WO2001036133A1 - Dispositif et procede de preparation d'une poudre tres fine faisant appel a la chaleur et a l'evaporation - Google Patents

Dispositif et procede de preparation d'une poudre tres fine faisant appel a la chaleur et a l'evaporation Download PDF

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Publication number
WO2001036133A1
WO2001036133A1 PCT/CN2000/000001 CN0000001W WO0136133A1 WO 2001036133 A1 WO2001036133 A1 WO 2001036133A1 CN 0000001 W CN0000001 W CN 0000001W WO 0136133 A1 WO0136133 A1 WO 0136133A1
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WO
WIPO (PCT)
Prior art keywords
evaporation chamber
heating
raw material
evaporation
laser
Prior art date
Application number
PCT/CN2000/000001
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English (en)
Chinese (zh)
Inventor
Changsheng Xie
Junhui Hu
Original Assignee
Huazhong University Of Science And Technology
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 Huazhong University Of Science And Technology filed Critical Huazhong University Of Science And Technology
Priority to AU19618/00A priority Critical patent/AU1961800A/en
Publication of WO2001036133A1 publication Critical patent/WO2001036133A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/20—Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
    • C01F7/422—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation with a gaseous oxidator at a high temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy

Definitions

  • the invention relates to a technique for preparing ultrafine powder. Specifically, it relates to a method and equipment for preparing ultrafine powder by heating and evaporation.
  • the heating temperature is generally lower than 2000 *, which makes this method unsuitable for the preparation of ultrafine powders of high melting point metals and alloys and high boiling non-metals and compounds.
  • This temperature is also lower than the boiling point of common metals and alloys.
  • the melting point of aluminum is 660t: but the boiling point is as high as 2450X; the melting point of copper is 1083; the boiling point is 25951 :; the melting point of iron is 1536 * and the boiling point is 3000 "C.
  • the heating temperatures for preparing ultrafine powders of aluminum, copper and iron by induction heating evaporation methods are generally 1400 ", 1500 *, 1600, respectively, which are far below their respective boiling points. Therefore, it is not difficult to understand that the production of ultrafine powders of metals, alloys and non-metals and compounds by induction heating is low.
  • both at home and abroad have been adopted to increase the evaporation area (enlarge the crucible diameter) and increase the power (which has exceeded 200KW).
  • the yield of ultrafine powders of metals and alloys prepared by this method is generally 0.1-0.5 Kg / hr, some of which are even lower than 0.1 Kg / h, and the energy consumption is huge, and the product is expensive.
  • a solid metal or alloy is heated in an emotional gas (Ar, He, etc.) to evaporate, and the evaporated atoms are cooled in a continuous collision with the gas molecules, reaching a supersaturated state, producing agglomerated growth and forming ultrafine powder .
  • the ultrafine powder prepared by the laser heating method has high purity, small particle size, concentrated distribution, and good sphericity.
  • solid metals and alloys have a strong ability to reflect laser light, and a large amount of energy is required to dissipate heat from the substrate. Therefore, it is inefficient to directly melt and evaporate metals and alloys with lasers to prepare ultrafine powders.
  • the purpose of the present invention is to solve the shortcomings of the method and equipment for preparing ultrafine powder in the prior art, and to provide an improved method which can not only maintain the cleanliness and purity of the ultrafine powder produced, but also improve the yield and yield of ultrafine powder.
  • Method and equipment for preparing ultrafine powder are to solve the shortcomings of the method and equipment for preparing ultrafine powder in the prior art, and to provide an improved method which can not only maintain the cleanliness and purity of the ultrafine powder produced, but also improve the yield and yield of ultrafine powder.
  • the present invention provides a method of heating evaporation preparing ultrafine powders:
  • the evaporation chamber is evacuated to IX 10 1 - starting material IX 10- 5 Pa, with a heating apparatus for heating for the preparation of superfine powder, During this period, a laser is introduced to the surface of the raw material to accelerate its melting and vaporization, and the evaporated vapor condenses to form ultrafine powder.
  • an inert gas is introduced to make the pressure of the evaporation chamber reach and maintain at IX 10 1 -IX 10 5 Pa, and then the next steps are performed.
  • the above-described method may also be evacuated evaporation chamber, introducing a reactive gas, the pressure of the evaporation chamber and maintained at 1 ⁇ 10 1 - 1 X 10 5 Pa, then the subsequent steps.
  • the above-described method may also be evacuated evaporation chamber, introducing an inert gas and reactive gas, the pressure in the evaporation chamber and maintained at 1 X 10 1 - 1 X 10 5 Pa, then the subsequent steps.
  • the present invention also provides an evaporation chamber device for implementing the above method, including: a container with a laser inlet on the wall, a raw material heating zone and a heating device provided in the container, and a raw material heating zone provided above the raw material heating zone.
  • Metal tube which is fixed on the wall of the container and connected to the powder trap.
  • the heating device in the above evaporation chamber device may be an induction heater, a resistance heater or an arc heater; a cooling device may be arranged on the outer surface of the metal tube; a raw material heating zone may be provided with a crucible for storing raw materials; The crucible is set and sent directly to the raw material heating zone.
  • the wall of the container in the evaporation chamber device may be provided with a feed port through which raw materials are fed, and may also have one or two gas ports through which the inert gas and the reactive gas are introduced separately or simultaneously.
  • the lower end of the metal tube in the container can also be equipped with a radiation protection cover communicating with it.
  • the radiation protection cover can be designed in a spherical shape, and laser through holes and raw material through holes can be opened on it.
  • the invention has the advantages that when preparing ultrafine powder of metal or alloy, the metal or alloy is heated and melted by using a heating device to maintain a high temperature and has a large absorption rate for laser light, Then, the laser is introduced into the evaporation chamber, and acts on the surface of the liquid metal or alloy, so that its laser action zone reaches or approaches the boiling point, forming a high pressure gradient and temperature gradient near the upper part of the liquid metal or alloy surface, and accelerating the evaporation of the surface of the liquid metal or alloy
  • the preparation of ultrafine powder by using the present invention can increase the yield, increase the output, reduce energy consumption and production cost, and maintain the high purity and cleanliness of the ultrafine powder.
  • FIG. 1 is a schematic structural diagram of an embodiment of an evaporation chamber device used for a method of preparing ultrafine powder by laser and heating.
  • Fig. 1 is a schematic structural view of another embodiment of an evaporation chamber device for a method of preparing ultrafine powder by laser and heating.
  • Fig. 1 shows a specific embodiment in which a crucible is provided in the raw material heating zone.
  • a laser inlet 13 On the wall of the double-layer internally cooled stainless steel container 6, there is a laser inlet 13, a gas inlet 7, or two gas inlets 7, 8, and a feed inlet 3 and an observation window 4 may also be opened.
  • the raw materials in the container 6 The heating zone 14 is provided with a high temperature resistant crucible 9 and an induction heater 5, the crucible 9 contains a raw material 10 for preparing ultrafine powder, and a metal tube 2 is arranged above the crucible 9, the metal tube 2 and a trap and an exhaust The devices are connected, and a cooling device 1 is arranged on the outer surface.
  • the cooling device 1 is composed of water-cooled or fluorine-cooled steel pipes, and is directly brazed to the outer wall of the metal pipe 2.
  • the metal pipe 2 is fixed on the wall of the container 6.
  • the metal tube 2 is a collecting channel of the ultrafine powder, and the cooling device 1 cools the evaporated raw material vapor through the wall of the metal tube, and suppresses the growth of the ultrafine powder.
  • a radiation protection cover 11 is installed at the lower end of the metal tube 2 and communicates with the metal tube 2.
  • a laser through hole 12 and a material opening 15 are opened thereon. When a metal or alloy is used as a raw material, it is used to block liquid metal or The alloy directly irradiates the laser.
  • the radiation shield 11 adopts a spherical shape design, and improves the thermal efficiency of the evaporated metal and the alloy through spherical reflection.
  • the laser enters the evaporation chamber through the laser inlet 13 and interacts with the raw materials in the crucible 9. Before the laser enters the evaporation chamber, it can be changed by the adjusting device on the liquid surface of the raw materials. Laser spot size.
  • the introduced laser can be a CO 2 gas laser or a YAG solid laser.
  • an inert gas or reactive gas (0 2 , N 2 , NH 3 , H 2 , CH 4 , C 2 H 2, etc.) is introduced from the gas inlet 7; when two gas inlets are opened At 7, 8 hours, inert gas or reactive gas is introduced from the gas inlets 7, 8 respectively.
  • the introduction of inert gas can better control the evaporation pressure and protect the molten pool.
  • ultrafine powder of metal, nonmetal or alloy When only inert gas is introduced, ultrafine powder of metal, nonmetal or alloy is generated, and when only reactive gas or both inert gas and reactive gas are introduced, ultrafine powder of compound is generated.
  • the dynamic feeding device connected to the feeding port raw materials can be added dynamically and in real time, so that the liquid level of the raw materials in the crucible 9 is maintained within a fixed height range.
  • the observation window 4 the evaporation process of the raw materials in the evaporation chamber can be observed.
  • the evaporation chamber is evacuated to IX 10 1 - IX 10- 5 Pa , and then introduced into the inert gas inlet 7 from the gas, the gas from the inlet 8 to a reactive gas,
  • the evaporation chamber pressure was brought to IX 10 1 -IX 10 5 Pa, the induction heater 5 was turned on, and the raw material in the crucible 9 was heated until it melted.
  • the laser is introduced to act on the surface of the molten pool (it can also be introduced before the raw material is melted), so that the raw material is quickly evaporated.
  • start the dynamic feeding device to add raw materials into the crucible 9.
  • the generated ultrafine powder is dynamically and continuously collected by the cooled metal pipe 2 and the trap connected to it.
  • Figure 2 shows an embodiment where the rod-shaped raw material enters the raw material heating zone directly through the feed port.
  • a feeding port 3 is opened on the wall of the container 6, and the rod-shaped raw material 10 is dynamically and real-time fed into the raw material heating zone 14 from the feeding port 3, so that the top of the raw material 10 is maintained within a fixed height range, and the laser passes through the laser inlet. 13 and the laser through hole 12 directly act on the top of the raw material 10 in the raw material heating zone 14.
  • the raw material 10 is melted by the resistance heater 16 and the laser and evaporated.
  • rod-shaped pure titanium is continuously fed from the feeding port.
  • the evaporation chamber is pre-evacuated to 1 x 10-iPa, and then filled with argon and a small amount of oxygen to 5 x 103 Pa.
  • the arc heater was started to heat the titanium rod to a higher temperature.
  • a 400W YAG laser was introduced, and the laser was irradiated on a pure titanium rod through a focusing lens. 22nm average particle diameter of the ultrafine Ti0 2, with a yield of 0.4 kg / hr.
  • the invention can be used for preparing ultrafine powder.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne un dispositif et un procédé de préparation d'une poudre très fine faisant appel à la chaleur et à l'évaporation. Dans des conditions d'atmosphère inerte ou réactive, on chauffe une matière métallique ou d'alliage ou non métallique ou un composé chimique par induction, par résistance ou à l'arc électrique que l'on soumet directement à un laser sous forme gazeuse CO2 ou sous forme solide YAG de manière à accélérer sa fusion et sa gazéification. Sur la partie adjacente à la surface du métal ou alliage, on obtient un gradient élevé de pression et un gradient élevé de température ce qui accélère l'évaporation du métal fondu et augmente le taux de poudre très fine. On augmente ainsi la production de poudre sans tirer les coûts à la hausse. Le dispositif de préparation de la poudre utilise un laser spécifique prévu combiné à une chambre d'évaporation de chauffage sous vide.
PCT/CN2000/000001 1999-11-18 2000-01-04 Dispositif et procede de preparation d'une poudre tres fine faisant appel a la chaleur et a l'evaporation WO2001036133A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU19618/00A AU1961800A (en) 1999-11-18 2000-01-04 Process and equipment for preparing superfine powder by heating and evaporation

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN99120058.6 1999-11-18
CN99120058.6A CN1250701A (zh) 1999-11-18 1999-11-18 加热蒸发制备超微粉的方法和设备

Publications (1)

Publication Number Publication Date
WO2001036133A1 true WO2001036133A1 (fr) 2001-05-25

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PCT/CN2000/000001 WO2001036133A1 (fr) 1999-11-18 2000-01-04 Dispositif et procede de preparation d'une poudre tres fine faisant appel a la chaleur et a l'evaporation

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CN (1) CN1250701A (fr)
AU (1) AU1961800A (fr)
WO (1) WO2001036133A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005097379A1 (fr) * 2004-04-08 2005-10-20 Alexei Konstantinovich Axenov Procede de production de suspensions de poudres
US20220193768A1 (en) * 2020-12-23 2022-06-23 Hamilton Sundstrand Corporation Method and apparatus for manufacturing powder for additive manufacturing

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100444995C (zh) * 2004-07-22 2008-12-24 北京颐鑫安科技发展有限公司 超细铝粉及纳米级铝粉的生产方法
CN100402196C (zh) * 2005-12-21 2008-07-16 北京工业大学 金属粉末激光微成型气体保护装置
CN101239391B (zh) * 2008-02-27 2010-06-02 天津大学 激光合成碳包覆金属纳米颗粒的方法
CN102815870B (zh) * 2011-06-10 2016-08-03 深圳市纳宇材料技术有限公司 一种纳米玻璃粉及其制备方法和用途
CN102632234B (zh) * 2012-04-27 2013-10-16 四川大学 超细w-k金属粉末的真空热蒸发混料工艺
CN104392883A (zh) * 2014-10-22 2015-03-04 常州博锐恒电子科技有限公司 一种注入机固体进料方法
CN105129829B (zh) * 2015-08-31 2017-08-04 国家电网公司 一种三氧化二铝纳米刺球制作装置
CN105598460B (zh) * 2016-03-21 2018-03-06 台州市金博超导纳米材料科技有限公司 用于制造微纳米级金属粉末的高温蒸发器
CN110814357A (zh) * 2018-08-14 2020-02-21 深圳市百柔新材料技术有限公司 纳米材料制备设备和方法
CN109759601A (zh) * 2019-01-25 2019-05-17 大连理工大学 激光蒸发多腔体金属/碳纳米粉体连续生产方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5544123B2 (fr) * 1973-11-30 1980-11-11
JPS56136634A (en) * 1980-03-29 1981-10-26 Res Dev Corp Of Japan Production of ultra-fine powder and particle using laser beam
CN1240687A (zh) * 1998-07-08 2000-01-12 华中理工大学 加热蒸发制备超微粉的方法和设备

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5544123B2 (fr) * 1973-11-30 1980-11-11
JPS56136634A (en) * 1980-03-29 1981-10-26 Res Dev Corp Of Japan Production of ultra-fine powder and particle using laser beam
CN1240687A (zh) * 1998-07-08 2000-01-12 华中理工大学 加热蒸发制备超微粉的方法和设备

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005097379A1 (fr) * 2004-04-08 2005-10-20 Alexei Konstantinovich Axenov Procede de production de suspensions de poudres
US20220193768A1 (en) * 2020-12-23 2022-06-23 Hamilton Sundstrand Corporation Method and apparatus for manufacturing powder for additive manufacturing

Also Published As

Publication number Publication date
AU1961800A (en) 2001-05-30
CN1250701A (zh) 2000-04-19

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