CN101716683B - Equipment and method for producing high-purity nano-metal ultrafine powder - Google Patents

Equipment and method for producing high-purity nano-metal ultrafine powder Download PDF

Info

Publication number
CN101716683B
CN101716683B CN2009102192077A CN200910219207A CN101716683B CN 101716683 B CN101716683 B CN 101716683B CN 2009102192077 A CN2009102192077 A CN 2009102192077A CN 200910219207 A CN200910219207 A CN 200910219207A CN 101716683 B CN101716683 B CN 101716683B
Authority
CN
China
Prior art keywords
raw material
metal
high temperature
ultrafine powder
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN2009102192077A
Other languages
Chinese (zh)
Other versions
CN101716683A (en
Inventor
杨俊武
贾兰惠
杨继东
武婷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xi'an Huiwei Nano Metal Materials Co Ltd
Original Assignee
Xi'an Huiwei Nano Metal Materials Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xi'an Huiwei Nano Metal Materials Co Ltd filed Critical Xi'an Huiwei Nano Metal Materials Co Ltd
Priority to CN2009102192077A priority Critical patent/CN101716683B/en
Publication of CN101716683A publication Critical patent/CN101716683A/en
Application granted granted Critical
Publication of CN101716683B publication Critical patent/CN101716683B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention discloses equipment and a method for producing high-purity nano-metal ultrafine powder. The production equipment comprises a raw material conveying and pre-treatment device, a supersonic nozzle, a high-temperature atomizing combustion quick reducer, an inert gas quick condensing device, a multi-stage metal ultrafine powder grading device and a powder collection device; and the inside of each of the devices is sequentially communicated with a production circulation channel for producing the high-purity nano-metal ultrafine powder, and the tail end of the channel is connected with an induced draft fan which is communicated with the inside of the channel. The production method comprises the following steps of: 1, the conveying and pretreatment of raw materials; 2, the atomization and conveying of metal oxide; 3, high-temperature quick reduction reaction; 4, quick condensation; and 5, the grading and collection of powder, wherein a condensate is combined with high-pressure oxygen-rich direct oxidation combustion to generate metal oxidized liquid fog, and then hydrocarbon fuels and high-pressure rich oxygen are used to form high-temperature reducing atmosphere to finally generate spherical nano-metal ultrafine powder. The production equipment has the advantages of reasonable design, broad applicable raw materials, short production flow and high efficiency, and can realize continuous industrialized production.

Description

A kind of production equipment of high-purity nano-metal ultrafine powder and production method
Technical field
The invention belongs to the nano metal powder technical field of material, especially relate to a kind of production equipment and production method of high-purity nano-metal ultrafine powder.
Background technology
In recent years, along with the develop rapidly of field of new, the sharp increase of nano-metal ultrafine powder demand, the quality and the performance requirement of tackling nano-metal ultrafine powder mutually also improve day by day.With the molybdenum is example, its metal and alloy material have that fusing point height, hardness height, intensity are big, wearability and characteristics such as heat-conductivity conducting is good, the coefficient of expansion is little, corrosion resisting property is good, be widely used in technical fields such as electronics, chemical industry, metallurgy, national defence and aerospace industry, representative as liquid crystal display transparency conducting layer, solar cell, glass heat insulating coating, metal and non metallic decorative coating, surperficial superhard wear coating, corrosion-resistant finishes etc.
Above-mentioned ultra micro preparation method of molybdenum mainly contains following three kinds: the first, use the ammonium paramolybdate activation reduction method, this method is a raw material with the ammonium paramolybdate that adds some ammonium chloride, makes ultrafine molybdenum powder through pure hydrogen reduction once at low temperatures.Compare with conventional method, its technology is simpler, and reduction temperature is low, reduces about 200~300 ℃ than traditional handicraft.The molybdenum powder that obtains, its particle mean size is 0.1 μ m, and powder has good sintering character.Because chloride utilizes hydrogen to carry out reduction reaction, can produce poisonous chlorine, hydrogen chloride in the stove, so also there is the problem of the high equipment such as burn into leakage of process units.The second, adopting nanometer molybdenum trioxide fiber is raw material, reduces under hydrogen atmosphere, obtains superfine metal molybdenum powder.Three, adopt nanoscale eight molybdic acids by being raw material, carry out the reverse reduction reaction of hydrogen under enclosed environment twice, by the furnace temperature and the hydrogen flowing quantity of control reduction for the first time, reduction for the second time, the nano-scale molybdenum powder of preparing is purple, its particle diameter is at 55~92nm, and purity is all more than 99.80%.
Owing to use nano material to be raw material, hydrogen is as reducing gas, thereby existing above-mentioned three kinds of production methods all are expensive production methods.
In sum, existing method of producing nano-metal ultrafine powder all must use nano material to be raw material, use hydrogen as reducing gas, thereby not only raw material is restricted, and the production cost height.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned deficiency of the prior art, provides a kind of reasonable in design, applicable raw materials is extensive and production procedure is short, production efficiency is high, can realize the high-purity nano-metal ultrafine powder production equipment of continuous industry production.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of production equipment of high-purity nano-metal ultrafine powder, it is characterized in that: comprise processed raw material is carried and pretreated raw material conveying and pretreatment unit, be arranged on that raw material is carried and pretreatment unit is inner and the metal oxide that raw material obtains be atomized into the superonic flow nozzzle of metal oxide liquid mist after preliminary treatment, charging aperture and raw material are carried and the discharging opening of pretreatment unit joins and described metal oxide liquid mist high temperature reduction can be reacted into the high temperature spray combustion fast restore device of ball shaped nano metal ultrafine powder, described ball shaped nano metal ultrafine powder is carried out rapid condensation and can prevent effectively that the ball shaped nano metal ultrafine powder that generates from the inert gas rapid condensation device of oxidation further taking place, with multistage metal ultrafine powder grading plant and a plurality of powder gathering-device that is laid in described multistage metal ultrafine powder grading plant below respectively and joins with described multistage metal ultrafine powder grading plant below discharging opening that inert gas rapid condensation device discharging opening joins, described inert gas rapid condensation device is that the discharging opening of charging aperture and high temperature spray combustion fast restore device joins and the inner reaction vessel that inert gas is housed; Described raw material conveying and pretreatment unit, high temperature spray combustion fast restore device, inert gas rapid condensation device and described multistage metal ultrafine powder grading plant inside are communicated with the production circulation passage that composition is handled processed raw material successively, and described production circulation passage afterbody is connected with the air-introduced machine that communicates with its inside, raw material is carried and the charging aperture and the oxygen cylinder of pretreatment unit join, and superonic flow nozzzle and air compressor join; The reaction vessel of described high temperature spray combustion fast restore device for joining by pipeline and reducing atmosphere source of the gas, and correspondence has the reducing atmosphere import on the high temperature spray combustion fast restore device;
Described processed raw material is wire and/or metal-powder, and described raw material is carried and pretreatment unit should be mutually the wire of independent input is carried and pretreated raw material carries and pretreatment unit one, the metal-powder of independent input is carried and pretreated raw material is carried and pretreatment unit two and to the wire of input simultaneously with metal-powder is carried and pretreated raw material is carried and pretreatment unit three; Described raw material carry and pretreatment unit one by have the wire input unit and can to the input wire carry out the device of arc of arc-melting, the charging aperture of high temperature spray combustion fast restore device and the discharging opening of described device of arc join; Described raw material is carried and pretreatment unit two comprises dust feeder, and the charging aperture of high temperature spray combustion fast restore device and the discharging opening of described dust feeder join; Described raw material is carried and pretreatment unit three comprises and has wire input unit and can be to importing the device of arc that wire and metal dust carry out arc-melting simultaneously, and the charging aperture place of described device of arc is provided with dust feeder; Described device of arc and direct-current arc power supply join.
Described high temperature spray combustion fast restore device comprise have before plug and rearward end be uncovered external shell, have feed openings, a plurality of reducing atmosphere import and a plurality of secondary oxygen supply import that feeds for described metal oxide liquid mist on the plug before described; The oxygen that described oxygen cylinder provided enters high temperature spray combustion fast restore device by feed openings; Described external shell inside is provided with corresponding cooling water inlet and the coolant outlet that joins with described water cooling pipeline that have on water cooling pipeline and its sidewall; Feed openings and raw material are carried and the discharging opening of pretreatment unit joins, and the rearward end of external shell is uncovered to communicate with inert gas rapid condensation device inside.
Described external shell is a cylindrical shell, preceding plug is circular, feed openings is arranged on preceding plug center, and a plurality of reducing atmosphere imports along the circumferential direction evenly are laid in the feed openings outside, and a plurality of secondary oxygen supply imports along the circumferential direction evenly are laid in described a plurality of reducing atmosphere imports outside; In described a plurality of reducing atmosphere import the reducing atmosphere jet blower is housed all, in a plurality of secondary oxygen supply imports secondary oxygen jet blower is housed all.
Described raw material conveying and pretreatment unit, high temperature spray combustion fast restore device and inert gas rapid condensation device are assembled into one and the coaxial setting of three.
Described raw material conveying and pretreatment unit are cylindrical structural with high temperature spray combustion fast restore device and the external diameter of the two is identical; Described raw material conveying and pretreatment unit and high temperature spray combustion fast restore device are installed as that the charging aperture from inert gas rapid condensation device penetrates inert gas rapid condensation device inside after the one, and are tightly connected between the sidewall of the charging aperture of inert gas rapid condensation device and raw material conveying and pretreatment unit or high temperature spray combustion fast restore device.
Described multistage metal ultrafine powder grading plant comprises successively three grades of high-pressure electrostatic grading plants that join with inert gas rapid condensation device discharging opening.
Simultaneously, the present invention also provides a kind of and has become to produce that cost is low, production craft step is simple and realizes the production method of high-purity nano-metal ultrafine powder easily, it is characterized in that method may further comprise the steps:
Step 1, raw material are carried and preliminary treatment: when the processed raw material of import is wire, adopt described device of arc that the metal to be treated silk of sending into by wire feeder is carried out arc-melting; When the processed raw material of import is wire and metal dust, adopt described device of arc that metal to be treated silk and the metal dust of sending into by wire feeder and dust feeder carried out arc-melting simultaneously; When carrying out arc-melting, the output voltage of described direct-current arc power supply is that 26-36V and its output current are 20-400A; When sending into wire or wire and metal dust are carried out arc-melting, under the effect of oxygen that oxygen cylinder provides, the metal melt that is generated behind the arc-melting is carried and the reaction of the inner generation of pretreatment unit high-temperature oxydation at raw material, and the corresponding metal oxide that generates;
When the processed raw material of import is metal dust, adopts described dust feeder and be that source of the gas carries out powder feeding, and should will light before the powder feeding described HC fuel with the HC fuel; Under the effect of oxygen that oxygen cylinder provides, the metal-powder after lighting is carried and the reaction of the inner generation of pretreatment unit high-temperature oxydation at raw material, and the corresponding metal oxide that generates;
Step 2, metal oxide atomizing and carrying: in the step 1 when generating metal oxide, by the supersonic airstream that superonic flow nozzzle produced the metal oxide that is generated is atomized into metal oxide liquid mist, and the metal oxide liquid mist that is generated is admitted to high temperature spray combustion fast restore device under the effect of supersonic airstream that superonic flow nozzzle is sent into;
The conveying of step 3, the reaction of high temperature fast restore and the ball shaped nano metal ultrafine powder that generates: after described metal oxide liquid mist is admitted to high temperature spray combustion fast restore device inside together with the high pressure oxygen that supersonic airstream and oxygen cylinder provided, correspondingly in inside is high temperature spray combustion fast restore device under the reducing atmosphere, carry out the high temperature reduction reaction, and generate the size-controllable spherical nano-metal ultrafine powder; The ball shaped nano metal ultrafine powder that is generated is admitted to inert gas rapid condensation device under the effect of supersonic airstream that superonic flow nozzzle produces;
Step 4, rapid condensation: after described ball shaped nano metal ultrafine powder is admitted to inert gas rapid condensation device, carry out described ball shaped nano metal ultrafine powder by the inner inert gas that is full of of inert gas rapid condensation device and carry out rapid condensation, described indifferent gas physical efficiency effectively prevents described ball shaped nano metal ultrafine powder generation secondary oxidation simultaneously;
Step 5, particle classifying and collection: successively the nano-metal ultrafine powder after rapid condensation is carried out multiple fractionation by described multistage metal ultrafine powder grading plant, and corresponding to corresponding other ball shaped nano metal ultrafine powder of a plurality of grain-size grades of collecting respectively of a plurality of powder gathering-devices; Carry out in particle classifying and the collection process, under the acting in conjunction of supersonic airstream that described production circulation passage head superonic flow nozzzle is produced and the set air-introduced machine of afterbody, finish whole particle classifying and collection process.
High temperature spray combustion fast restore device described in the above-mentioned steps three joins by pipeline and secondary oxygen supply source of the gas, and correspondence has secondary oxygen supply import on the high temperature spray combustion fast restore device; Correspondingly, the high temperature fast restore reacts described metal oxide liquid mist when being admitted to high temperature spray combustion fast restore device inside together with the high pressure oxygen that supersonic airstream and oxygen cylinder provided in the step 3, in high temperature spray combustion fast restore device, feed secondary oxygen by secondary oxygen supply import, to guarantee in the described metal oxide liquid mist that unburned metal melt and/or metal dust fully burn, and being converted into metal oxide fully, the corresponding again high temperature fast restore that carries out under reducing atmosphere reacts.
In the above-mentioned steps one raw material carry and pretreatment unit in oxygen cylinder the pressure of high pressure oxygen is provided is 0.1-0.95Mpa; The pressure of supersonic airstream described in the step 2 to five is 0.3-0.8Mpa; It is 0.1-0.98Mpa that the interior oxygen cylinder of the spray combustion of high temperature described in step 3 fast restore device provides high pressure oxygen and secondary oxygen supply import that the total pressure of secondary oxygen is provided, and the pressure of reducing atmosphere is 0.15-1.3Mpa described in the spray combustion of high temperature described in the step 3 fast restore device.
Reducing atmosphere described in the above-mentioned steps three is a HC fuel.
The present invention compared with prior art has the following advantages:
1, reasonable in design, the use raw material is extensive, production efficiency is high, cost is low, the metal ultrafine powder particle diameter that generates controlled, be specially the metal ultrafine powder of 10 nanometers~1 micron grain size.
2, powder purity is equal to high pure raw material self purity, can not introduce impurity in the preparation process, and powder has kept original metal phase.
3, production procedure is short and production efficiency is high, can realize continuous industry production.
But 4, use extensive, the applied widely and industrialization production of raw material, can be applicable to the production preparation of multiple metalloid and alloy, oxidate nano ultra micro powder.
In sum, the present invention is reasonable in design, the use raw material is extensive, production efficiency is high, cost is low, can effectively solve existing existing number of drawbacks of Apparatus and method for and deficiency of producing nano-metal ultrafine powder.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the structural representation of the production equipment of high-purity nano-metal ultrafine powder of the present invention.
Fig. 2 is the structural representation of high temperature spray combustion fast restore device of the present invention.
Fig. 3 is the right view of Fig. 2.
Fig. 4 is the process chart of the production method of high-purity nano-metal ultrafine powder of the present invention.
Fig. 5 by the present invention to the fundamental diagram of input wire when carrying out arc-melting.
Ignition temperature distribution map when Fig. 6 carries out arc-melting for the present invention.
Description of reference numerals:
The 1-raw material is carried and preliminary treatment dress 1-1-ignition tip; The 1-2-conducting block;
Put;
The 2-wire pushing roller; The 3-superonic flow nozzzle; 4-high temperature spray combustion is fast
The speed reductor;
The 4-1-external shell; The 4-11-overcoat; Cover in the 4-12-;
Plug before the 4-2-; The 4-3-feed openings; The import of 4-4-reducing atmosphere;
4-5-secondary oxygen supply import; The 4-6-cooling water inlet; The 4-7-coolant outlet;
The 4-8-sealing ring; 4-9-powder feeding passage; The 5-high temperature reaction stove;
The 6-air-introduced machine; The 8-oxygen cylinder; The 9-air compressor;
10-high-pressure electrostatic grading plant; 11-powder gathering-device; 13-direct-current arc power supply.
The specific embodiment
As shown in Figure 1, high-purity nano-metal ultrafine powder production equipment of the present invention, comprise processed raw material is carried and pretreated raw material conveying and pretreatment unit 1, be arranged on that raw material is carried and pretreatment unit 1 is inner and the metal oxide that raw material obtains after preliminary treatment is atomized into the superonic flow nozzzle 3 of metal oxide liquid mist, charging aperture and raw material are carried and the discharging opening of pretreatment unit 1 joins and described metal oxide liquid mist high temperature reduction can be reacted into the high temperature spray combustion fast restore device 4 of ball shaped nano metal ultrafine powder, described ball shaped nano metal ultrafine powder is carried out rapid condensation and can prevent effectively that the ball shaped nano metal ultrafine powder that generates from the inert gas rapid condensation device 5 of oxidation further taking place, with multistage metal ultrafine powder grading plant and a plurality of powder gathering-device 11 that is laid in described multistage metal ultrafine powder grading plant below respectively and joins with described multistage metal ultrafine powder grading plant below discharging opening that inert gas rapid condensation device 5 discharging openings join, described inert gas rapid condensation device 5 joins and the inner reaction vessel that inert gas is housed for the discharging opening of charging aperture and high temperature spray combustion fast restore device 4.Described raw material is carried and pretreatment unit 1, high temperature spray combustion fast restore device 4, inert gas rapid condensation device 5 and described multistage metal ultrafine powder grading plant inside are communicated with the production circulation passage that composition is handled processed raw material successively, and described production circulation passage afterbody is connected with the air-introduced machine 6 that communicates with its inside, raw material is carried and the charging aperture and the oxygen cylinder 8 of pretreatment unit 1 join, and superonic flow nozzzle 3 joins with air compressor 9.The reaction vessel of described high temperature spray combustion fast restore device 4 for joining by pipeline and reducing atmosphere source of the gas, and correspondence has reducing atmosphere import 4-4 on the high temperature spray combustion fast restore device 4.
Described processed raw material is wire and/or metal-powder, and described raw material is carried and pretreatment unit 1 should be mutually the wire of independent input is carried and pretreated raw material carries and pretreatment unit one, the metal-powder of independent input is carried and pretreated raw material is carried and pretreatment unit two and to the wire of input simultaneously with metal-powder is carried and pretreated raw material is carried and pretreatment unit three.Described raw material carry and pretreatment unit one by have the wire input unit and can to the input wire carry out the device of arc of arc-melting, the charging aperture of high temperature spray combustion fast restore device 4 and the discharging opening of described device of arc join.Described raw material is carried and pretreatment unit two comprises dust feeder, and the charging aperture of high temperature spray combustion fast restore device 4 and the discharging opening of described dust feeder join.Described raw material is carried and pretreatment unit three comprises and has wire input unit and can be to importing the device of arc that wire and metal dust carry out arc-melting simultaneously, and the charging aperture place of described device of arc is provided with dust feeder; Described device of arc and direct-current arc power supply 13 join.
As shown in Figure 4, high-purity nano-metal ultrafine powder production method of the present invention may further comprise the steps:
Step 1, raw material are carried and preliminary treatment: when the processed raw material of import is wire, adopt described device of arc that the metal to be treated silk of sending into by wire feeder is carried out arc-melting; When the processed raw material of import is wire and metal dust, adopt described device of arc that metal to be treated silk and the metal dust of sending into by wire feeder and dust feeder carried out arc-melting simultaneously; When carrying out arc-melting, the output voltage of described direct-current arc power supply 13 is that 26-36V and its output current are 20-400A; When sending into wire or wire and metal dust are carried out arc-melting, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit 1 inner generation high-temperature oxydation reaction at raw material, and the corresponding metal oxide that generates.The output voltage of described 26-36V is respectively six grades of 26V, 28V, 30V, 32V, 34V and 36V.
When the processed raw material of import is metal dust, adopts described dust feeder and be that source of the gas carries out powder feeding, and should will light before the powder feeding described HC fuel with the HC fuel; Under the effect of oxygen cylinder 8 oxygen that provides, the metal-powder after lighting is carried and pretreatment unit 1 inner generation high-temperature oxydation reaction at raw material, and the corresponding metal oxide that generates.
Step 2, metal oxide atomizing and carrying: in the step 1 when generating metal oxide, the supersonic airstream that is produced by superonic flow nozzzle 3 is atomized into metal oxide liquid mist with the metal oxide that is generated, and the metal oxide liquid mist that is generated is admitted to high temperature spray combustion fast restore device 4 under the effect of superonic flow nozzzle 3 supersonic airstream of sending into.
The conveying of the reaction of step 3, high temperature fast restore and the ball shaped nano metal ultrafine powder that generates: after the high pressure oxygen that described metal oxide liquid mist is provided together with supersonic airstream and oxygen cylinder 8 is admitted to high temperature spray combustion fast restore device 4 inside, correspondingly in inside is high temperature spray combustion fast restore device 4 under the reducing atmosphere, carry out the high temperature reduction reaction, and generate the size-controllable spherical nano-metal ultrafine powder; The ball shaped nano metal ultrafine powder that is generated is admitted to inert gas rapid condensation device 5 under the effect of superonic flow nozzzle 3 supersonic airstream that produces.And, the corresponding secondary oxygen supply import 4-5 that joins with secondary oxygen supply source of the gas that has on the described high temperature spray combustion fast restore device 4.
Step 4, rapid condensation: after described ball shaped nano metal ultrafine powder is admitted to inert gas rapid condensation device 5, carry out described ball shaped nano metal ultrafine powder by the inert gas rapid condensation device 5 inner inert gases that are full of and carry out rapid condensation, described indifferent gas physical efficiency effectively prevents described ball shaped nano metal ultrafine powder generation secondary oxidation simultaneously.
Step 5, particle classifying and collection: successively the nano-metal ultrafine powder after rapid condensation is carried out multiple fractionation by described multistage metal ultrafine powder grading plant, and corresponding to a plurality of powder gathering-device 11 corresponding other ball shaped nano metal ultrafine powders of a plurality of grain-size grades of collecting respectively; Carry out in particle classifying and the collection process, under the acting in conjunction of supersonic airstream that described production circulation passage head superonic flow nozzzle 3 is produced and the set air-introduced machine 6 of afterbody, finish whole particle classifying and collection process.
The pressure of raw material conveying and the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.1-0.95Mpa in the step 1.The pressure of supersonic airstream described in the step 2 to five is 0.3-0.8Mpa.It is 0.1-0.98Mpa that the spray combustion of high temperature described in step 3 fast restore device 4 interior oxygen cylinder 8 high pressure oxygen that provide and secondary oxygen supply import 4-5 provide the total pressure of secondary oxygen, and the pressure of reducing atmosphere is 0.15-1.3Mpa described in the spray combustion of high temperature described in the step 3 fast restore device 4.When not opening secondary oxygen supply import 4-5 on the high temperature spray combustion fast restore device 4, should guarantee in the step 3 that the pressure of the oxygen cylinder 8 high pressure oxygen that provides in the high temperature spray combustion fast restore device 4 is 0.1-0.98Mpa.In the actual production process, can adjust the oxygen-supplying amount of oxygen cylinder 8 and described secondary oxygen supply source of the gas as required, the purpose that the pressure to providing high pressure oxygen pressure and secondary oxygen adjusts accordingly is provided then.
Embodiment 1
In the present embodiment, processed raw material is a molybdenum filament.Thereby, in the present embodiment, employed high-purity nano-metal ultrafine powder production equipment comprises raw material is carried and pretreatment unit one, be arranged on the superonic flow nozzzle 3 of raw material conveying and pretreatment unit one inside, the high temperature spray combustion fast restore device 4 that the discharging opening of charging aperture and raw material conveying and pretreatment unit one joins, the inert gas rapid condensation device 5 that the discharging opening of charging aperture and high temperature spray combustion fast restore device 4 joins, the multistage metal ultrafine powder grading plant that joins with inert gas rapid condensation device 5 discharging openings and a plurality of powder gathering-device 11 that is laid in described multistage metal ultrafine powder grading plant below respectively and joins with described multistage metal ultrafine powder grading plant below discharging opening.
In the present embodiment, described multistage metal ultrafine powder grading plant comprises successively three grades of high-pressure electrostatic grading plants 10 that join with inert gas rapid condensation device 5 discharging openings.Described raw material is carried and pretreatment unit one, high temperature spray combustion fast restore device 4, inert gas rapid condensation device 5 and three grades of high-pressure electrostatic grading plant 10 inside are communicated with the production circulation passage that composition is handled processed molybdenum filament successively, and produce the circulation passage afterbody and be connected with the air-introduced machine 6 that communicates with its inside, raw material is carried and the charging aperture and the oxygen cylinder 8 of pretreatment unit one join, and superonic flow nozzzle 3 joins with air compressor 9.The reaction vessel of described high temperature spray combustion fast restore device 4 for joining by pipeline and reducing atmosphere source of the gas, and correspondence has reducing atmosphere import 4-4 on the high temperature spray combustion fast restore device 4.
Described raw material is carried and pretreatment unit one, high temperature spray combustion fast restore device 4 and inert gas rapid condensation device 5 is assembled into one and the coaxial setting of three; And described raw material carries and pretreatment unit one is cylindrical structural with high temperature spray combustion fast restore device 4 and the external diameter of the two is identical.Described raw material is carried and pretreatment unit one and high temperature spray combustion fast restore device 4 are installed as that the charging aperture from inert gas rapid condensation device 5 penetrates inert gas rapid condensation device 5 inside after the one, and is tightly connected between the sidewall of the charging aperture of inert gas rapid condensation device 5 and raw material conveying and pretreatment unit one or high temperature spray combustion fast restore device 4.In the present embodiment, be tightly connected between the sidewall of the charging aperture of inert gas rapid condensation device 5 and raw material conveying and pretreatment unit one.
In conjunction with Fig. 2, Fig. 3, described high temperature spray combustion fast restore device 4 comprise have before plug 4-2 and rearward end be uncovered external shell 4-1, have feed openings 4-3, a plurality of reducing atmosphere import 4-4 and a plurality of secondary oxygen supply import 4-5 that feeds for described metal oxide liquid mist on the plug 4-2 before described.The oxygen that described oxygen cylinder 8 is provided enters high temperature spray combustion fast restore device 4 by feed openings 4-3.Described external shell 4-1 inside is provided with corresponding cooling water inlet 4-6 and the coolant outlet 4-7 that joins with described water cooling pipeline that have on water cooling pipeline and its sidewall.Described feed openings 4-3 and raw material are carried and the discharging opening of pretreatment unit 1 joins, and the rearward end of external shell 4-1 is uncovered to communicate with inert gas rapid condensation device 5 inside.Described external shell 4-1 is a cylindrical shell, preceding plug 4-2 is circular, feed openings 4-3 is arranged on preceding plug 4-2 center, a plurality of reducing atmosphere import 4-4 along the circumferential direction evenly are laid in the feed openings 4-3 outside, and a plurality of secondary oxygen supply import 4-5 along the circumferential direction evenly are laid in described a plurality of reducing atmosphere import 4-4 outside.On described a plurality of reducing atmosphere import 4-4 the reducing atmosphere jet blower is housed all, on a plurality of secondary oxygen supply import 4-5 secondary oxygen jet blower is housed all.Be connected and sealed by sealing ring 4-8 between described external shell 4-1 and preceding plug 4-2, to be cylindrical shell and its be made up of overcoat 4-11 and the interior cover 4-12 that is sleeved on overcoat 4-11 inside external shell 4-1.
In conjunction with Fig. 5, Fig. 6, in the present embodiment, described device of arc is an arc gum, and described wire feeder is the wire pushing roller 2 that is used with arc gum.The conducting block 1-2 that described arc gum inside is provided with ignition tip 1 and is arranged on ignition tip 1-1 outside and joins with direct-current arc power supply 13.
In the present embodiment, utilize the production method of molybdenum filament high-purity nano-metal ultrafine powder, may further comprise the steps:
Step 1, raw material are carried and preliminary treatment: carrying and a pair of described molybdenum filament conveying of pretreatment unit and preliminary treatment by raw material, specifically is to adopt arc gum that the molybdenum filament of sending into by wire pushing roller 2 is carried out arc-melting; When carrying out arc-melting, the output voltage of described direct-current arc power supply 13 is that 36V and its output current are 400A, and the wire feed rate of wire pushing roller 2 is 3.5m/min.In the actual production process, the wire feed rate of wire pushing roller 2 can be adjusted accordingly in the scope of 2-6m/min.
When sending into molybdenum filament was carried out arc-melting, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting was carried and pretreatment unit one inner generation high-temperature oxydation reaction at raw material, and the corresponding metal oxide that generates.In this step, raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.1Mpa.
Step 2, metal oxide atomizing and carrying: in the step 1 when generating metal oxide, the supersonic airstream that is produced by superonic flow nozzzle 3 is atomized into the oxide ultra micro liquid mist that metal oxide liquid mist is a metal molybdenum with the metal oxide that is generated, and the metal oxide liquid mist that is generated is admitted to high temperature spray combustion fast restore device 4 under the effect of superonic flow nozzzle 3 supersonic airstream of sending into.In the present embodiment, the pressure of supersonic airstream is 0.6Mpa and with consumed cabin air 〉=3m 3The speed of/min atomizes.
The conveying of the reaction of step 3, high temperature fast restore and the ball shaped nano metal ultrafine powder that generates: after the high pressure oxygen that described metal oxide liquid mist is provided together with supersonic airstream and oxygen cylinder 8 is admitted to high temperature spray combustion fast restore device 4 inside, correspondingly in inside is high temperature spray combustion fast restore device 4 under the reducing atmosphere, carry out the high temperature reduction reaction, and to generate the size-controllable spherical nano-metal ultrafine powder be molybdenum powder; The molybdenum powder that is generated is admitted to inert gas rapid condensation device 5 under the effect of superonic flow nozzzle 3 supersonic airstream that produces.
High temperature spray combustion fast restore device 4 described in this step 3 joins by pipeline and secondary oxygen supply source of the gas, and correspondence has secondary oxygen supply import 4-5 on the high temperature spray combustion fast restore device 4; Correspondingly, when the high pressure oxygen that the high temperature fast restore reacts described metal oxide liquid mist and provided together with supersonic airstream and oxygen cylinder 8 in the step 3 is admitted to high temperature spray combustion fast restore device 4 inside, in high temperature spray combustion fast restore device 4, feed secondary oxygen by secondary oxygen supply import 4-5, to guarantee in the described metal oxide liquid mist that unburned metal melt and/or metal dust fully burn, and being converted into metal oxide fully, the corresponding again high temperature fast restore that carries out under reducing atmosphere reacts.It is 0.06Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen.
In the present embodiment, described reducing atmosphere is a HC fuel, and described HC fuel is a hydrocarbon fuels, is specially LPG (being liquefied petroleum gas) or LNG (being liquefied natural gas), the gas pressure intensity of the LPG that sends into or LNG be 0.2Mpa.The total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.16Mpa.
Step 4, rapid condensation: after described ball shaped nano metal ultrafine powder is admitted to inert gas rapid condensation device 5, carry out described ball shaped nano metal ultrafine powder by the inert gas rapid condensation device 5 inner inert gases that are full of and carry out rapid condensation, described indifferent gas physical efficiency effectively prevents described ball shaped nano metal ultrafine powder generation secondary oxidation simultaneously.Described inert gas is argon gas or nitrogen.
Step 5, particle classifying and collection: successively the molybdenum powder after rapid condensation is carried out three classifications by three grades of high-pressure electrostatic grading plants 10, and corresponding three powder gathering-devices, 11 corresponding other ball shaped nano metal ultrafine powders of three grain-size grades of collecting respectively that pass through; Carry out in particle classifying and the collection process, under the acting in conjunction of supersonic airstream that described production circulation passage head superonic flow nozzzle 3 is produced and the set air-introduced machine 6 of afterbody, finish the whole particle classifying and the collection process of molybdenum powder.
In the actual production process, control adjustment by the high pressure oxygen (i.e. oxygen) and the input quantity of secondary oxygen and HC fuel that control oxygen cylinder 8 is provided, adjust accordingly with the redox ratio that high-temperature oxydation reaction and high temperature fast restore are reacted, the high pure spherical and the particle mean size that finally can obtain purity and be more than 99% are the molybdenum powder of 10-100nm.
Embodiment 2
In the present embodiment, processed raw material is that average grain diameter is selenium (Se) powder of 60 μ m, thereby different with the high-purity nano-metal ultrafine powder production equipment among the embodiment 1 be: the raw material that is adopted is carried and pretreatment unit 1 is that source of the gas (promptly under the HC fuel effect) carries out powder feeding for raw material conveying and pretreatment unit two and with the HC fuel, and described dust feeder is that powder feeder 1 and described powder feeder 1 inside are provided with ignition.During actual the use, the selenium powder after also can will lighting as dust feeder with the powder feeding swash plate is sent into high temperature spray combustion fast restore device 4.Described high temperature spray combustion fast restore device 4 front portions are provided with the powder feeding passage 4-9 that the discharging opening with powder feeder 1 joins.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 1 is: adopt raw material to carry in the step 1 and pretreatment unit two carries out raw material and carries and preliminary treatment, specifically be to adopt the selenium powder after powder feeder 1 will be lighted by ignition to send into high temperature spray combustion fast restore device 4 under the effect of HC fuel, and powder feed rate is 10kg/h.In the actual process, can be according to powder feed rate 4-13kg/h scope in corresponding adjust of concrete needs with powder feeder 1.Selenium powder body after lighting is carried and pretreatment unit 1 inner generation high-temperature oxydation reaction at raw material.And, adopting by HC fuel 0.1-0.4Mpa, preferred 0.3Mpa lights as the powder feeding source of the gas and to it; And in this step, the gas pressure of the described oxygen cylinder 8 high pressure oxygen that provides is 0.15Mpa, and the pressure of supersonic airstream is 0.3Mpa and with consumed cabin air 〉=3m 3The speed of/min atomizes.In the step 3, the gas pressure intensity of the LPG that sends into or LNG be 0.25Mpa, it is 0.05Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen, the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.2Mpa, and finally generating average grain diameter is the ball ultra micro powder (being the spherical ultra micro powder of Se) of 80nm.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 1.
Embodiment 3
In the present embodiment, processed raw material is that diameter is that copper (Cu) silk and the average grain diameter of 2mm is indium (In) powder, gallium (Ga) powder and selenium (Se) powder of 60 μ m, and the atomic molar of prepared product requirement ratio is 1: 0.7~1: 0.1~0.3: 2, during actual processing and preparing, can the molar content of Se be adjusted in the 1.3-2.5 scope according to concrete needs.Thereby in the present embodiment, different with the high-purity nano-metal ultrafine powder production equipment among the embodiment 1 is: raw material conveying of being adopted and pretreatment unit 1 are to the wire of input simultaneously and metal-powder is carried and pretreated raw material is carried and pretreatment unit three.Described raw material is carried and pretreatment unit three comprises and has wire input unit and can be to importing the arc gum that wire and metal dust carry out arc-melting simultaneously, and the charging aperture place of arc gum is provided with dust feeder.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 1 is: adopt raw material to carry in the step 1 and pretreatment unit three carries out raw material and carries and preliminary treatment, specifically be to adopt wire pushing roller 2 and dust feeder respectively Cu silk and In, Ga and Se powder to be carried simultaneously, the wire feed rate of wire pushing roller 2 is 15m/min, and the powder feed rate of described dust feeder is 0.8kg/h; And adopt electric arc that arc gum produced simultaneously Cu silk and In, Ga and Se powder to be carried out arc-melting.During actual processing and fabricating,, tackle the wire feed rate of wire pushing roller 2 and the powder feed rate of dust feeder mutually and adjust accordingly according to the component of mixing of made finished product.When sending into Cu silk and In, Ga and Se powder are carried out arc-melting, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding alloyed oxide that generates.In this step, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, and output voltage is that 30V and output current are 300A, and the arc energy that arc gum produced melts Cu silk and In, Ga and Se powder simultaneously; Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.2Mpa.The supersonic airstream that is produced by superonic flow nozzzle 3 in the step 2 is atomized into alloyed oxide ultra micro liquid mist with the alloy liquation that is generated, and the alloyed oxide ultra micro liquid mist that is generated is admitted to high temperature spray combustion fast restore device 4 under the effect of superonic flow nozzzle 3 supersonic airstream of sending into.In the present embodiment, the pressure of supersonic airstream is 0.5Mpa and with consumed cabin air 〉=3m 3The speed of/min atomizes.In the step 3, the gas pressure intensity of the LPG that sends into or LNG be 0.3Mpa, it is 0.05Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen, the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.25Mpa, final generation average grain diameter is CIGS (Cu (In, Ga) Se of 80nm 2) compound powder.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 1.
During actual processing and fabricating,, also can produce the nano metal alloy ultra micro powder of multiple different content by changing raw-material kind and input speed and relevant control parameter.
Embodiment 4
In the present embodiment, processed raw material is allumen (wherein the content of Zn is a 95wt%) silk, thereby used high-purity nano-metal ultrafine powder production equipment and embodiment 1 are identical.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 1 is: in the step 1, the wire feed rate of wire pushing roller 2 is 5.5m/min, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, output voltage is that 32V and output current are 200A, and the electric arc that arc gum produced carries out arc-melting to Zn-Al alloy wire.Simultaneously, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding metal oxide that generates.Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.1Mpa.In the step 2, the pressure of supersonic airstream is 0.5Mpa and with consumed cabin air 〉=3m 3The speed of/min atomizes.In the step 3, it is 0.04Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen, and the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.14Mpa, and the spherical aluminium that finally generates particle diameter and be 10-100nm is mixed zinc oxide (ZAO) powder.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 1.
Embodiment 5
In the present embodiment, processed raw material is the zinc silk, thereby used high-purity nano-metal ultrafine powder production equipment and embodiment 1 are identical.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 1 is: in the step 1, the wire feed rate of wire pushing roller 2 is 4.5m/min, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, output voltage is that 36V and output current are 400A, and the electric arc that arc gum produced carries out arc-melting to the zinc silk.Simultaneously, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding metal oxide that generates.Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.1Mpa.In the step 2, the pressure of supersonic airstream is 0.4Mpa and with consumed cabin air 〉=3m 3The speed of/min atomizes.In the step 3, do not feed reducing atmosphere, it is 0.04Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen, and the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.14Mpa, and finally generating particle diameter is the spherical oxide powder and zinc of 10-100nm.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 1.
Embodiment 6
In the present embodiment, processed raw material is a copper wire, thereby used high-purity nano-metal ultrafine powder production equipment and embodiment 1 are identical.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 1 is: in the step 1, the wire feed rate of wire pushing roller 2 is 7m/min, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, output voltage is that 30V and output current are 400A, and the electric arc that arc gum produced carries out arc-melting to copper wire.Simultaneously, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding metal oxide that generates.Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.15Mpa.In the step 2, the pressure of supersonic airstream is 0.5Mpa and with consumed cabin air 〉=3m 3The speed of/min atomizes.In the step 3, the gas pressure intensity of the LPG that sends into or LNG be 0.2Mpa, it is 0.05Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen, the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.2Mpa, and finally generating purity is more than 99% and granularity is the high pure spherical copper powder of 10-100nm.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 1.
Embodiment 7
In the present embodiment, processed raw material is a tungsten filament, thereby used high-purity nano-metal ultrafine powder production equipment and embodiment 1 are identical.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 1 is: in the step 1, the wire feed rate of wire pushing roller 2 is 3.5m/min, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, output voltage is that 36V and output current are 400A, and the electric arc that arc gum produced carries out arc-melting to tungsten filament.Simultaneously, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding metal oxide that generates.Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.16Mpa.In the step 2, the pressure of supersonic airstream is 0.8Mpa and with consumed cabin air 3m 3The speed of/min atomizes.In the step 3, the gas pressure intensity of the LPG that sends into or LNG be 0.2Mpa, it is 0.04Mpa that described secondary oxygen supply advance 4-5 to provide the pressure of secondary oxygen, the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.2Mpa, and finally generating purity is more than 99% and granularity is the high pure spherical tungsten powder of 10-100nm.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 1.
Embodiment 8
In the present embodiment, processed raw material is iron (Fe) silk, thereby used high-purity nano-metal ultrafine powder production equipment and embodiment 6 are identical.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 6 is: in the step 1, the wire feed rate of wire pushing roller 2 is 3.0m/min, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, output voltage is that 30V and output current are 300A, and the electric arc that arc gum produced carries out arc-melting to iron wire.Simultaneously, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding metal oxide that generates.Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.65Mpa.In the step 2, the pressure of supersonic airstream is 0.3Mpa and with consumed cabin air 3m 3The speed of/min atomizes.In the step 3, the gas pressure intensity of the LPG that sends into or LNG be 0.2Mpa, it is 0.13Mpa that described secondary oxygen supply advance 4-5 to provide the pressure of secondary oxygen, the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.78Mpa, and finally generating purity is more than 99% and granularity is the high pure spherical iron powder of 10-100nm.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 6.
Embodiment 9
In the present embodiment, processed raw material is silver (Ag) silk, thereby used high-purity nano-metal ultrafine powder production equipment and embodiment 8 are identical.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 6 is: in the step 1, the wire feed rate of wire pushing roller 2 is 3.5m/min, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, output voltage is that 28V and output current are 200A, and the electric arc that arc gum produced carries out arc-melting to filamentary silver.Simultaneously, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding metal oxide that generates.Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.8Mpa.In the step 2, the pressure of supersonic airstream is 0.3Mpa and with consumed cabin air 〉=3m 3The speed of/min atomizes.In the step 3, the gas pressure intensity of the LPG that sends into or LNG be 0.4Mpa, it is 0.18Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen, the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.98Mpa, and finally generating purity is more than 90% and granularity is the high pure spherical silver powder of 10-100nm.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 6.
Embodiment 10
In the present embodiment, processed raw material is tin (Sn) silk, thereby used high-purity nano-metal ultrafine powder production equipment and embodiment 8 are identical.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 6 is: in the step 1, the wire feed rate of wire pushing roller 2 is 3.0m/min, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, output voltage is that 30V and output current are 300A, and the electric arc that arc gum produced carries out arc-melting to the tin silk.Simultaneously, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding metal oxide that generates.Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.8Mpa.In the step 2, the pressure of supersonic airstream is 0.3Mpa and with consumed cabin air 〉=3m 3The speed of/min atomizes.In the step 3, the gas pressure intensity of the LPG that sends into or LNG be 0.4Mpa, it is 0.15Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen, the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.95Mpa, and finally generating purity is more than 92% and granularity is the high pure spherical glass putty of 10-100nm.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 6.
Embodiment 11
In the present embodiment, processed raw material is nickel (Ni) silk, thereby used high-purity nano-metal ultrafine powder production equipment and embodiment 8 are identical.
In the present embodiment, different with high-purity nano-metal ultrafine powder production method among the embodiment 6 is: in the step 1, the wire feed rate of wire pushing roller 2 is 2.0m/min, the DC input voitage of the direct-current arc power supply 13 that joins with arc gum is 380V, output voltage is that 26V and output current are 50A, and the electric arc that arc gum produced carries out arc-melting to nickel wire.Simultaneously, under the effect of oxygen cylinder 8 oxygen that provides, the metal melt that is generated behind the arc-melting is carried and pretreatment unit three inner generation high-temperature oxydations reactions at raw material, and the corresponding metal oxide that generates.Raw material is carried and the pressure of the pretreatment unit 1 interior oxygen cylinder 8 high pressure oxygen that provides is 0.6Mpa.In the step 2, the pressure of supersonic airstream is 0.3Mpa and with consumed cabin air 3m 3The speed of/min atomizes.In the step 3, the gas pressure intensity of the LPG that sends into or LNG be 0.4Mpa, it is 0.1Mpa that described secondary oxygen supply import 4-5 provides the pressure of secondary oxygen, the total pressure of described oxygen cylinder 8 high pressure oxygen that provides and secondary oxygen is 0.7Mpa, and finally generating purity is more than 99% and granularity is the high pure spherical nickel powder of 10-100nm.In the present embodiment, all the other procedure of processings, operation principle and the course of work are all identical with embodiment 6.
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, everyly any simple modification that above embodiment did, change and equivalent structure changed, all still belong in the protection domain of technical solution of the present invention according to the technology of the present invention essence.

Claims (10)

1. the production equipment of a high-purity nano-metal ultrafine powder, it is characterized in that: comprise processed raw material is carried and pretreated raw material conveying and pretreatment unit (1), be arranged on that raw material is carried and pretreatment unit (1) is inner and the metal oxide that raw material obtains be atomized into the superonic flow nozzzle (3) of metal oxide liquid mist after preliminary treatment, charging aperture and raw material are carried and the discharging opening of pretreatment unit (1) joins and described metal oxide liquid mist high temperature reduction can be reacted into the high temperature spray combustion fast restore device (4) of ball shaped nano metal ultrafine powder, described ball shaped nano metal ultrafine powder is carried out rapid condensation and can prevent effectively that the ball shaped nano metal ultrafine powder that generates from the inert gas rapid condensation device (5) of oxidation further taking place, with multistage metal ultrafine powder grading plant and a plurality of powder gathering-device (11) that is laid in described multistage metal ultrafine powder grading plant below respectively and joins with described multistage metal ultrafine powder grading plant below discharging opening that inert gas rapid condensation device (5) discharging opening joins, described inert gas rapid condensation device (5) joins and the inner reaction vessel that inert gas is housed for the discharging opening of charging aperture and high temperature spray combustion fast restore device (4); Described raw material is carried and pretreatment unit (1), high temperature spray combustion fast restore device (4), inert gas rapid condensation device (5) and described multistage metal ultrafine powder grading plant inside are communicated with the production circulation passage that composition is handled processed raw material successively, and described production circulation passage afterbody is connected with the air-introduced machine (6) that communicates with its inside, raw material is carried and the charging aperture and the oxygen cylinder (8) of pretreatment unit (1) join, and superonic flow nozzzle (3) joins with air compressor (9); The reaction vessel of described high temperature spray combustion fast restore device (4) for joining by pipeline and reducing atmosphere source of the gas, and the last correspondence of high temperature spray combustion fast restore device (4) has reducing atmosphere import (4-4);
Described processed raw material is wire and/or metal-powder, and described raw material is carried and pretreatment unit (1) should be mutually the wire of independent input is carried and pretreated raw material carries and pretreatment unit one, the metal-powder of independent input is carried and pretreated raw material is carried and pretreatment unit two and to the wire of input simultaneously with metal-powder is carried and pretreated raw material is carried and pretreatment unit three; Described raw material carry and pretreatment unit one by have the wire input unit and can to the input wire carry out the device of arc of arc-melting, the charging aperture of high temperature spray combustion fast restore device (4) and the discharging opening of described device of arc join; Described raw material is carried and pretreatment unit two comprises dust feeder, and the charging aperture of high temperature spray combustion fast restore device (4) and the discharging opening of described dust feeder join; Described raw material is carried and pretreatment unit three comprises and has wire input unit and can be to importing the device of arc that wire and metal dust carry out arc-melting simultaneously, and the charging aperture place of described device of arc is provided with dust feeder; Described device of arc and direct-current arc power supply (13) join.
2. according to the production equipment of the described a kind of high-purity nano-metal ultrafine powder of claim 1, it is characterized in that: described high temperature spray combustion fast restore device (4) comprises that having preceding plug (4-2) rearward end is uncovered external shell (4-1), has feed openings (4-3), a plurality of reducing atmosphere import (4-4) and a plurality of secondary oxygen supply imports (4-5) that feed for described metal oxide liquid mist on the described preceding plug (4-2); The oxygen that described oxygen cylinder (8) is provided enters high temperature spray combustion fast restore device (4) by feed openings (4-3); Described external shell (4-1) inside is provided with corresponding cooling water inlet (4-6) and the coolant outlet (4-7) that joins with described water cooling pipeline that have on water cooling pipeline and its sidewall; Feed openings (4-3) is carried with raw material and the discharging opening of pretreatment unit (1) joins, and the rearward end of external shell (4-1) is uncovered to communicate with inert gas rapid condensation device (5) inside.
3. according to the described a kind of high-purity nano-metal ultrafine powder production equipment of claim 2, it is characterized in that: described external shell (4-1) is a cylindrical shell, preceding plug (4-2) is circular, feed openings (4-3) is arranged on preceding plug (4-2) center, a plurality of reducing atmosphere imports (4-4) along the circumferential direction evenly are laid in feed openings (4-3) outside, and a plurality of secondary oxygen supply imports (4-5) along the circumferential direction evenly are laid in described a plurality of reducing atmosphere imports (4-4) outside; In described a plurality of reducing atmosphere imports (4-4) the reducing atmosphere jet blower is housed all, secondary oxygen jet blower all is housed in a plurality of secondary oxygen supply imports (4-5).
4. according to the production equipment of claim 2 or 3 described a kind of high-purity nano-metal ultrafine powders, it is characterized in that: described raw material is carried and pretreatment unit (1), high temperature spray combustion fast restore device (4) and inert gas rapid condensation device (5) are assembled into one and the coaxial setting of three.
5. according to the production equipment of the described a kind of high-purity nano-metal ultrafine powder of claim 4, it is characterized in that: described raw material carries and pretreatment unit (1) is cylindrical structural with high temperature spray combustion fast restore device (4) and the external diameter of the two is identical; Described raw material is carried and pretreatment unit (1) and high temperature spray combustion fast restore device (4) are installed as that the charging aperture from inert gas rapid condensation device (5) penetrates inert gas rapid condensation device (5) inside after the one, and is tightly connected between the sidewall of the charging aperture of inert gas rapid condensation device (5) and raw material conveying and pretreatment unit (1) or high temperature spray combustion fast restore device (4).
6. according to the production equipment of claim 1,2 or 3 described a kind of high-purity nano-metal ultrafine powders, it is characterized in that: described multistage metal ultrafine powder grading plant comprises successively the three grades of high-pressure electrostatic grading plants (10) that join with inert gas rapid condensation device (5) discharging opening.
7. one kind is utilized the method for the production equipment production high-purity nano-metal ultrafine powder of high-purity nano-metal ultrafine powder according to claim 1, it is characterized in that this method may further comprise the steps:
Step 1, raw material are carried and preliminary treatment: when the processed raw material of import is wire, adopt described device of arc that the metal to be treated silk of sending into by wire feeder is carried out arc-melting; When the processed raw material of import is wire and metal dust, adopt described device of arc that metal to be treated silk and the metal dust of sending into by wire feeder and dust feeder carried out arc-melting simultaneously; When carrying out arc-melting, the output voltage of described direct-current arc power supply (13) is that 26-36V and its output current are 20-400A; When sending into wire or wire and metal dust are carried out arc-melting, under the effect of oxygen cylinder (8) oxygen that provides, the metal melt that is generated behind the arc-melting is carried and the reaction of the inner generation of pretreatment unit (1) high-temperature oxydation at raw material, and the corresponding metal oxide that generates;
When the processed raw material of import is metal dust, adopts described dust feeder and be that source of the gas carries out powder feeding, and should will light before the powder feeding described HC fuel with the HC fuel; Under the effect of oxygen cylinder (8) oxygen that provides, the metal-powder after lighting is carried and the reaction of the inner generation of pretreatment unit (1) high-temperature oxydation at raw material, and the corresponding metal oxide that generates;
Step 2, metal oxide atomizing and carrying: in the step 1 when generating metal oxide, the supersonic airstream that is produced by superonic flow nozzzle (3) is atomized into metal oxide liquid mist with the metal oxide that is generated, and the metal oxide liquid mist that is generated is admitted to high temperature spray combustion fast restore device (4) under the effect of superonic flow nozzzle (3) supersonic airstream of sending into;
The conveying of the reaction of step 3, high temperature fast restore and the ball shaped nano metal ultrafine powder that generates: after the high pressure oxygen that described metal oxide liquid mist is provided together with supersonic airstream and oxygen cylinder (8) is admitted to high temperature spray combustion fast restore device (4) inside, correspondingly in inside is high temperature spray combustion fast restore device (4) under the reducing atmosphere, carry out the high temperature reduction reaction, and generate the size-controllable spherical nano-metal ultrafine powder; The ball shaped nano metal ultrafine powder that is generated is admitted to inert gas rapid condensation device (5) under the effect of superonic flow nozzzle (3) supersonic airstream that produces;
Step 4, rapid condensation: after described ball shaped nano metal ultrafine powder is admitted to inert gas rapid condensation device (5), carry out described ball shaped nano metal ultrafine powder by the inner inert gas that is full of of inert gas rapid condensation device (5) and carry out rapid condensation, described indifferent gas physical efficiency effectively prevents described ball shaped nano metal ultrafine powder generation secondary oxidation simultaneously;
Step 5, particle classifying and collection: successively the nano-metal ultrafine powder after rapid condensation is carried out multiple fractionation by described multistage metal ultrafine powder grading plant, and corresponding to corresponding other ball shaped nano metal ultrafine powder of a plurality of grain-size grades of collecting respectively of a plurality of powder gathering-devices (11); Carry out in particle classifying and the collection process, under the acting in conjunction of supersonic airstream that described production circulation passage head superonic flow nozzzle (3) is produced and the set air-introduced machine of afterbody (6), finish whole particle classifying and collection process.
8. according to the production method of the described high-purity nano-metal ultrafine powder of claim 7, it is characterized in that: the high temperature spray combustion fast restore device (4) described in the step 3 joins by pipeline and secondary oxygen supply source of the gas, and the last correspondence of high temperature spray combustion fast restore device (4) has secondary oxygen supply import (4-5); Correspondingly, the high pressure oxygen that the high temperature fast restore reacts described metal oxide liquid mist and provided together with supersonic airstream and oxygen cylinder (8) in the step 3 is admitted to high temperature spray combustion fast restore device (4) inner the time, in high temperature spray combustion fast restore device (4), feed secondary oxygen by secondary oxygen supply import (4-5), to guarantee in the described metal oxide liquid mist that unburned metal melt and/or metal dust fully burn, and being converted into metal oxide fully, the corresponding again high temperature fast restore that carries out under reducing atmosphere reacts.
9. according to the production method of the described high-purity nano-metal ultrafine powder of claim 8, it is characterized in that: the pressure of raw material conveying and the interior oxygen cylinder of pretreatment unit (1) (8) the high pressure oxygen that provides is 0.1-0.95MPa in the step 1; The pressure of supersonic airstream described in step 2, step 3 and the step 5 is 0.3-0.8MPa; The interior oxygen cylinder of the spray combustion of high temperature described in step 3 fast restore device (4) (8) the total pressure of the high pressure oxygen that provides and secondary oxygen supply import (4-5) the secondary oxygen that provides be 0.1-0.98MPa, the pressure of reducing atmosphere is 0.15~1.3MPa described in the spray combustion of high temperature described in the step 3 fast restore device (4).
10. according to the production method of claim 7 or 8 described high-purity nano-metal ultrafine powders, it is characterized in that: the reducing atmosphere described in the step 3 is a HC fuel.
CN2009102192077A 2009-11-27 2009-11-27 Equipment and method for producing high-purity nano-metal ultrafine powder Expired - Fee Related CN101716683B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2009102192077A CN101716683B (en) 2009-11-27 2009-11-27 Equipment and method for producing high-purity nano-metal ultrafine powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2009102192077A CN101716683B (en) 2009-11-27 2009-11-27 Equipment and method for producing high-purity nano-metal ultrafine powder

Publications (2)

Publication Number Publication Date
CN101716683A CN101716683A (en) 2010-06-02
CN101716683B true CN101716683B (en) 2011-11-30

Family

ID=42431372

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2009102192077A Expired - Fee Related CN101716683B (en) 2009-11-27 2009-11-27 Equipment and method for producing high-purity nano-metal ultrafine powder

Country Status (1)

Country Link
CN (1) CN101716683B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103273067B (en) * 2013-06-19 2015-08-12 四川坤森微纳科技股份有限公司 Micro-nano ball-type metal powder preparation system and technique thereof
CN106493379B (en) * 2016-12-12 2018-02-27 佛山市金纳新材料科技有限公司 A kind of 3D printing powder Preparation equipment and its application method
CN111298522A (en) * 2020-03-31 2020-06-19 西北工业大学 Separation device and method for metal powder condensed phase combustion products
CN112338198B (en) * 2020-10-29 2022-08-05 中国科学院过程工程研究所 Micron-sized molybdenum powder and preparation method and application thereof
CN112299483B (en) * 2020-10-29 2022-02-01 中国科学院过程工程研究所 Nano molybdenum dioxide and preparation method and application thereof
WO2022156229A1 (en) * 2021-01-25 2022-07-28 钟笔 Controller for controlling formation of ultrafine powder particles

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201529772U (en) * 2009-11-27 2010-07-21 西安慧维纳米金属材料有限公司 Production device of high-pure nanometer metal ultrafine powder

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201529772U (en) * 2009-11-27 2010-07-21 西安慧维纳米金属材料有限公司 Production device of high-pure nanometer metal ultrafine powder

Also Published As

Publication number Publication date
CN101716683A (en) 2010-06-02

Similar Documents

Publication Publication Date Title
CN101716683B (en) Equipment and method for producing high-purity nano-metal ultrafine powder
CN107243640B (en) High-performance metal ceramic composite powder used as thermal spraying structure feed and preparation method thereof
CN102910630A (en) Production method of nano silicon powder
CN110181066A (en) High sphericity 3D printing tantalum powder, preparation method and application
CN108557783B (en) Preparation method of high-purity nano titanium nitride powder
CN106670505A (en) Method for preparing tungsten-cobalt-carbon composite powder through spray pyrolysis method
CN108500283B (en) Method for preparing nano tungsten powder by low-cost two-stage reduction
CN103219514B (en) Method for assisted preparation of carbon composite lithium iron phosphate micro-nanometer powder through industrially modified starch
CN105772737A (en) Method for preparing dispersion-strengthening copper powder through in-situ oxidation-reduction method
CN103920887A (en) Method for preparing WC-Co powder used for thermal spraying
CN102078965A (en) Method for preparing WC-Co (tungsten carbide-cobalt) nano-powder
CN102248171A (en) Gas atomization method for preparing oxygen supersaturated iron-based alloy powder
CN103484814A (en) Preparation method of titanium boride based inorganic composite coating
CN105648383A (en) Preparing method for WC-Co composite powder for thermal spraying
CN102909386B (en) Production method of superfine spherical aluminium powder
CN102489710B (en) Method for increasing collection efficiency in preparing nanometer copper-silver alloy powder by using inductive plasmas
CN110385442A (en) A kind of production method of silver paste of solar cells ultrafine silver bismuth powder
CN107470646A (en) A kind of preparation method of ultrafine tungsten powder composite granule
CN105798316A (en) Processing technology of nanoscale tungsten powder
KR20200003302A (en) Manufacturing method of metal poswer for 3 dimentional printer
CN102059343A (en) Manufacturing method for nano-fabric NiCr-Cr3C2 compound granulation powder used for hot spraying
CN113909479A (en) Preparation method of superfine spherical zirconium powder capable of realizing particle size classification
CN102299016A (en) Method for forming silver-base alloy contact directly
CN201529772U (en) Production device of high-pure nanometer metal ultrafine powder
CN101891193A (en) Sol-gel Method for preparing nano vanadium carbide

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20111130

Termination date: 20131127