CN1240687A - Method and equipment for preparing superfine powder by heating and evaporation - Google Patents
Method and equipment for preparing superfine powder by heating and evaporation Download PDFInfo
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- CN1240687A CN1240687A CN 98113626 CN98113626A CN1240687A CN 1240687 A CN1240687 A CN 1240687A CN 98113626 CN98113626 CN 98113626 CN 98113626 A CN98113626 A CN 98113626A CN 1240687 A CN1240687 A CN 1240687A
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- vaporization chamber
- metal
- alloy
- laser
- micro powder
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- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000001704 evaporation Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000008020 evaporation Effects 0.000 title claims abstract description 17
- 238000010438 heat treatment Methods 0.000 title claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 41
- 239000002184 metal Substances 0.000 claims abstract description 41
- 239000000956 alloy Substances 0.000 claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 33
- 238000009834 vaporization Methods 0.000 claims abstract description 25
- 230000008016 vaporization Effects 0.000 claims abstract description 25
- 230000006698 induction Effects 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 21
- 230000008676 import Effects 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 230000005855 radiation Effects 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 4
- 229910001338 liquidmetal Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000007738 vacuum evaporation Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 238000009835 boiling Methods 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000004093 laser heating Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
本发明公开了一种加热蒸发制备超微粉的方法和设备。在惰性气氛或反应性气氛条件下,用感应加热金属或合金的同时,引入大功率CO2气体激光或YAG固体激光直接作用于金属或合金,使其加速熔化和汽化,在液态金属或合金表面上部附近形成高的压力梯度和温度梯度,加速液态金属或合金的蒸发,进而增大超微粉产率,提高其产量,使生产成本大为下降。制粉系统采用了专门设计的激光与感应复合加热真空蒸发室。
The invention discloses a method and equipment for preparing superfine powder by heating and evaporating. Under the condition of inert atmosphere or reactive atmosphere, while the metal or alloy is heated by induction, a high-power CO 2 gas laser or YAG solid-state laser is introduced to directly act on the metal or alloy to accelerate its melting and vaporization, and on the surface of the liquid metal or alloy A high pressure gradient and temperature gradient are formed near the upper part to accelerate the evaporation of liquid metal or alloy, thereby increasing the yield of superfine powder, increasing its output, and greatly reducing the production cost. The pulverizing system uses a specially designed laser and induction combined heating vacuum evaporation chamber.
Description
The present invention relates to prepare the technology of ultra micro powder.Specifically, it relates to the method and apparatus that a kind of heating evaporation prepares the ultra micro powder.
When adopting the eddy-current heating evaporation to prepare metal and alloy ultra micro powder, its heating-up temperature generally is lower than 2000 ℃, these characteristics make this method not be suitable for the ultra micro powder of preparation refractory metal and alloy and compound, simultaneously, this temperature is also far below the boiling point of common metal and alloy, fusing point as aluminium is 660 ℃, and boiling point is but up to 2450 ℃; The fusing point of copper is 1083 ℃, and boiling point reaches 2595 ℃; The fusing point of iron is 1536 ℃, and boiling point is 3000 ℃.And generally be respectively 1400 ℃, 1500 ℃, 1600 ℃ with the heating-up temperature that the eddy-current heating evaporation prepares aluminium, copper, iron ultra micro powder, far below boiling point separately.Thereby to prepare the productive rate of metal and alloy ultra micro powder low with the eddy-current heating evaporation be understandable.In order to increase productive rate, to improve output, all adopt increase disengagement area (strengthening the crucible bore) and raising power (having surpassed 200KW) to realize both at home and abroad.But for above-mentioned reasons, the productive rate for preparing metal and alloy ultra micro powder in this way is generally at 0.1～0.5Kg/hr, and domestic productive rate is lower than 0.1Kg/hr.And energy consumption is huge, valuable product.See " Metal Substrate Investigation on Ultrafine Powders " (Zhongnan Polytechnic Univ's thesis for the doctorate, in October, 1997) that Yan Hongge delivers.
Utilize laser as thermal source, heat solid metal or alloy in inert gas (Ar, He etc.) makes it evaporation, evaporation atom with the continuous collision of gas molecule in cool off, reach hypersaturated state, produce the cohesion growth, form the ultra micro powder.With the ultra micro powder purity height that laser heating method is produced, particle diameter is little, distributes to concentrate, and sphere is good.But solid metal and alloy are strong to the albedo of laser, and matrix heat radiation also will consume big energy, therefore, directly with laser metal and alloy are carried out fusion and evaporation and to prepare the efficient of ultra micro powder lower.The interactive of laser and material be studies show that the absorptivity of material for laser light changes with temperature, its variation tendency is to increase with temperature rising absorptivity.Metal absorptivity to laser when room temperature is very little (to CO
2Laser, the absorptivity of Al, Cu, Fe is respectively 1.9%, 1.5%, 3.5%), when temperature was elevated near fusing point, its absorptivity can reach 40～50%; Near boiling point, its absorptivity is up to 90% as temperature.
The present invention is according to preparation metal and the eddy-current heating evaporation of alloy ultra micro powder and the These characteristics of LASER HEATING method, these two kinds of methods are compound, purpose is to provide a kind of brand-new laser and responds to the method and apparatus that compound heating evaporation prepares the ultra micro powder, on the high basis of the ultra micro powder cleannes that keep being produced and purity, improve the productive rate and the output of ultra micro powder.
The objective of the invention is to realize by following method and apparatus.
Heating evaporation prepares the method for ultra micro powder: vaporization chamber is evacuated to 1 * 10
1～1 * 10
-5Pa in the time of with eddy-current heating metal or alloy raw material, introduces laser action in the metal or alloy surface, makes it quicken fusing and vaporization, and by cooling, the metal or alloy devaporation that is evaporated becomes the ultra micro powder.
The vaporization chamber device of realizing said method comprises: have the container of laser import on the wall, be provided with crucible and induction heater in container.
Advantage of the present invention is to utilize eddy-current heating fusing metal or alloy, make it to keep higher temperature, and laser had bigger absorptivity, then laser is introduced vaporization chamber, act on liquid metal or alloy surface, its laser action district is reached or near boiling point, near liquid metal or alloy surface top, form high barometric gradient and thermograde, quicken the evaporation of liquid metal or alloy, and then can increase ultra micro powder productive rate, raising output, cut down the consumption of energy and production cost.
Accompanying drawing is to be used for laser and the compound structural representation that adds a kind of embodiment of vaporization chamber device of hot preparation ultra micro powder method of induction.
Describe optimum implementation of the present invention in detail below in conjunction with accompanying drawing.
In double-deck, have laser import 12 on the wall of cold rustless steel container 6, a gas feed 7 or two gas feeds 7,8, also can have charging aperture 3 and watch window 4, in container 6, be provided with resistant to elevated temperatures crucible 9 and induction heater 5, above crucible 9, be provided with metal tube 2, metal tube 2 links to each other with trap and air extractor, its outer surface is mounted with cooling device 1, cooling device 1 is made up of water-cooled or the cold copper pipe of fluorine, directly soldering is on metal tube 2 outer walls, and metal tube 2 is fixed on the wall of container 6.Metal tube 2 is capture passages of ultra micro powder, and cooling device then cools off by the metal and the alloy vapor of metal pipe-wall to evaporation, and suppresses the ultra micro powder and grow up.In the lower end of metal tube 2 radiation shield 10 is housed, and communicate with metal tube 2, have laser via 11 on it, be used for blocking the direct radiation of liquid metal or alloy to laser, radiation shield 10 adopts the sphere configuration design, improves the thermal efficiency of evaporated metal or alloy by the spheric reflection effect.
Laser enters vaporization chamber by laser import 12, and with crucible in metal or alloy raw material reciprocation, laser enters before the vaporization chamber, can change the laser facula size act on the metal or alloy liquid level by adjusting device, the laser of introducing can be CO
2Gas laser or YAG Solid State Laser.When having a gas feed 7, import inert gas or reactant gas (O from gas feed 7
2, N
2, NH
3, H
2, CH
4, C
2H
2Deng), when having two gas feeds 7,8, then import inert gas and reactant gas respectively from gas feed 7,8.Import inert gas and can control evaporating pressure better, and the protection molten bath.When only importing inert gas, generate metal or alloy ultra micro powder, when only importing reactant gas or importing inert gas and reactant gas simultaneously, generate compound ultra micro powder.By the dynamic feeding device that links to each other with charging aperture, can add raw material dynamically, in real time, the metal or alloy liquid level in the crucible is remained in the altitude range of fixing.Can observe the evaporation process of metal or alloy in the vaporization chamber by watch window.
To be placed in crucible and the dynamic feeding device through pretreated metal or alloy raw material, vaporization chamber is evacuated to 1 * 10
1～1 * 10
-5Pa then imports inert gas or reactant gas from gas feed 7, or imports inert gas from gas feed 7, imports reactant gas from gas feed 8, makes vaporization chamber pressure reach 1 * 10
-1～1 * 10
5Pa connects induction heater, and the raw material in the crucible is heated until fusing.Introduce laser action this moment in weld pool surface (also can before the raw material fusing, introduce), form the evaporating field of metal or alloy atom.Look the decline degree of liquid level in the crucible, start dynamic feeding device and in crucible, add raw material.The ultra micro powder that produces by the metal tube 2 that is cooled and coupled trap dynamically, collect continuously.
Embodiment 1:
Adopt 99.99% block pure iron, place Al
2O
3In the crucible.Vaporization chamber forvacuum to 1 * 10
-1Pa charges into argon gas to 1 * 10 then
3Pa.Start high frequency electric source, pure iron is heated to fusing.Introduce CO
2Laser, laser is through focus lamp, and spot diameter is φ 4mm, and laser power is 1000W.Obtaining average grain diameter is the pure iron ultra micro powder of 40nm, and its productive rate is 0.8 kilogram/hour.
Embodiment 2:
Adopt 99.99% block fine aluminium, place Al
2O
3In the crucible.Vaporization chamber forvacuum to 1 * 10
-1Pa charges into argon gas ten trace oxygens to 1 * 10 then
3Pa.Start high frequency electric source, fine aluminium is heated to fusing.Introduce CO
2Laser, laser is through focus lamp, and spot diameter is φ 4mm, and laser power is 800W.Obtain γ-Al
2O
3The ultra micro powder, it is as shown in the table through distributing for its grain, and productive rate is 0.6 kilogram/hour.
γ-Al
2O
3The ultra micro powder through the grain that distributes through scope (nm) 10～20 20～30 40～50 50～60 70～80 80～90 90～100 percentages (%) 12 32 19 15 322
Claims (8)
1. a heating evaporation prepares the method for ultra micro powder, it is characterized in that: vaporization chamber is evacuated to 1 * 10
1～1 * 10
-5Pa in the time of with eddy-current heating metal or alloy raw material, introduces laser action in the metal or alloy surface, makes it quicken fusing and vaporization, and by cooling, the metal or alloy devaporation that is evaporated becomes the ultra micro powder.
2. method according to claim 1 is characterized in that: after vaporization chamber vacuumizes, introduce inert gas, the pressure of vaporization chamber is reached and maintain 1 * 10
-1～1 * 10
5Pa.
3. method according to claim 1 is characterized in that: after vaporization chamber vacuumizes, introduce reactant gas, the pressure of vaporization chamber is reached and maintain 1 * 10
-1～1 * 10
5Pa.
4. method according to claim 1 is characterized in that: after vaporization chamber vacuumizes, introduce inert gas and reactant gas, the pressure of vaporization chamber is reached and maintain 1 * 10
-1～1 * 10
5Pa.
5. a vaporization chamber device that is used for claim 1 method comprises container (6), is provided with crucible (9) and induction heater (5) in container (6), it is characterized in that: have laser import (12) on the wall of container (6).
6. vaporization chamber device according to claim 5 is characterized in that: be provided with metal tube (2) in crucible (9) top, its outer surface is mounted with cooling device (1), and metal tube (2) is fixed on the wall of container (6).
7. vaporization chamber device according to claim 6 is characterized in that: in the lower end of metal tube (2) radiation shield (10) is housed, and communicates with metal tube (2), have laser via (11) on it.
8. vaporization chamber device according to claim 7 is characterized in that: radiation shield (10) adopts the sphere configuration design.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98113626A CN1075753C (en) | 1998-07-08 | 1998-07-08 | Method and equipment for preparing superfine powder by heating and evaporation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98113626A CN1075753C (en) | 1998-07-08 | 1998-07-08 | Method and equipment for preparing superfine powder by heating and evaporation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1240687A true CN1240687A (en) | 2000-01-12 |
| CN1075753C CN1075753C (en) | 2001-12-05 |
Family
ID=5223335
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98113626A Expired - Fee Related CN1075753C (en) | 1998-07-08 | 1998-07-08 | Method and equipment for preparing superfine powder by heating and evaporation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1075753C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001036133A1 (en) * | 1999-11-18 | 2001-05-25 | Huazhong University Of Science And Technology | Process and equipment for preparing superfine powder by heating and evaporation |
| CN102962466A (en) * | 2012-11-29 | 2013-03-13 | 哈尔滨工业大学 | Method for preparing metal nanoparticles through laser |
| CN111390186A (en) * | 2020-04-16 | 2020-07-10 | 北京科技大学顺德研究生院 | Preparation method of submicron spherical tantalum metal powder |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5853699B2 (en) * | 1979-12-27 | 1983-11-30 | セイコーエプソン株式会社 | Method for manufacturing rare earth intermetallic compound magnets |
| JPS6254005A (en) * | 1985-09-02 | 1987-03-09 | Hitachi Ltd | Production of hyperfine particles |
-
1998
- 1998-07-08 CN CN98113626A patent/CN1075753C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001036133A1 (en) * | 1999-11-18 | 2001-05-25 | Huazhong University Of Science And Technology | Process and equipment for preparing superfine powder by heating and evaporation |
| CN102962466A (en) * | 2012-11-29 | 2013-03-13 | 哈尔滨工业大学 | Method for preparing metal nanoparticles through laser |
| CN111390186A (en) * | 2020-04-16 | 2020-07-10 | 北京科技大学顺德研究生院 | Preparation method of submicron spherical tantalum metal powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1075753C (en) | 2001-12-05 |
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