage is 26KV, the high pressure lightning of generation makes the nickel wire gasification, realizes the preparation to nano particle.Nano particle is collected behind the cooling passivation of protective gas, circulation classification can obtain nickel nano powder product.With reference to Fig. 4, be the transmission electron microscope photo of the prepared nickel nano particle of present embodiment.
Claims (7)
1. the method for a preparing nano particle by flash gasifying metal wire is characterized in that utilizing in being filled with the container of protective gas lightning that electrion produces that the wire after coagulation that gasifies is obtained nano particle.
2. the method for a kind of preparing nano particle by flash gasifying metal wire according to claim 1 is characterized in that comprising following processing step:
A. adorn silk: suitable wire is sent in the reaction system, and selected suitable high-tension electricity voltage;
B. charge into protective gas: at first reaction system is vacuumized, then protective gas is charged in the reaction system, to the atmospheric pressure value of setting;
C. prepare nano particle: start reaction system, form high pressure between battery lead plate and the wire and produce lightning, the wire gasification is also solidified the formation nano particle in protective gas, and nano particle enters into gatherer with protective gas and collects;
D. passivation nano particle: unload gatherer, and put it in the passivation case that is filled with protective gas.
3. the method for a kind of preparing nano particle by flash gasifying metal wire according to claim 2 is characterized in that described high-tension electricity voltage is 10-35KV.
4. the method for a kind of preparing nano particle by flash gasifying metal wire according to claim 2 is characterized in that wire diameter is 0.1-0.8mm.
5. the method for a kind of preparing nano particle by flash gasifying metal wire according to claim 2 is characterized in that wire length is 3-12cm.
6. the method for a kind of preparing nano particle by flash gasifying metal wire according to claim 2, the air pressure that it is characterized in that protective gas is 1 * 10
5-1 * 10
6Pa.
7. the method for a kind of preparing nano particle by flash gasifying metal wire according to claim 1 and 2 is characterized in that described protective gas is inert gas or inert gas and oxygen mix body or inert gas and ammonia mixture.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105234424A (en) * | 2015-10-12 | 2016-01-13 | 湖南金旺铋业股份有限公司 | Process for producing nanometer sliver powder through electric-arc furnace evaporating method |
CN107275652A (en) * | 2017-06-30 | 2017-10-20 | 佛山市能翼科技有限公司 | catalyst, preparation method and zinc-air battery |
CN107520457A (en) * | 2016-06-20 | 2017-12-29 | 张家港市华舰五金工具有限公司 | The preparation method of monel nano powder |
CN107520458A (en) * | 2016-06-20 | 2017-12-29 | 张家港市华舰五金工具有限公司 | A kind of preparation method of nickel nano powder |
CN107520456A (en) * | 2016-06-20 | 2017-12-29 | 张家港市华舰五金工具有限公司 | The preparation method of copper nano |
-
2005
- 2005-10-04 CN CN 200510100256 patent/CN1943924A/en active Pending
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105234424A (en) * | 2015-10-12 | 2016-01-13 | 湖南金旺铋业股份有限公司 | Process for producing nanometer sliver powder through electric-arc furnace evaporating method |
CN107520457A (en) * | 2016-06-20 | 2017-12-29 | 张家港市华舰五金工具有限公司 | The preparation method of monel nano powder |
CN107520458A (en) * | 2016-06-20 | 2017-12-29 | 张家港市华舰五金工具有限公司 | A kind of preparation method of nickel nano powder |
CN107520456A (en) * | 2016-06-20 | 2017-12-29 | 张家港市华舰五金工具有限公司 | The preparation method of copper nano |
CN107275652A (en) * | 2017-06-30 | 2017-10-20 | 佛山市能翼科技有限公司 | catalyst, preparation method and zinc-air battery |
CN107275652B (en) * | 2017-06-30 | 2021-05-07 | 佛山市能翼科技有限公司 | Catalyst, preparation method and zinc-air battery |
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