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EP3766601A1 - Poudre de titane et son procédé de production - Google Patents

Poudre de titane et son procédé de production Download PDF

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Publication number
EP3766601A1
EP3766601A1 EP19767251.2A EP19767251A EP3766601A1 EP 3766601 A1 EP3766601 A1 EP 3766601A1 EP 19767251 A EP19767251 A EP 19767251A EP 3766601 A1 EP3766601 A1 EP 3766601A1
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EP
European Patent Office
Prior art keywords
titanium
powder
mgcl
less
raw material
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.)
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Application number
EP19767251.2A
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German (de)
English (en)
Other versions
EP3766601A4 (fr
Inventor
Shigehisa Takenaka
Kenji Hirashima
Kazuhiro Taki
Kazuya Saito
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Toho Technical Service Co Ltd
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Toho Technical Service Co Ltd
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Publication of EP3766601A1 publication Critical patent/EP3766601A1/fr
Publication of EP3766601A4 publication Critical patent/EP3766601A4/fr
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • 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
    • B22F9/023—Hydrogen absorption
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/048—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by pulverising a quenched ribbon

Definitions

  • the present invention relates to a titanium-based powder, and more particularly, to an entirely novel titanium-based powder and a method for producing the same, which are produced by a Hydrogenation-DeHydrogenation method (hereinafter, referred to as an HDH method).
  • a Hydrogenation-DeHydrogenation method hereinafter, referred to as an HDH method
  • the prior art documents relating to the production of the titanium-based powder include patent document 1 and patent document 2.
  • the titanium powder and titanium alloy powder are referred to as the titanium-based powder.
  • the present invention is intended to solve the above problems, that is, to provide a titanium-based powder with reduced pores in the titanium-based powder.
  • the present invention In order to achieve the production of the titanium-based powder having a small number of pores as described above, in the present invention, a structure and a mechanism of a generation of the pores were analyzed in detail. As a result, it was found that the number of pores generated was significantly changed by adjusting the raw material and the producing method of the titanium-based powder, and we focused on the analysis results that the generation of pores was the pores having a substantially circular (spherical) cross-sectional shape remain due to the presence of gas (or the presence of gas in the past) in the titanium-based powder.
  • a titanium-based powder having a ratio of a pore area obtained by dividing a cross-sectional area of pores in a cross-section of the titanium-based powder by an area of the cross-section of the titanium-based powder is 0.3% or less is provided.
  • the titanium-based powder may be HDH powder.
  • a method for producing a titanium-based powder includes a Hydrogenation-DeHydrogenation method including a hydrogenation process, a pulverization process, and a dehydrogenation process using a titanium-based raw material is provided.
  • a concentration of total MgCl 2 contained in the titanium-based raw material is 1.0 mass% or less, and a concentration of internal MgCl 2 contained in the titanium-based raw material is 0.1 mass% or less.
  • the titanium-based raw material may have a maximum thickness of 20 mm or less.
  • a hydrogenation titanium-based powder may be pulverized to have a D95 particle size of 300 ⁇ m or less in the pulverizing process.
  • the titanium-based raw material may be hydrogenated within a temperature range of 716°C or more and 1050°C or less over a period of 90 minutes or more in the hydrogenation process.
  • the pore generation in titanium-based powder is closely related to gas.
  • the number of titanium-based powders containing pores can be significantly reduced by not entraining gas in the titanium-based powder, not generating gas inside the titanium-based powder, or by quickly removing the generated gas from inside the titanium-based powder.
  • titanium powder Most of the titanium powder is currently made from sponge titanium produced by the Kroll method. In some cases, scrap is used as a raw material from the viewpoint of economic efficiency and resource protection.
  • the Kroll method is a method of obtaining metallic titanium by reducing titanium tetrachloride (TiCl 4 ) obtained by chlorinating titanium ore with magnesium (Mg).
  • MgCl 2 remaining on the surface of the sponge titanium (surface MgCl 2 ) which is not sufficiently removed in the separation process can be removed by applying heat in a reduced pressure again.
  • MgCl 2 trapped inside the sponge titanium inner MgCl 2 ) cannot be removed by this method.
  • the method for producing the titanium powder is roughly divided into the atomization method and the HDH method.
  • the titanium powder is produced by melting titanium raw material, forming fine liquid particles of titanium liquefied in the Ar gas, and simultaneously quenching and solidifying the particles.
  • the first is a mechanism in which MgCl 2 present inside the titanium raw material (inner MgCl 2 ) is gasified at once and rapidly quenched, whereby the gasified MgCl 2 is trapped inside the particles of the liquefied titanium so that the pores are generated in the titanium powder.
  • the second is a mechanism in which the liquefied titanium particles are solidifying by incorporating Ar gas or vaporized MgCl 2 gas so that the pores are generated in the titanium powder. Therefore, it has been concluded that the HDH method is suitable for achieving the object of the present invention.
  • the HDH method is a method of obtaining the titanium powder by once hydrogenating titanium raw material to form fragile TiH 2 , then pulverizing and dehydrogenating.
  • it is a method for producing the titanium powder (HDH powder) by a process of hydrogenation, pulverization, dehydrogenation, and crushing.
  • the above crushing process is optional, but in the production of the titanium powder (HDH powder) is preferably subjected to a crushing process.
  • the titanium raw material is charged into a vacuum replaceable hydrogenation furnace, hydrogenated at a temperature of 400°C or higher in hydrogen gas atmosphere, and obtained the body of titanium hydride by substituting the Ar gas atmosphere from the hydrogen gas atmosphere.
  • the titanium raw material is hydrogen embrittled by the process of hydrogenation.
  • the next step is the pulverization process.
  • the body of titanium hydride is mechanically pulverized to the titanium hydride powder having a mechanical fractured surface, a pulverized surface.
  • the resulting titanium hydride powder is classified and/or sieved to remove the fine powder of titanium hydride.
  • the pulverization device such as a ball mill or a vibration mill may be used for the mechanical pulverization of titanium hydride, and a sieve separation device such as a circular vibrating sieve or an air flow classifier may be used for adjusting the particle size of the titanium hydride powder.
  • the above-mentioned titanium hydride powder is put into a container, charged into a dehydrogenation furnace of a vacuum heating type, and obtain the dehydrogenated titanium powder, for example, by heating at the temperature of 450°C or more in a vacuum of 10 -3 Torr (0.13Pa) or less. Ar gas is inserted in the container as needed.
  • the present inventors have studied and investigated the conditions in each producing process of the HDH method in detail from the viewpoint of the pores, and examined how to prevent the generation of the pores.
  • the HDH method if titanium is not melted and liquefied during each producing process, Ar gas in the atmosphere is not incorporated and does not cause the pores.
  • Heat treatment in the HDH method is consisting of two processes of hydrogenation and dehydrogenation, both of them should be performed below the melting point.
  • stainless steel is generally used as a container for containing the titanium material, when the iron contained in the stainless steel and titanium came into contact with each other and the temperature of both becomes equal to or higher than the eutectic temperature of iron and titanium, titanium becomes a liquid and does not meet the above purpose.
  • the present inventor has found that it is necessary to control titanium below the eutectic temperature of iron and titanium and prevent the liquefaction of titanium in order to prevent the generation of the pores. That is, it becomes an important component of the present invention to control the upper limit of the temperature.
  • Patent Document 1 and Patent Document 2 there is only described that the temperature has been raised to 650°C in the vacuum atmosphere, and there is no description about the temperature control of the titanium material after the subsequent introduction of the hydrogen gas. Since the hydrogenation reaction for hydrogenating titanium is an exothermic reaction, initially, for example, hydrogen absorption is performed at 650°C in a vacuum furnace, but thereafter, the temperature rises spontaneously. Therefore, it is necessary to finely control how to put into the container of titanium material, the charge amount of hydrogen and Ar, the charging time, and cooling to suppress the temperature rise while constantly observing the temperature of each site etc., so that the eutectic temperature or less at any location including a local.
  • the boiling point of MgCl 2 at normal pressure is 1412°C, and at this temperature, MgCl 2 trapped inside the titanium raw material (inner MgCl 2 ) gasifies.
  • the melting point of titanium is 1668°C, titanium is present in the solid state at 1412°C.
  • the gasified inner MgCl 2 has a larger volume compared to the solid state, which causes a very high pressure state to be formed inside the titanium. This high pressure condition due to the gasified inner MgCl 2 generates cracks in the hydrogenated titanium which has become embrittled by hydrogenation, from which MgCl 2 can be discharged to the outside of the titanium hydride.
  • the container containing the titanium material is often stainless steel, and it cannot be raised above the eutectic temperature of iron and titanium (1085°C).
  • MgCl 2 is set to liquid phase by setting the temperature of the titanium raw material to a temperature equal to or higher than the melting point of MgCl 2 (714°C) at a minimum, and the volume of MgCl 2 is expanded relative to the state of the solid.
  • the inner MgCl 2 has a larger volume in the liquid state than in the solid state, which causes a very high pressure state inside the titanium.
  • This high pressure condition due to the inner MgCl 2 of liquid phase causes cracking in the hydrogenated titanium which has become embrittled by hydrogenation.
  • MgCl 2 of liquid phase exposed to the outside of the titanium by cracking is allowed to vaporize by gradual evaporation.
  • the control of the temperature and heating time (maintaining time of the temperature) in the furnace in this case is also determined by considering the thickness and hydrogenation time of the titanium raw material to be hydrogenated.
  • the temperature of the titanium raw material can be set in a range from the melting point of MgCl 2 (714°C) or more to less than the eutectic temperature of iron and titanium (1085°C), but more reliable temperature control can be performed by setting the above temperature range.
  • titanium of the raw material is prevented from being melted by controlling the temperature.
  • MgCl 2 is vaporized during the process of the HDH method if MgCl 2 is attached to the surface of the titanium raw material, it is preferable to make it high-vacuum in order to remove MgCl 2 of the surface.
  • the total MgCl 2 concentration of the titanium raw material should be kept at 1.0 mass% or less. Then, the total MgCl 2 concentration of the titanium raw material is preferably suppressed to 0.05 mass% or less, more preferably suppressed to 0.001 mass% or less.
  • MgCl 2 concentration present in the interior of the titanium raw material is 0.5 mass% or less, it was found that it is possible to efficiently remove MgCl 2 responsible for the pores even when the time of maintaining the temperature of the titanium raw material in the range from the melting point of MgCl 2 (714°C) or more to less than the eutectic temperature of iron and titanium (1085°C) is 90 minutes in the HDH method.
  • the effect is more clearly exhibited by setting the MgCl 2 concentration present in the interior of the titanium raw material (internal MgCl 2 concentration) to 0.1 mass% or less.
  • the MgCl 2 concentration trapped inside the titanium raw material is preferably 0.1 mass% or less, more preferably 0.001 mass% or less.
  • the titanium raw material has a maximum thickness of 20mm or less, more preferably 10mm or less.
  • the maximum thickness of the titanium raw material is 20mm or less, hydrogen is sufficiently diffused inside the raw material during hydrogenation for rapidly causing cracks to embrittle titanium.
  • the method of measuring the concentration of total MgCl 2 is described.
  • the chlorine concentration of the target titanium raw material is measured by a silver nitrate titration method (JIS H 1615).
  • the value of the chlorine concentration is converted into the MgCl 2 concentration, and this is defined as MgCl 2 concentration (total MgCl 2 concentration) contained in the titanium raw material.
  • the method of measuring the concentration of the inner MgCl 2 is described. First, the target titanium raw material is heat-treated under reduced pressure (50pa or less) at about 750°C for 1 hour to remove MgCl 2 of the surface. Thereafter, the chlorine concentration of the present material is measured by a silver nitrate titration method (JIS H 1615). The value of the chlorine concentration is converted into the MgCl 2 concentration, and this is defined as an MgCl 2 concentration trapped and present inside the titanium raw material (internal MgCl 2 concentration).
  • JIS H 1615 silver nitrate titration method
  • the particle diameter of the titanium hydride powder may be 300 ⁇ m or less, preferably 150 ⁇ m or less.
  • the particle diameter of the titanium hydride powder produced and pulverized by the HDH method has a distribution, and 95% or more of the particle diameter of the total titanium hydride powder may be equal to or less than the above value.
  • the D95 particle diameter of the titanium hydride powder is 300 ⁇ m or less, and it is more effective if the D95 particle diameter is suppressed to 150 ⁇ m or less.
  • the lower limit of the D95 particle diameter is not particularly limited, but may be 70 ⁇ m or more, and may be 80 ⁇ m or more, as an example.
  • D95 refers to a particle size at which a volume-based cumulative distribution is 95% in a particle size distribution measurement obtained by a laser diffraction/scattering method. For details, it is measured based on JIS Z8825:2013.
  • 95% or more of the total titanium particle diameter of the titanium powder produced and crushed by the HDH method may be 150 ⁇ m or less.
  • the titanium powder produced by the HDH method described above has less MgCl 2 residue.
  • the titanium powder produced by the HDH method of the present invention is suitable as a raw material powder for obtaining a spherical powder by melting (e.g., plasma melting) the surface of the titanium powder, and spheronizing the angular surface which is a pulverized surface or a crushed surface. Since the titanium powder produced and crushed by the HDH method has a pulverized surface or a crushed surface having an uneven structure, it is possible to promote melting when introduced into the plasma due to its wide surface area. Since there is no entrainment of plasma gas such as Ar even if the titanium powder surface is melted to spheronize, new pores can be suppressed.
  • the present embodiment has been described based on the titanium powder.
  • the raw material titanium alloy is prevented from melting by controlling the temperature by the HDH method, and the same effect as the titanium powder can be obtained.
  • the element to be contained in titanium is preferably 20 mass% or less, more preferably 15 mass% or less.
  • the titanium alloy powder may contain multiple types of elements.
  • the titanium alloy powder may be Ti-AI-V alloy powder.
  • the Ti-AI-V powder can have an Al content of 5.5 to 7.5 mass% and a V content of 3.5 to 4.5 mass%.
  • the value (pore area ratio of the cross section) obtained by dividing the cross-sectional area of the encapsulated pores (hereinafter referred to as internal pores) observed in any cross-section of the titanium-based powder by the area of the cross-section of the titanium-based powder can be realized 0.3% or less. It is preferable that the titanium-based powder produced in the present invention has a number of the inner pores which appear by observing an arbitrary cross-section of the titanium-based powder of 20pieces/mm 2 or less per unit area.
  • the pore area ratio of the titanium-based powder cross-section of 0.3% or less means that, after embedding the titanium-based powder in the resin and polishing, a value obtained by dividing the cross-sectional area of the inner pore observed as an image ranging from the brightness of 90 to 250 by the total cross-sectional area of the powder is 0.3% or less by the image processing, when the cross-section is observed by an optical microscope at a magnification of 500 times and an arbitrary location of 700 ⁇ m ⁇ 500 ⁇ m size is observed at 16 locations.
  • the number of the internal pores means the number of the internal pores observed as images in the range of brightness 90-250 by image processing during the above observation. In any observation, the powder having a major axis of 10 ⁇ m or less is excluded by image processing.
  • FIG.1 is a photograph before image processing and FIG.2 is a photograph after image processing). Even if the two pores were clearly in contact, they were calculated as one as long as they were one internal pore connected by image processing.
  • the pore area ratio of the above cross-section is 0.3% or less, the titanium powder produced by the manufacturing method according to the present invention is suitable for use in a technical field in which the pores must be small(e.g., an Air-craft material or the like).
  • the pore area ratio of the cross-section exceeds 0.3 percent, it is difficult to use in the technical field.
  • the sponge titanium was used as the titanium raw material.
  • the titanium raw material had total MgCl 2 concentration and internal MgCl 2 concentration of 0.05mass% or less, and a diameter of 1/2 inch or less.
  • the atmosphere was heated to 650°C with a heater, and held for 120 minutes. Thereafter, hydrogen was supplied to cause a reaction of hydrogen adsorption and heat generation, and the titanium raw material was hydrogenated for 120 minutes while controlling the temperature so as to be 1000°C or less by controlling the heater, insertion of Ar gas, and operating the cooling device.
  • the temperature range at this time was 716°C or more and 1000°C or less.
  • the bulk density of the titanium raw material at the process of hydrogenation was 1.2g/cm 3 .
  • the body of titanium hydride was pulverized by a pulverizer/classifier to obtain the titanium hydride powder having a particle diameter of 10 ⁇ m to 150 ⁇ m.
  • the body of dehydrogenated titanium was subjected to crushing treatment.
  • the D95 particle diameter of the obtained titanium powder was 100 ⁇ m.
  • Titanium powder was embedded in the resin, polished the cross-section of the sample, and observed at 16 locations of arbitrary locations of 700 ⁇ m ⁇ 500 ⁇ m size with an optical microscope at a magnification of 500.
  • the number of pores and the area ratio the number of detected pores was 20pieces/mm 2 per unit area.
  • the pore area ratio was 0.11%.
  • the chip produced using the sponge titanium raw material having a total MgCl 2 concentration of 0.1 mass% or less, having a total MgCl 2 concentration of 0.0002 mass% or less and a maximum thickness of 7mm thereof was used as a titanium raw material. That is, the inner MgCl 2 concentration of the titanium raw material was also 0.0002 mass% or less.
  • the atmosphere was heated to 650°C with a heater, and held for 120 minutes. Thereafter, hydrogen was supplied to cause a reaction of hydrogen adsorption and heat generation, and the titanium raw material was hydrogenated for 120 minutes while controlling the temperature so as to be 1000°C or less by controlling the heater, insertion of Ar gas, and operating the cooling device.
  • the temperature range at this time was 716°C or more and 1000°C or less.
  • the bulk density at the process of hydrogenation was 1.2g/cm 3 .
  • the body of titanium hydride was pulverized by a pulverizer/classifier to obtain the titanium hydride powder having a particle diameter of 10 ⁇ m to 150 ⁇ m.
  • the body of dehydrogenated titanium was subjected to crushing treatment.
  • the D95 particle diameter of the obtained titanium powder was 100 ⁇ m.
  • Titanium powder was embedded in the resin, polished the cross-section of the sample, and observed at 16 locations of arbitrary locations of 700 ⁇ m ⁇ 500 ⁇ m size with an optical microscope at a magnification of 500.
  • the number of detected pores was 8pieces/mm 2 per unit area.
  • the pore area ratio was 0.02%.
  • the titanium powder was produced from two types: the titanium raw material having the concentration of iron as an impurity of 200 ppm by mass or less and the titanium raw material having the concentration of iron of more than 200 ppm by mass and 500 ppm by mass or less.
  • the number of detected pores ranged from 8 to 10pieces/mm 2 per unit area.
  • the pore area ratio was 0.02%. Therefore, it is considered that the amount of iron as an impurity, in other words, the purity of titanium, is not correlated with the behavior of the pore.
  • the 90%Ti-6%AI-4%V (mass%) chips produced using the sponge titanium raw material having a total MgCl 2 concentration of 0.1 mass% or less and an alloy of 60%AI-40%V was used as the raw material.
  • the total MgCl 2 concentration of the titanium-alloy chips used as a raw material was 0.0002 mass% or less, and its maximum thickness was 7mm. That is, the inner MgCl 2 concentration of the titanium-alloy chips was also 0.0002 mass% or less. After vacuuming 300kg of the raw material to 5Pa or less, the atmosphere was heated to 650°C with a heater, and held for 120 minutes.
  • the titanium alloy chip was hydrogenated for 120 minutes while controlling the temperature so as to be 1000°C or less by controlling the heater, insertion of Ar gas, and operating the cooling device.
  • the temperature range at this time was 716°C or higher 1000°C or less.
  • the bulk density at the process of hydrogenation was 1.2g/cm 3 .
  • the body of titanium hydride was pulverized by a pulverizer/classifier to obtain the powders of 10 ⁇ m to 150 ⁇ m.
  • the body of dehydrogenated titanium was subjected to crushing treatment.
  • the D95 particle diameter of the obtained titanium powder was 100 ⁇ m.
  • Titanium alloy powder was embedded in the resin, polished the cross-section of the sample, and observed at 16 locations of arbitrary locations of 700 ⁇ m ⁇ 500 ⁇ m size with an optical microscope at magnification of 500.
  • the number of detected pores was 9pieces/mm 2 per unit area.
  • the pore area ratio was 0.03%.
  • the titanium alloy powder obtained above was spheroidized by melting the surface by Ar gas as a plasma gas using the high-frequency heat induction plasma apparatus.
  • the conditions for spheronization are as shown in Table 1.
  • An optical micrograph of the obtained titanium alloy powder is shown in FIG.4 .
  • the titanium alloy powder was embedded in the resin, and the cross-section of the sample was observed at 16 locations of arbitrary locations of 700 ⁇ m ⁇ 500 ⁇ m size with an optical microscope at magnification of 500.
  • the pore area ratio was 0.01%.
  • the titanium alloy powder produced and crushed by the HDH method was confirmed to be useful as a raw material powder of the spherical powder.
  • the 89%Ti-7%AI-4%V (mass%) chips produced using the sponge titanium raw material having the total MgCl 2 concentration of 0.1 mass% or less and an alloy of 70%AI-40%V was used as the raw material.
  • the total MgCl 2 concentration of the titanium-alloy chips used as the raw material was 0.0002 mass% or less, and its maximum thickness was 2mm. That is, the inner MgCl 2 concentration of the titanium-alloy chips was also 0.0002 mass% or less. After vacuuming 300kg of the raw material to 5Pa or less, the atmosphere was heated to 650°C with a heater, and held for 120 minutes.
  • the titanium alloy chip was hydrogenated for 120 minutes while controlling the temperature so as to be 1000°C or less by controlling the heater, insertion of Ar gas, and operating the cooling device.
  • the temperature range at this time was 716°C or higher 1000°C or less.
  • the bulk density at the process of hydrogenation was 1.2g/cm 3 .
  • the body of the titanium hydride was pulverized by a pulverizer/classifier to obtain the powder of 10 ⁇ m to 150 ⁇ m.
  • the body of dehydrogenated titanium was subjected to crushing treatment.
  • the D95 particle diameter of the obtained titanium powder was 100 ⁇ m.
  • Titanium alloy powder was embedded in resin, polished the cross-section of the sample, and observed at 16 locations of arbitrary locations of 700 ⁇ m ⁇ 500 ⁇ m size with an optical microscope at magnification of 500.
  • the number of detected pores was 9pieces/mm 2 per unit area.
  • the pore area ratio was 0.03%.
  • the method for producing the titanium powder according to the present embodiment is also suitable for producing the titanium alloy powder.
  • Titanium powder was produced using the sponge titanium having the inner MgCl 2 concentration of 0.2 mass% as a titanium raw material, otherwise under the same conditions as in Example 1.
  • the total MgCl 2 concentration of the sponge titanium was 0.3 mass%.
  • Titanium powder was embedded in resin, polished cross-section of the sample, and observed at 16 locations of arbitrary locations of 700 ⁇ m ⁇ 500 ⁇ m size with an optical microscope at magnification of 500.
  • the number of pores and area ratio were analyzed, and the detected pores were 85pieces/mm 2 per unit area.
  • the pore area ratio was 0.7%.
  • Titanium powder produced by the gas atomization method having the same particle diameter as in Example 1. Titanium powder was embedded in the resin, polished the cross-section of the sample, and observed at 16 locations of arbitrary locations of 700 ⁇ m ⁇ 500 ⁇ m size with an optical microscope at magnification of 500. The number of pores and area ratio were analyzed, and the detected pores were 130pieces/mm 2 per unit area. The pore area ratio was 1.0% ( FIG.5 ).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
EP19767251.2A 2018-03-16 2019-03-06 Poudre de titane et son procédé de production Pending EP3766601A4 (fr)

Applications Claiming Priority (2)

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JP2018049468 2018-03-16
PCT/JP2019/008968 WO2019176700A1 (fr) 2018-03-16 2019-03-06 Poudre de titane et son procédé de production

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EP3766601A1 true EP3766601A1 (fr) 2021-01-20
EP3766601A4 EP3766601A4 (fr) 2021-12-01

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JP (1) JP6976415B2 (fr)
CN (1) CN112055628A (fr)
TW (1) TW201938810A (fr)
WO (1) WO2019176700A1 (fr)

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CN107760897A (zh) * 2017-10-30 2018-03-06 东北大学 以氢化海绵钛为原材料制造钛与钛合金及其零部件的方法

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JP6976415B2 (ja) 2021-12-08
EP3766601A4 (fr) 2021-12-01
CN112055628A (zh) 2020-12-08

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