Classifications

• • 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
  • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
• • 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
  • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
• • 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
• • 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
  • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
  • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
• • 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
  • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
  • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
  • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
  • B22F2009/0848—Melting process before atomisation
• • 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
  • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
  • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
  • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
  • B22F2009/086—Cooling after atomisation

Definitions

• the present invention relates to a method and an apparatus for economically producing a metal powder having a high purity of an elemental metal and a uniform powder shape and particle size.
• the present invention relates to the production of titanium powder as the metal powder.
• Elemental metal raw materials are processed into various forms depending on the application, such as molded products, plate materials, rods, fine wires and foil materials.
• metal powders have been used as molding raw materials in the molding fields such as powder metallurgy and thermal spraying.
• powder metallurgy is widely regarded as important, for example, in the manufacture of mechanical parts, and the demand for metal powder as a starting material is also increasing.
• metal powders have been manufactured using the classical method of mechanically directly grinding metal particles into powder, or the method of blowing molten metal into powder by blowing it off with gas.
• the classical method of mechanically directly grinding metal particles into powder or the method of blowing molten metal into powder by blowing it off with gas.
• problems in the uniformity or economical efficiency of such a method there were difficulties in the uniformity or economical efficiency of such a method.
• an electrolytic production method is also known, and when a metal is deposited outside the range of electrolytic conditions for obtaining a smooth, dense and uniform crystal structure, a brittle sponge is obtained. It has been reported that metallic or powdery metals can be obtained.
• titanium in particular is a relatively new metal compared to ancient iron, copper, or aluminum, etc., and is widely used industrially by taking advantage of its light strength, high strength at high temperatures, and corrosion resistance. I have.
• jet engine materials in the aerospace field structural members of spacecraft or spacecraft, heat exchanger materials in thermal power generation and nuclear power generation, catalyst materials in the polymer chemical industry, eyeglass frames and golf club heads in the daily necessities field
• products such as health supplies, medical equipment, and medical and dental materials, and the fields of application are expanding. In the future, applications are competing with stainless steel and duralumin, etc., and it is expected that the material will surpass them.
• Titanium metal is difficult to machine and hard to cut, so when manufacturing mechanical parts with complicated shapes, if a molten material is used as a raw material, it is cut after plastic working such as hot forging or rolling. And other machining processes, which increases the number of manufacturing steps and increases the manufacturing cost. Therefore, when metal titanium is used, powder metallurgy is frequently used, which requires titanium powder, especially titanium powder with high purity and good uniformity in powder shape and particle size. . Even if titanium powder is manufactured by the conventional powder manufacturing method for metals in general, there are problems in terms of powder shape, particle size uniformity, economic efficiency, etc., as with other metals. Development of a method for producing titanium powder that is more excellent in terms of particle size and uniformity is awaited.
• a hydrodehydration method or a rotating electrode method has been put into practical use.
• the hydrodehydration method is based on the use of titanium sponge, a molten material, or chips generated by cutting or the like.
• this raw material As a raw material, this raw material is heated in a hydrogen atmosphere, absorbs hydrogen gas to be embrittled, and is crushed in this embrittled state, and then heated again in vacuum to release hydrogen gas to obtain a powder. Is the way.
• the rotating electrode method uses a material that is formed into a round bar from a melted material or a melt-processed material obtained by adding a process such as forging or rolling to the melted material, and the raw material of the round bar is inert gas such as argon or helium.
• the tip is melted by a heat source such as an arc or plasma arc while rotating at high speed in a gas atmosphere, and the flowing molten metal is scattered by centrifugal force to obtain a spherical powder.
• the titanium powder obtained by the hydrodehydrogenation method has irregular spheres and can be molded using a mold, but the heating step must be repeated twice. Although a mechanical pulverization process using a ball mill or the like can be performed, contamination of titanium powder with oxygen is inevitable. In addition, in the rotating electrode method, the titanium raw material melted in an inert gas is pulverized, so that the powder has a spherical shape, so that the flowability is good and there is no contamination by oxygen. There is a disadvantage that is inferior. Furthermore, since both of the above methods are of a batch type, there is a problem that the production cost of the powder increases.
• An atomizing method has been developed as a method for producing titanium powder that has solved such problems of quality and production cost. This involves melting the raw material in a water-cooled copper crucible using a heat source such as a plasma arc, causing the molten metal to flow continuously from one end of the crucible, and injecting an inert gas such as argon or helium into the molten metal flow. Is a method of obtaining powder by atomizing the powder. However, even in this method, since a molten material or a melt-processed material of titanium is used as a raw material, it was difficult to significantly reduce the production cost as compared with the conventional method.
• Japanese Patent Application Laid-Open No. 5-93213 discloses a method for producing powdered titanium which further reduces the production cost, avoids contamination by oxygen, and is easy to mold, has an irregular spherical shape, or has improved fluidity.
• a rod-shaped material solidified by cold isostatic pressing of titanium sponge is used as a molten metal stream in an inert gas, and an inert gas such as an argon-helium gas is injected into the molten metal stream.
• a powder can be obtained by atomizing the molten metal.
• the purity, the spherical shape of the powder, or the uniformity of the powder particle size were not satisfactory, and the production cost was not satisfactory. Disclosure of the invention
• metal powders especially metal titanium powders
• powder metallurgy are new products such as powder metallurgy.
• the necessity and demand are increasing along with the progress of the shaping method.However, powder manufacturing methods that can sufficiently respond to such demands have not been developed, and especially the purity of elemental metals, the spherical shape of powder and the like. There were problems with the uniformity of the particle size of the powder and the production cost.
• an object of the present invention is to provide an elemental metal powder raw material having excellent uniformity of the spherical shape of the powder and uniformity of the powder particle size for forming means such as powder metallurgy.
• the present inventor has proposed various methods for producing elemental metal powders such as titanium powder in order to solve problems such as purity of elemental metal, uniformity of spherical shape of powder, uniformity of powder particle size and production cost. Was considered.
• the present inventors have solved the above-mentioned problem by utilizing the technology regarding the utilization of titanium raw materials for the production of titanium-containing high-performance water, which was filed by the present inventor in a patent application (Japanese Patent Application No. 2000-136932). .
• the previously developed invention of the production of high-performance titanium-containing water (Japanese Patent Application No. 2000-136932) is characterized in that a mixed gas of oxygen and hydrogen is burned in high-pressure water, and the combustion gas is used to melt titanium metal. It is an invention of a method for producing high-performance water in which a titanium melt is dissolved, and by using this technology, in the production of elemental metal powders, especially metal titanium powders, the purity is high and the spherical shape of the powder is obtained. And a powder having excellent uniformity in powder particle size were obtained, and the production cost was significantly reduced.
• the present invention is completely different from the conventional method for producing metal powder or titanium powder in the concept or configuration. Basically, a mixed gas of oxygen and hydrogen is burned in high-pressure water, and the combustion gas is used. This method obtains metal powder submerged in water by melting elemental metal titanium. The method for producing metal powder has been improved from a completely different point from the conventional method.
• the metal raw material is heated without using conventional heating means such as heat melting, arc discharge or laser irradiation, and without powdering by flowing down molten metal or scattering and atomizing by gas. Element metal powder can be produced efficiently.
• the method of the present invention there is no generation of by-products or impurities other than the target metal powder.
• the generation of metal oxides due to heating of the metal raw material is extremely small, and the obtained metal powder has excellent uniformity of spherical shape and uniformity of powder particle size, so that the production cost can be significantly reduced. is there.
• continuous production is possible together with batch production, and mass production of metal powder with a uniform particle size is possible.
• the basic configuration of the present invention is to burn a mixed gas of oxygen and hydrogen in high-pressure water. Then, the elemental metal raw material is heated and powdered by the combustion gas to produce a metal powder having a uniform particle size.
• the outline of the production process is shown in a production flowchart in FIG.
• the present invention has the following constitutions (1) to (5), and comprises burning a mixed gas of oxygen and hydrogen in high-pressure water, and melting and pulverizing the metal raw material with the combustion gas. It is the basis.
• a method for producing metal powder by burning a mixed gas of oxygen and hydrogen in high-pressure water, heating the elemental metal raw material with the combustion gas, and pulverizing the raw material.
• the elemental metal raw material is titanium (T i), zirconium (Zr), germanium (Ge), tin (Sn), gold (Au), platinum (Pt), or silver (Ag).
• a method for producing a metal powder according to the above (1) characterized in that:
• a device for producing metal powder comprising a high-pressure water storage tank, a mixed gas injection nozzle of oxygen and hydrogen, an elemental metal material supply unit, a spark plug, and a pressure-resistant container equipped with a combustion chamber.
• the apparatus for producing metal powder according to (3) further including a water electrolysis apparatus for producing a mixed gas of oxygen and hydrogen.
• Fig. 1 Flow chart for manufacturing metal powder of the present invention
• titanium metal powder will be described as an example, but the present invention is not limited to the production of titanium powder.
• purified water such as distilled water in a high-pressure water storage tank in a metal titanium powder producing pressure-resistant container
• a metal titanium raw material such as a metal titanium rod
• an elemental metal raw material supply unit pressurize it under high pressure to inject hydrogen and oxygen from a nozzle as a mixed gas, ignite the mixed gas, completely burn the mixed gas in the combustion chamber, and create a complete ultra-high temperature steam gas combustion state.
• the titanium material is instantaneously dissolved in the combustion gas and dispersed in water. At this time, very fine titanium microparticles on the micron scale are generated, and are dispersed in a powdery state. The generated fine titanium powder settles in a short time without melting or floating.
• the production of titanium powder with high purity can be realized extremely efficiently, but for this purpose, the control of the amount of the mixed gas to be burned, the reaction pressure, and the supply amount of the metal titanium raw material are required. is important.
• the injection amount of the mixed gas of about 2 to 4 L per second is good, and if the gas pressure is too high, the structure of the apparatus becomes too large. There is a risk of destruction. If the pressure is low, the gas blows up from the nozzle, and the heated and melted metal fine particles are wrapped in bubbles as they are and diverge on the water, and the generation state of the metal fine particles deteriorates.
• the pressure of the water pressurized to a high pressure in the pressurized tank is 1.2 to 1.5 atm.
• a titanium raw material having the highest possible purity is preferable so as not to generate impurities in the titanium powder product.
• the metal titanium raw material may be used either of the bar and sheet or particles ⁇ Pi foil c
• the metal titanium raw material may be used either of the bar and sheet or particles ⁇ Pi foil c
• metal raw materials include, for example, zirconium, germanium, tin, gold, platinum, and silver, but are not limited thereto. It is not something to be done.
• the high-pressure water storage tank used in the apparatus of the present invention is a metal, preferably steel, pressure-resistant tank, and it is preferable that other members such as the combustion chamber are also made of steel.
• the gas pump is installed to eject the mixed gas at high pressure. Elemental metal raw materials are supplied continuously and continuously according to the amount of combustion.
• Element metal raw materials must be supplied at a position where the mixed gas completely burns and becomes completely high-temperature water vapor gas.Therefore, a combustion chamber for burning the mixed gas is installed. . This setting produces a pure metal powder without impurities or by-products. Also, high pressure is required to completely burn the pure gas mixture.
• FIG. 1 shows a flow chart for producing a metal powder according to the present invention as described above.
• the metal powder production apparatus A shown in FIG. 2 includes a high-pressure water storage tank 2, a mixed gas injection nozzle of oxygen and hydrogen 5, an elemental metal raw material supply unit 22, a spark plug 12 and a combustion chamber 7.
• Pressure vessel B The metal powder production apparatus A shown in FIG. 2 includes a high-pressure water storage tank 2, a mixed gas injection nozzle of oxygen and hydrogen 5, an elemental metal raw material supply unit 22, a spark plug 12 and a combustion chamber 7.
• Metal powder production equipment A is composed of a metal powder production pressure vessel B.
• the metal powder production pressure vessel has a gas jet pump 1, a high-pressure water storage tank 2, a combustion chamber 7, a pressure control valve 8, and a metal powder outlet. 1, 3, purified water 3, elemental metal raw material 21 for powder production, point hydrant 12, elemental metal raw material supply unit 2, and mixed gas jet nozzle 5. 4 represents the produced metal powder.
• Purified water 3 such as distilled water is injected into the high-pressure water storage tank 2 in the metal powder production pressure vessel B, and metal titanium material 21 such as metal titanium rods is supplied from the elemental metal raw material supply unit 22 And pressurize the mixture under high pressure, inject hydrogen and oxygen as a mixture gas from the nozzle 5, ignite the mixture gas with the igniter 12 and completely burn the mixture gas in the combustion chamber 7 to complete the combustion.
• Ultra-high temperature steam gas combustion is performed, and the titanium material is instantaneously melted in the combustion gas and dispersed in water.
• the supply of a mixed gas of hydrogen and oxygen requires precise control so that the ratio of hydrogen to oxygen is 2: 1.
• the mixed gas of hydrogen and oxygen is supplied from a commercially available gas cylinder.
• a water electrolysis device C is installed to produce a mixed gas of hydrogen and oxygen by electrolysis of water. Then, a completely pure gas can be obtained, and the mixed gas can be supplied efficiently and suitably.
• a water electrolysis device C instead of supplying a mixed gas of hydrogen and oxygen from a commercially available gas cylinder, a water electrolysis device C is provided, and if a mixed gas of hydrogen and oxygen is produced by electrolysis of water, it is completely pure. A simple gas can be obtained, and the mixed gas can be supplied easily and efficiently.
• the electrolyzer C is an optional device for producing and supplying a mixed gas of hydrogen and oxygen by electrolysis of water.
• the supply pipes 9 and 10 for hydrogen and oxygen gas, the electrodes 19 and 20, the partition 18 and the water 16 are shown.
• this electrolysis apparatus acidic or alkaline raw water is electrolyzed, and oxygen gas is generated at an anode and hydrogen gas is generated at a cathode, and supplied as a raw material gas for combustion.
• highly pure metal powder particularly titanium powder
• the production method of the present invention by-products other than the elemental components and impurities are not generated, and the obtained powder has extremely excellent spherical shape and uniformity of powder particle size, and further significantly reduces the production cost. be able to. Also, batch production, continuous production, and mass production are possible.

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• Manufacture Of Metal Powder And Suspensions Thereof (AREA)
• Powder Metallurgy (AREA)
• Physical Or Chemical Processes And Apparatus (AREA)

Priority Applications (10)

Applications Claiming Priority (2)

Publications (1)

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Country Status (14)

Cited By (3)

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Citations (2)

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• 2002
  • 2002-03-12 TW TW091104638A patent/TW570851B/zh not_active IP Right Cessation
  • 2002-03-26 KR KR10-2003-7011575A patent/KR20030080062A/ko not_active Application Discontinuation
  • 2002-03-26 PL PL02365332A patent/PL365332A1/xx not_active Application Discontinuation
  • 2002-03-26 WO PCT/JP2002/002911 patent/WO2002078883A1/ja not_active Application Discontinuation
  • 2002-03-26 EP EP02708666A patent/EP1393841A4/en not_active Withdrawn
  • 2002-03-26 CA CA002442153A patent/CA2442153A1/en not_active Abandoned
  • 2002-03-26 HU HU0303939A patent/HUP0303939A3/hu unknown
  • 2002-03-26 BR BR0208466-0A patent/BR0208466A/pt not_active IP Right Cessation
  • 2002-03-26 MX MXPA03008818A patent/MXPA03008818A/es unknown
  • 2002-03-26 US US10/472,702 patent/US20040118244A1/en not_active Abandoned
  • 2002-03-26 JP JP2002577135A patent/JP4137643B2/ja not_active Expired - Lifetime
  • 2002-03-26 CN CNB028071344A patent/CN1248812C/zh not_active Expired - Lifetime
  • 2002-03-26 NZ NZ528630A patent/NZ528630A/en unknown
• 2003
  • 2003-09-26 NO NO20034327A patent/NO20034327L/no not_active Application Discontinuation

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