CN1382547A - Equipment for preparing nano metal powder - Google Patents

Equipment for preparing nano metal powder Download PDF

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Publication number
CN1382547A
CN1382547A CN 02110837 CN02110837A CN1382547A CN 1382547 A CN1382547 A CN 1382547A CN 02110837 CN02110837 CN 02110837 CN 02110837 A CN02110837 A CN 02110837A CN 1382547 A CN1382547 A CN 1382547A
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China
Prior art keywords
particle
pipeline
controller
housing
particle controller
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Granted
Application number
CN 02110837
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Chinese (zh)
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CN1203948C (en
Inventor
陈钢强
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Jiangsu Bo move new materials Limited by Share Ltd
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NINGBO GUANGBO NANOMETER MATERIAL CO Ltd
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Priority to CN 02110837 priority Critical patent/CN1203948C/en
Publication of CN1382547A publication Critical patent/CN1382547A/en
Application granted granted Critical
Publication of CN1203948C publication Critical patent/CN1203948C/en
Anticipated expiration legal-status Critical
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Abstract

An equipment for preparing metallic nanoparticles is composed of a casing with internal refractory liner, plasma gun arranged at upper part of said casing, the crucible containing melten metal arranged at lower part of said casing, particle controller, particle collector, evaporator and MF induction coil in the evaporator. Its advantages are simple structure, high output and easy control of granularity.

Description

Produce the Nano metal powder device
Technical field
The present invention relates to a kind of production nano metal powder device technique field.
Background technology
New material is one of the most active field of current development in science and technology, and key industry developed country is all the emphasis of new material research as scientific and technological progress and economic development in the world.Nano material is because the particle scale microminiaturization, the common material that millimeter or micrometer structure particle constituted during its reaction to light, electricity, mechanical stress was different from exceeds 5 times nanometer copper, the nano ceramics that does not fall broken, strength ratio iron and steel as intensity and exceeds 100 times appearance in succession such as CNT.Granularity is less than the superfine metal material of 100 nanometers, has all size premium properties that material is beyond one's reach, at powder metallurgy, fine chemistry industry, there is wide prospect in fields such as electronic information, the method of producing nano metal powder now mainly contains chemical method and physical method, each advantage and limitation are respectively arranged, chemical method such as electrolysis, the carbonyl thermal decomposition method, water slurry pressurised oxygen reducing process etc., generally can not produce fairly largely, certain contaminative is arranged, the physics method has laser method and plasma method, general transferred-arc plasma method is to operate under higher vacuum, and there is not the particle control device, yield poorly so have, particle is grown up and is not easy, shortcomings such as size distribution is bigger, especially at electron trade such as circuit, needing in the coating of electronic elements is the above metal dust of hundreds of nanometer, to prevent nanoparticle agglomerates, the metal nanoparticle of such range scale adopts chemical method and general laser method to obtain not too easily.In the Chinese patent literature storehouse, concentrate report nano metal particles production method morely, few for the process units report of producing the metal nanoparticle powder in enormous quantities, it as the patent No. 00233180.2 Chinese patent " a kind of process units of nano metal ", it is by the discharge-induced explosion tube, valve, cooler, vacuum blower, conveyance conduit, a separation bin, backwind tube, No. two separation bins, No. three separation bins, packing case, support), console, vavuum pump, motor constitutes, it is characterized in that: the discharge-induced explosion tube is by shell, two end cap constitutes a cylindrical shell, be arranged with A within it, B, C chamber and chamber, top, at B, C is provided with inner casing in the chamber, the middle cooling layer that forms, on the B chamber, be provided with delivery outlet, peep hole, return-air hole, vacuumize the hole, funnel, be provided with charging tray in the A chamber of discharge-induced explosion tube, support, cathode terminal, conduit, charging tray is hubbed on the support, cathode carrier in cathode terminal and the B chamber connects, and conduit is installed on the dividing plate between A chamber and the B chamber; In the B chamber, be provided with cathode carrier, cathode taps, insulator, insulator, positive plate, establish cathode taps on the cathode carrier in the B chamber, distance between positive plate and the cathode taps is adjustable, positive plate is located on the anode conducting post, go up sheathed insulator for one section of the close positive plate of anode conducting post, another section is sealed insulator; Connect the damping discharge frame between the anode conducting post in the C chamber, the arcing distance of damping discharge frame is adjustable, sheathed insulator on the anode conducting post of close incoming call one side in the C chamber; In the chamber, top, be provided with insulator and anode terminal, seal insulator on the anode conducting post that anode terminal was communicated with; The discharge-induced explosion tube places on the support, its delivery outlet and valve join, valve is connected with chimney cooler, the other end of cooler connects conveyance conduit, the conveyance conduit other end is connected with the air admission hole of a separation bin, No. one the separation bin lower end is provided with vacuum packaging box, its upper end is provided with venthole and connects conveyance conduit, the conveyance conduit other end connects the air admission hole that valve connects No. two separation bins again, herewith connect separation bin No. three, the venthole of No. three separation bin upper ends connects valve again, valve is connected with backwind tube again, the other end of backwind tube links to each other with vacuum blower, vacuum blower links to each other with conveyance conduit again, and the other end of conveyance conduit is connected with the return-air hole of discharge-induced explosion tube again, forms the operating path of a circulation.Its shortcoming is the process units more complicated, and the nano particle yardstick of producing distributes than broad, and output is big inadequately etc.
The inventor is that 01246486.4 Chinese patent " is produced the Nano metal powder device " and at length reported new production Nano metal powder device at number of patent application for this reason, it is mounted with plasma gun on the top of the housing of high-temperature resistant material of inner lining, the bottom is mounted with the crucible that contains metal liquid and has constituted evaporimeter accordingly, while housing also opening is connected with particle controller, another outlet of particle controller is connected with particle collector, particle collector has discharging opening and gaseous phase outlet, gaseous phase outlet is by the loop head of pipeline and pump difference body contact body and particle controller, it has simple in structure, output is big, granularity is controlled advantage easily, promotes the use of industrial having obtained.Use in practice and show that also there is following deficiency in it:
When 1, plasma began the heating igniting, programming rate was too fast, was difficult to the control rate of warming, caused ceramic crucible to break easily, influenced the equipment ordinary production and used;
When 2, using plasma heats, improve the restriction that the evaporation of metals amount often is subjected to plasma heating power size, and in order to improve the evaporation of metal amount, adopt under the big current work situation, the life-span of plasma gun just shortens greatly.
Summary of the invention
First purpose of the present invention with regard to be to provide at above-mentioned prior art present situation a kind of relatively simple for structure, production output is big, the particle size production Nano metal powder device of control easily.
Further object of the present invention is to provide a kind of production Nano metal powder device of further improved, and it can avoid the too fast crucible that causes of evaporimeter intensification to break, and improves the evaporation of metal amount simultaneously, avoids the problem that causes the plasma gun life-span to shorten greatly again.
First purpose of the present invention is achieved in that this kind production Nano metal powder device, it is characterized in that being mounted with plasma gun on the top of the housing of high-temperature resistant material of inner lining, the bottom is mounted with the crucible that contains metal liquid accordingly, while housing also opening is connected with particle controller, another outlet of particle controller is connected with particle collector, particle collector has discharging opening and gaseous phase outlet, and gaseous phase outlet is by the loop head of pipeline and pump difference body contact body and particle controller.
Above-mentioned particle controller is a pipeline, is distributed with gas distribution grid in the pipeline, and the loop head of gas distribution grid and particle controller is connected.
Further object of the present invention is achieved in that housing has been installed the Medium frequency induction coil in evaporimeter on above-mentioned technical scheme basis.
Compared with prior art, the invention has the advantages that the transferred-arc plasma method that adopts, can be pressed onto under 0.5 atmospheric pressure at 1.2 atmosphere and operate, so the metallic vapour evaporation capacity is big, can reach big output, and particle is grown easily, under the particle controller effect, obtain the nano metal powder of narrower particle size distribution, and particle size can reach tens to several thousand nanometers, artificially control, referring to table 1, be easy to obtain each type oxide, nitride and carbide particle according to feeding the gas difference, and simple in structure, make easily.In evaporimeter, be provided with the Medium frequency induction coil especially and assist heating, in the firing up stage, only use the Medium frequency induction coil to heat, can control programming rate, by the time after being heated to uniform temperature, open the plasma heating again, the phenomenon that can avoid ceramic crucible to break effectively like this, when plasma heats, can also open Frequency Induction Heating simultaneously, the evaporation of metal amount is improved greatly, thereby improve production capacity, and the operating current of plasma gun need not be very big, avoids its working life to shorten greatly.For example at identical plasma heating power 60KW, the zero intermediate frequency eddy-current heating, output is 1.2 kilograms/hour, and Frequency Induction Heating 50KW is arranged, output can be brought up to 2.8 kilograms/hour.
Table 1 is various nano metal powder experimental results
The experiment number ??1 ???2 ???3 ????4 ????5
Metal Nickel Nickel Nickel Copper Aluminium
The inlet amount kilogram/hour ??1.1 ???1.8 ???1.8 ????2.4 ????1.5
Plasma power kw ??45 ???55 ???55 ????60 ????50
Plasma gas ??N 2 ???N 2+20%H 2 ???N 2+20%H 2 ????Ar+20%H 2 ????Ar
Operating pressure kPa ??70 ???95 ???95 ????110 ????100
Particle control valve length m ??0.05 ???0.50 ???0.20 ????0.75 ????0.05
Cooldown rate ℃/S ??5100 ???560 ???1500 ????340 ????4000
Specific area m 2/g ??11.13 ???1.36 ???3.40 ????0.49 ????23.39
Average grain diameter nm ??55 ???450 ???180 ????1250 ????95
Size distribution μ m D10 ??0.02 ???0.31 ???0.15 ????0.67 ????0.07
Size distribution μ m D50 ??0.07 ???0.91 ???0.42 ????1.44 ????0.17
Size distribution μ m D90 ??0.15 ???1.68 ???1.06 ????2.28 ????0.49
Size distribution μ m D100 ??0.23 ???2.65 ???1.68 ????3.60 ????0.78
Description of drawings
Fig. 1 produces the structure principle chart of Nano metal powder device
Specific implementation method
Below in conjunction with description of drawings embodiments of the invention are described in further detail.
Anticipate as shown in the figure, this produces the Nano metal powder device, it has device case 1, liner high temperature resistant composite in the housing 1 makes housing 1 inside can tolerate the metal boiling temperature, and the top of housing is mounted with plasma gun 3, the bottom is mounted with the crucible 2 formation evaporimeters that contain metal liquid accordingly, Medium frequency induction coil 9 has been installed in evaporimeter, and the Medium frequency induction coil is connected the outer control device of housing by electric wire, and this control device is not signal in the drawings.When plasma gun 3 work, produce and shift plasma arcs 8, make metal vaporization evaporation, in housing 1, produce steam, housing middle and upper part also opening is connected with particle controller 5, control the particle growth, reach the yardstick that people wish, here particle controller 5 adopts a hollow pipeline, be distributed with a plurality of gas distribution grids in the pipeline successively, the loop head of gas distribution grid and particle controller 5 is connected, the metallic vapour that is evaporated from housing is subjected to the low gas excitation of temperature in particle controller, the cohesion of catching a cold, so particle can constantly be grown up, so by the adjustments of gas temperature, can control the nano particle yardstick to a certain extent, particle controller 5 another outlets are connected with particle collector 6, discharging opening is arranged at particle collector 6 bottoms, the nano metal particles that meets our demand is from deriving here, particle collector 6 tops are gaseous phase outlets, and this exports the loop head of distinguishing body contact bodies 1 and particle controller 5 by pipeline and pump 7 mutually gas, and gas circulation is used, also be provided with the metal charge door on housing 1 top, connect metal solid charger 4 with convenient reinforced.In order to cool off, housing 1 and particle controller 5, particle collector 6 outsides are distributed with the pipeline of logical recirculated cooling water.This process units only uses the Medium frequency induction coil to heat in the firing up stage, can control programming rate, when being heated to certain temperature by the time, opens the plasma heating again, can prevent breaking of ceramic crucible effectively like this.During the using plasma heating,, can use Frequency Induction Heating simultaneously, the evaporation of metal amount is improved greatly, improve production capacity, avoid plasma gun to pass through big operating current again, reduce its working life phenomenon in order to improve the evaporation of metal amount.

Claims (5)

1, a kind of production Nano metal powder device, the top that it is characterized in that the housing (1) at high-temperature resistant material of inner lining is mounted with plasma gun (3), the bottom is mounted with the crucible (2) that contains metal liquid accordingly, while housing also opening is connected with particle controller (5), another outlet of particle controller is connected with particle collector (6), particle collector has discharging opening and gaseous phase outlet, and gaseous phase outlet is by the loop head of pipeline and pump (7) difference body contact body and particle controller.
2, device according to claim 1 is characterized in that described particle controller (5) is a pipeline, is distributed with gas distribution grid in the pipeline, and the loop head of gas distribution grid and particle controller is connected.
3, device according to claim 1 is characterized in that described housing (1) and particle controller (5), particle collector (6) outside are distributed with the pipeline of logical recirculated cooling water.
4, device according to claim 1 is characterized in that described housing (1) is provided with the metal charge door and is connected with metal solid charger (4).
5, device according to claim 1 is characterized in that described housing (1) installed Medium frequency induction coil (9) in evaporimeter.
CN 02110837 2002-02-08 2002-02-08 Equipment for preparing nano metal powder Expired - Lifetime CN1203948C (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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CN1203948C CN1203948C (en) 2005-06-01

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Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100406110C (en) * 2004-12-21 2008-07-30 广西工学院 Purification of powder particle in cold plasma
CN100457339C (en) * 2006-11-09 2009-02-04 昆山密友实业有限公司 Continuous production apparatus for nano metal powder
CN102211197A (en) * 2011-05-06 2011-10-12 宁波广博纳米新材料股份有限公司 Metal evaporating device and method for preparing ultrafine metal powder by using same
CN102528065A (en) * 2012-03-02 2012-07-04 常熟市碧溪新城特种机械厂 Production device for nano metal powder
CN102873323A (en) * 2012-11-01 2013-01-16 泰克科技(苏州)有限公司 Electronic tantalum powder performance improvement device
CN102950289A (en) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 Method for producing nanoscale copper-manganese alloy powder
CN102950292A (en) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 Production method of submicron-order copper-manganesenickle alloy powder
CN102950290A (en) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 Method for producing nanoscale nickel-manganese alloy powder
CN102950291A (en) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 Production method of submicron-order tin-copper alloy powder
CN104588670A (en) * 2014-12-30 2015-05-06 宁波广博纳米新材料股份有限公司 Preparation method of nano-grade Mg-Y-Ni hydrogen storage alloy powder
CN104607646A (en) * 2014-12-30 2015-05-13 宁波广博纳米新材料股份有限公司 Production method for sub-micron-order Re-Ni rare earth hydrogen storage alloy powder
CN104858443A (en) * 2015-05-25 2015-08-26 常熟锐钛金属制品有限公司 Preparation method for high-purity nanoscale titanium-nickel alloy powder
CN104923800A (en) * 2015-06-01 2015-09-23 长沙市宇顺显示技术有限公司 Crucible for preparing metal nanometer powder by using evaporation condensation method
CN105598460A (en) * 2016-03-21 2016-05-25 台州市金博超导纳米材料科技有限公司 High-temperature evaporator for manufacturing micro-nanoscale metal powder
CN108480653A (en) * 2018-06-29 2018-09-04 中国科学院上海光学精密机械研究所 The device and method of hollow over spherical powder is prepared based on femtosecond laser
WO2020034090A1 (en) * 2018-08-14 2020-02-20 深圳市百柔新材料技术有限公司 Apparatus and method for preparing nanomaterial
CN110951458A (en) * 2019-12-25 2020-04-03 连云港高品再生资源有限公司 Preparation device and preparation method of nano rare earth grinding agent
CN114160801A (en) * 2021-11-01 2022-03-11 沈阳工业大学 Equipment and method for preparing alloy nanoparticles by arc process
CN115582551A (en) * 2021-07-05 2023-01-10 无锡金鹏环保科技有限公司 Process for continuously preparing nano metal powder in liquid phase environment

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100406110C (en) * 2004-12-21 2008-07-30 广西工学院 Purification of powder particle in cold plasma
CN100457339C (en) * 2006-11-09 2009-02-04 昆山密友实业有限公司 Continuous production apparatus for nano metal powder
CN102211197B (en) * 2011-05-06 2014-06-04 宁波广博纳米新材料股份有限公司 Metal evaporating device and method for preparing ultrafine metal powder by using same
CN102211197A (en) * 2011-05-06 2011-10-12 宁波广博纳米新材料股份有限公司 Metal evaporating device and method for preparing ultrafine metal powder by using same
CN102528065A (en) * 2012-03-02 2012-07-04 常熟市碧溪新城特种机械厂 Production device for nano metal powder
CN102950291B (en) * 2012-10-15 2015-02-11 宁波广博纳米新材料股份有限公司 Production method of submicron-order tin-copper alloy powder
CN102950292A (en) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 Production method of submicron-order copper-manganesenickle alloy powder
CN102950290A (en) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 Method for producing nanoscale nickel-manganese alloy powder
CN102950291A (en) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 Production method of submicron-order tin-copper alloy powder
CN102950289A (en) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 Method for producing nanoscale copper-manganese alloy powder
CN102950289B (en) * 2012-10-15 2014-10-15 宁波广博纳米新材料股份有限公司 Method for producing nanoscale copper-manganese alloy powder
CN102950290B (en) * 2012-10-15 2014-11-26 宁波广博纳米新材料股份有限公司 Method for producing nanoscale nickel-manganese alloy powder
CN102950292B (en) * 2012-10-15 2015-07-08 宁波广博纳米新材料股份有限公司 Production method of submicron-order copper-manganesenickle alloy powder
CN102873323A (en) * 2012-11-01 2013-01-16 泰克科技(苏州)有限公司 Electronic tantalum powder performance improvement device
CN104588670A (en) * 2014-12-30 2015-05-06 宁波广博纳米新材料股份有限公司 Preparation method of nano-grade Mg-Y-Ni hydrogen storage alloy powder
CN104607646A (en) * 2014-12-30 2015-05-13 宁波广博纳米新材料股份有限公司 Production method for sub-micron-order Re-Ni rare earth hydrogen storage alloy powder
CN104858443A (en) * 2015-05-25 2015-08-26 常熟锐钛金属制品有限公司 Preparation method for high-purity nanoscale titanium-nickel alloy powder
CN104923800A (en) * 2015-06-01 2015-09-23 长沙市宇顺显示技术有限公司 Crucible for preparing metal nanometer powder by using evaporation condensation method
CN105598460A (en) * 2016-03-21 2016-05-25 台州市金博超导纳米材料科技有限公司 High-temperature evaporator for manufacturing micro-nanoscale metal powder
CN105598460B (en) * 2016-03-21 2018-03-06 台州市金博超导纳米材料科技有限公司 For manufacturing the high-temperature evaporator of micro/nano level metal dust
CN108480653A (en) * 2018-06-29 2018-09-04 中国科学院上海光学精密机械研究所 The device and method of hollow over spherical powder is prepared based on femtosecond laser
WO2020034090A1 (en) * 2018-08-14 2020-02-20 深圳市百柔新材料技术有限公司 Apparatus and method for preparing nanomaterial
CN110951458A (en) * 2019-12-25 2020-04-03 连云港高品再生资源有限公司 Preparation device and preparation method of nano rare earth grinding agent
CN115582551A (en) * 2021-07-05 2023-01-10 无锡金鹏环保科技有限公司 Process for continuously preparing nano metal powder in liquid phase environment
CN114160801A (en) * 2021-11-01 2022-03-11 沈阳工业大学 Equipment and method for preparing alloy nanoparticles by arc process
CN114160801B (en) * 2021-11-01 2024-03-19 沈阳工业大学 Equipment and method for preparing alloy nano particles by arc method

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