CN1593821A - Preparation and equipment of metal nanometer power material - Google Patents

Preparation and equipment of metal nanometer power material Download PDF

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Publication number
CN1593821A
CN1593821A CN 200410040125 CN200410040125A CN1593821A CN 1593821 A CN1593821 A CN 1593821A CN 200410040125 CN200410040125 CN 200410040125 CN 200410040125 A CN200410040125 A CN 200410040125A CN 1593821 A CN1593821 A CN 1593821A
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China
Prior art keywords
metal
powder
reaction tube
crystal reaction
high frequency
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CN 200410040125
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唐永建
吴卫东
罗江山
李朝阳
韦建军
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Laser Fusion Research Center China Academy of Engineering Physics
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Laser Fusion Research Center China Academy of Engineering Physics
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Priority to CN 200410040125 priority Critical patent/CN1593821A/en
Publication of CN1593821A publication Critical patent/CN1593821A/en
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Abstract

The invention relates to a method of making nanometer metal powder and the device. Heated with high-frequency electric source, the metal material in quartz reaction tube become melted ball, which suspend in the tube and is heated with the electromagnetic field of countercurrent inductor. A lot of metal atom overflows the metal fluid. The inter gas skates over the surface of the metal melted ball from upside as the cooling medium at a certain speed a certain speed, and forms air pressure margin. After overflowing from the fluid, the metal ball is cooled and moves in a certain mode, cooling into flame of nanometer metal particle. The nanometer metal particle is sent into the collecting device carried by the inert gas, where the particle is classified and collected. The invention can be used to make better purity nanometer metal powder, the grain size of which is about 30~50mm. The device is small so can be used easily.

Description

Nano metal powder preparation methods and preparation facilities thereof
1. technical field
The invention belongs to field of nano material preparation, be specifically related to a kind of nano metal powder preparation methods and preparation facilities thereof.
2. background technology
At present, the preparation method of common nano-powder material mainly contains: gas evaporation condensation method, hybrid plasma method, chemical reduction method (methods such as similar sol-gel, liquid-phase precipitation, solvent evaporation), gamma-ray irradiation-hydrothermal treatment consists method, ultrasonic electrolysis sedimentation, organic compound thermal decomposition (hydroxyl) method, explosion method, mobile pasta evaporation, high-energy ball milling method, induced with laser method etc.
The preparation of metal nano powder powder material can only be adopted several among the above common nanometer powder preparation method, but all exist the restriction that is subjected to metal species, particle size, productive rate, device volume or the like problem, be in laboratory stage mostly, do not have the preparation facilities of the metal nano powder powder material of moulding." nano material and nanostructured " book that Science Press calendar year 2001 publishes, that write by Zhang Lide and Mu Jimei, describe the method that the condensation of gas legal system is equipped with nano metal powder in detail, its weak point is that productive rate is lower, the purity of nano metal powder is subjected to the influence of evaporative medium and cooling substrate, and apparatus expensive, preparation process is difficult to control.
The patent documentation publication number is 1382547, number of patent application is that the invention and created name of 02110837.4 bulletin discloses a kind of device of producing metal nanoparticle in batches for the application for a patent for invention of " produce Nano metal powder device ", its characteristics are to be 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.It also is provided with the Medium frequency induction coil in evaporimeter.Its weak point is that this apparatus structure complexity, product purity are not high.
3. summary of the invention
In order to overcome the deficiency of existing nano metal powder preparation method and device, the invention provides a kind of nano metal powder preparation methods and preparation facilities thereof.
The present invention is achieved in that under the heating of high frequency electric source metal material melted by heat in crystal reaction tube becomes the Metal Melting ball, and under the electromagnetic field effect that the counterflow inductive device produces, the Metal Melting ball is suspended in the crystal reaction tube and continues and is heated.When the Metal Melting ball was heated to uniform temperature, continuing to be heated had an a large amount of metallic atom molten ball liquid level of overflowing.Inert gas skims over Metal Melting ball surface with certain flow velocity all the time from top to bottom as cooling medium, form certain draught head, after catching a cold, metallic atom effusion liquid level will move according to certain mode, and be condensed into cluster, cluster nucleation in inert gas is also grown up thereupon, collision between metallic atom, cluster and merging finally form the cigarette flame of nano-metal particle.Nano-metal particle arrives at the appointment gathering-device under the transporting of inert gas, finish the classification and the collection of nano metal powder.
Nano metal powder preparation methods of the present invention contains following content: a, the metal feed arrangement is sent into wire in the crystal reaction tube, feeds circulated inert gas stream simultaneously; B, high frequency electric source produce the electromagnetic field of high frequency by the counterflow inductive device in crystal reaction tube, wire is heated and is fused into the molten ball of metal liquid, and is suspended in the electromagnetic field of high frequency; The molten ball of the metal liquid that is suspended in is wherein continued to heat in c, electromagnetic field of high frequency, and a large amount of metallic atoms are overflowed in the molten ball liquid level adding circulated inert gas; D, at the crystal reaction tube afterbody, feed as cooling medium, another road circulation transports inert gas flow, the metallic atom of effusion finally forms metal nanoparticle cigarette flame; E, nano-metal particle cigarette flame arrive at prescribed fractionated and gathering-device under the transporting of inert gas.
The preparation facilities of metal nano powder powder material of the present invention comprises: as the crystal reaction tube that produces metal nano powder powder material groundwork zone; Be arranged on around the crystal reaction tube, be used to produce the high frequency electric source and the counterflow inductive device of electromagnetic field of high frequency heat fused metal material; The metal material that will make nano metal powder is transported to the metal feed arrangement of crystal reaction tube; Be used to carry and cool off the inert gas automatic circulating system of nano metal particulate; The cold filtration gathering-device that is connected with the outlet of crystal reaction tube afterbody; Gas cooled and shunt treating apparatus.
The metal feed arrangement comprises wire wrapping head and buncher.The cold filtration gathering-device comprises powder cooler, powder receiver, main filter, the auxilliary filter that connects respectively successively; Be provided with the testing sieve shaker that filter element and timing shake filter cloth in the main filter.Gas cooled comprises gas compressor, gas cooler, vacuum meter, the two-way flowmeter that is connected successively with the shunt treating apparatus.
The metal feed arrangement is connected with crystal reaction tube, and the counterflow inductive device is arranged on around the crystal reaction tube, feeds high frequency electric and produce the electromagnetic field of high frequency in crystal reaction tube; With inert gas flow I and II respectively the gas pipeline of the air delivery device sent into of subchannel be connected with crystal reaction tube respectively; Crystal reaction tube is connected successively with powder cooler, powder receiver, main filter; Be provided with filter element in the main filter, main filter is provided with the testing sieve shaker that regularly shakes filter cloth; Main filter, auxilliary filter, gas compressor, gas cooler connect successively; Gas cooler, vacuum meter, two-way flowmeter connect successively; Regulate the two-way flowmeter respectively and obtain inert gas flow I and II, thereby form gas-circulating system, produce nano metal powder continuously.The wire that the buncher of metal feed arrangement drives in the wire wrapping head constantly enters in the crystal reaction tube.Inert gas is argon gas or helium.
Adopt that preparation method of the present invention and preparation facilities thereof can prepare that purity is higher, different-grain diameter distributes, average grain diameter is the nano metal powder of 30~50nm.Preparation facilities of the present invention is simple in structure, and volume is less relatively, is convenient to implement.
4. description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is the principle schematic of nano metal powder preparation method of the present invention and preparation facilities thereof
Fig. 2 is the structural representation of nano metal powder preparation method of the present invention and preparation facilities embodiment thereof
1. argon gas stream I among the figure, 2. wire, 3. counterflow inductive device, 4. Metal Melting ball, 5. nanometer powder ash mark, 6. argon gas stream II, 7. wire wrapping head, 8. buncher, 9. air gauge, 10. high frequency electric source, 11. crystal reaction tubes, 12. Metal Melting ball receivers, 13. the powder cooler, 14. testing sieve shakers, 15. main filters, 16. auxilliary filter, 17. compressor, 18. gas coolers, 19. vacuum meters, 20. flowmeter, 201. flowmeter, 22. nanometer powder receiver I, 23. nanometer powder receiver II, 24. nanometer powder receiver III, 25. connecting pipes.
5. the specific embodiment
Nano metal powder preparation method of the present invention contains following content: a, the metal feed arrangement is sent into wire 2 in the crystal reaction tube 11; Feed circulation argon gas current 1 in the time of charging; B, high frequency electric source 10 produce the electromagnetic field of high frequency by counterflow inductive device 3 in crystal reaction tube 11, wire 2 is heated and is fused into the molten ball 4 of metal liquid, and is suspended in the electromagnetic field of high frequency; The molten ball 4 of the metal liquid that is suspended in is wherein continued to heat in c, electromagnetic field of high frequency, and the molten ball liquid level of a large amount of metallic atoms effusions enters in the circulation argon gas body; D, crystal reaction tube 11 afterbodys feed as cooling medium, another road circulation transports argon gas current 6, the argon gas body at the uniform velocity skims over molten ball surface, form certain draught head, metallic atom effusion liquid level, flow and be condensed into cluster in the cooling back, cluster is the nucleation and the formation fine particle of thereupon growing up in argon gas stream, and collision between fine particle, cluster and merging finally form metal nanoparticle cigarette flame 5; E, metal nanoparticle cigarette flame arrive at prescribed fractionated and gathering-device under the transporting of argon gas stream.
The preparation facilities of metal nano powder powder material of the present invention comprises: as the crystal reaction tube 11 that produces metal nano material groundwork zone; Be arranged on around the crystal reaction tube 11, be used to produce the high frequency electric source 10 and the counterflow inductive device 3 of electromagnetic field of high frequency heat fused metal material; The metal material that will make nano metal powder is input to the metal feed arrangement of crystal reaction tube; Be used to carry working gas automatic circulating system with the cool metal nanoparticle; The cold filtration gathering-device that is connected with the outlet of crystal reaction tube 11 afterbodys; Gas cooled and shunt treating apparatus.The metal feed arrangement comprises wire wrapping head 7 and buncher 8.Cold filtration gathering-device bag 5 is drawn together powder cooler 13, powder receiver I22, powder receiver II23, powder receiver III24, main filter 15, the auxilliary filter 16 that connects respectively successively; Be provided with the testing sieve shaker 14 that filter element and timing shake filter cloth in the main filter 15.Gas cooled comprises gas compressor 17, gas cooler 18, vacuum meter 19, the flowmeter (20,201) that is connected successively with the shunt treating apparatus.
High frequency electric source 10 frequencies are 200~500kHz, and power is 10kW.
The metal feed arrangement is connected with crystal reaction tube 11, and counterflow inductive device 3 is arranged on around the crystal reaction tube 11, feeds high frequency electric and produce the electromagnetic field of high frequency in crystal reaction tube 11; With argon gas current I1 and argon gas current II6 respectively the gas pipeline of the air delivery device sent into of subchannel be connected with crystal reaction tube 11 respectively; Crystal reaction tube 11 is connected respectively with powder cooler 13, powder receiver I22, powder receiver II23, powder receiver III24, main filter 15; Be provided with filter element in the main filter 15, main filter 15 is provided with the testing sieve shaker 14 that regularly shakes filter cloth; Main filter 15, auxilliary filter 16, gas compressor 17, gas cooler 18 connect successively; Gas cooler 18, vacuum meter 19, flowmeter (20,201) connect successively; Regulate flowmeter (20,201) respectively and obtain argon gas current I1 and argon gas current II6, thereby form gas-circulating system, produce nano metal powder continuously.The wire 2 that the buncher 8 of metal feed arrangement drives in the wire wrapping head 7 constantly enters in the crystal reaction tube 11.
In Fig. 1, wire 2 enters in the electromagnetic field of high frequency of counterflow inductive device 3 generations, is heated to be fused into the molten ball 4 of metal liquid, and is suspended in the electromagnetic field of high frequency.When Metal Melting ball 4 is heated to uniform temperature, continue to be heated and have an a large amount of metallic atom molten ball liquid level of overflowing, simultaneously, argon gas stream I1 skims over molten ball surface as cooling medium with certain flow velocity, forms certain draught head, and atom flies out and just moves according to certain mode after liquid level is caught a cold, and be condensed into cluster, nucleation is also grown up thereupon in argon gas stream I1, and collision between particle, cluster and merging finally form nano metal powder ash mark 5.Nano particle 5 arrives at specified device under the transporting of argon gas stream II6, finish the classification and the collection of nano metal powder.
In Fig. 2, wire 2 in the wire wrapping head 7 constantly enters in the crystal reaction tube 11 by buncher 8, high frequency electric source 10 produces the electromagnetic field of high frequency by counterflow inductive device 3 in crystal reaction tube 11, wire 2 is heated and is fused into the molten ball 4 of metal liquid, and is suspended in the electromagnetic field of high frequency.There is a large amount of metallic atoms to overflow when continuing to be heated, argon gas stream I1 flows downward with certain flow velocity as cooling medium, form nano metal powder ash mark 5, under the continuation cooling of argon gas stream II6, flow downward, continue cooling during by powder cooler 13, have some nano metal powders and fall into powder receiver 22.By main filter 15 time, argon gas body and nano metal powder are separated by filter cloth, and a large amount of nano metal powders enter in the powder receiver 24, can also regularly shake filter cloth by testing sieve shaker 14.The gas that has micro-powder continues to be cleaned after entering and assisting filter 16, after this, gas enters gas cooler 18 coolings by compressor 17 after pressurized, regulate flowmeter (20,201) respectively and obtain argon gas stream I1 and argon gas stream II6, thereby the formation gas-circulating system is produced nano metal powder continuously.
The metal nano powder powder material adopts cooling of argon gas body and directed flow, continues to use water cooling then.Nano metal powder separates the back to be collected with the argon gas body, and the argon gas body adopts compressor to circulate automatically, and uses water cooling.

Claims (7)

1, a kind of nano metal powder preparation methods is characterized in that containing following content: a, the metal feed arrangement is sent into wire (2) in the crystal reaction tube (11), feeds circulated inert gas stream (1) simultaneously; B, high frequency electric source (10) produce the electromagnetic field of high frequency by counterflow inductive device (3) in crystal reaction tube (11), wire (2) is heated and is fused into the molten ball (4) of metal liquid, and is suspended in the electromagnetic field of high frequency; The molten ball (4) of the metal liquid that is suspended in is wherein continued to heat in c, electromagnetic field of high frequency, and a large amount of metallic atoms are overflowed in the molten ball liquid level adding circulated inert gas (1); D, at crystal reaction tube (11) afterbody, feed as cooling medium, another road circulation transports inert gas flow (6), the metallic atom of effusion finally forms metal nanoparticle cigarette flame (5); E, nano-metal particle cigarette flame (5) arrive at prescribed fractionated and gathering-device under the transporting of inert gas.
2, a kind of preparation facilities of metal nano powder powder material is characterized in that comprising: as the crystal reaction tube (11) that produces metal nano powder powder material groundwork zone; Be arranged on crystal reaction tube (11) on every side, be used to produce the high frequency electric source (10) and the counterflow inductive device (3) of electromagnetic field of high frequency heat fused metal material; The metal material that will make nano metal powder is transported to the metal feed arrangement of crystal reaction tube (11); Be used to carry inert gas automatic circulating system with the cool metal nanoparticle; The cold filtration gathering-device that is connected with the outlet of crystal reaction tube (11) afterbody; Gas cooled and shunt treating apparatus.
3, the preparation facilities of metal nano powder powder material according to claim 2 is characterized in that: described metal feed arrangement comprises wire wrapping head (7) and buncher (8).
4, the preparation facilities of metal nano powder powder material according to claim 2, it is characterized in that: described cold filtration gathering-device comprises powder cooler (13), main filter (15), the powder receiver (22 that connects respectively successively, 23,24), auxilliary filter (16).
5, the preparation facilities of metal nano powder powder material according to claim 4 is characterized in that: be provided with the testing sieve shaker (14) that filter element and timing shake filter cloth in the described main filter (15).
6, the preparation facilities of metal nano powder powder material according to claim 2 is characterized in that: described gas cooled comprises gas compressor (17), gas cooler (18), vacuum meter (19), the flowmeter (20,201) that is connected successively with the shunt treating apparatus.
7, the preparation facilities of metal nano powder powder material according to claim 2 is characterized in that: describedly be used to carry the inert gas with the cool metal nanoparticle to adopt gas compressor (17) to circulate automatically, and use water cooling.
CN 200410040125 2004-07-02 2004-07-02 Preparation and equipment of metal nanometer power material Pending CN1593821A (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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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102166654A (en) * 2010-12-30 2011-08-31 东莞市高能磁电技术有限公司 Preparation method for highly-efficient nickel-graphite powder and special device
CN108168660A (en) * 2016-12-07 2018-06-15 财团法人金属工业研究发展中心 The measuring device and method of weight suspension
CN110814357A (en) * 2018-08-14 2020-02-21 深圳市百柔新材料技术有限公司 Nanomaterial preparation device and method
CN111804926A (en) * 2020-07-06 2020-10-23 昆明理工大学 Method for preparing refractory metal powder
CN115533109A (en) * 2022-03-01 2022-12-30 哈尔滨工业大学(深圳) Device and method for manufacturing tin ball based on magnetic suspension technology
CN116160007A (en) * 2023-04-24 2023-05-26 成都佩克斯新材料有限公司 Gold-tin powder preparation device and preparation method

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102166654A (en) * 2010-12-30 2011-08-31 东莞市高能磁电技术有限公司 Preparation method for highly-efficient nickel-graphite powder and special device
CN102166654B (en) * 2010-12-30 2015-11-25 广东高鑫科技股份有限公司 Efficient nickel-graphite raw powder's production technology and special purpose device thereof
CN108168660A (en) * 2016-12-07 2018-06-15 财团法人金属工业研究发展中心 The measuring device and method of weight suspension
CN110814357A (en) * 2018-08-14 2020-02-21 深圳市百柔新材料技术有限公司 Nanomaterial preparation device and method
CN111804926A (en) * 2020-07-06 2020-10-23 昆明理工大学 Method for preparing refractory metal powder
CN115533109A (en) * 2022-03-01 2022-12-30 哈尔滨工业大学(深圳) Device and method for manufacturing tin ball based on magnetic suspension technology
CN116160007A (en) * 2023-04-24 2023-05-26 成都佩克斯新材料有限公司 Gold-tin powder preparation device and preparation method

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