EP3705588B1 - Procédé de purification de matériau à base de titane - Google Patents

Procédé de purification de matériau à base de titane Download PDF

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Publication number
EP3705588B1
EP3705588B1 EP18874635.8A EP18874635A EP3705588B1 EP 3705588 B1 EP3705588 B1 EP 3705588B1 EP 18874635 A EP18874635 A EP 18874635A EP 3705588 B1 EP3705588 B1 EP 3705588B1
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Prior art keywords
titanium
melting
titanium material
hydrogen
melting step
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German (de)
English (en)
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EP3705588A1 (fr
EP3705588A4 (fr
Inventor
Daisuke Matsuwaka
Takayuki Narushima
Kyosuke Ueda
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Kobe Steel Ltd
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Kobe Steel Ltd
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1295—Refining, melting, remelting, working up of titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04—Refining by applying a vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16—Remelting metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

Definitions

  • the present invention relates to a method for refining a titanium material in which oxygen contained in a titanium material made of a pure titanium, a titanium alloy or an intermetallic compound containing titanium as one of main components, and further hydrogen are removed from the titanium material.
  • titanium Since titanium is active, it is called active metal. Titanium is very easily combined with light elements such as oxygen, nitrogen, etc. Typically, once titanium is combined with such a light element, it is very difficult to remove the light element. Although titanium has excellent properties as described above, there is a problem that light elements combined with titanium are hardly removed. Further, there is another problem that titanium is more expensive than a steel material or an aluminum material that has been typically used. Because of those problems, currently, titanium has not been spread to the market yet.
  • Non-Patent Literature 1 or Non-Patent Literature 2 is a technical literature describing a method for removing contained oxygen from a titanium material such as a pure titanium or a titanium alloy by use of hydrogen.
  • Non-Patent Literature 1 describes that oxygen can be reduced by arc melting of sponge titanium or a Ti-6Al-4V alloy under an Ar atmosphere containing 1 to 30 vol% of H 2 .
  • oxygen concentration decreases from 0.04 mass% to 0.016 mass%.
  • Ti-6Al-4V alloy is used as a material, an oxygen concentration decreases from 0.12 mass% to 0.028 mass% and an oxygen concentration decreases from 1.6 mass% to 0.3 mass%.
  • Non-Patent Literature 2 describes that oxygen can be reduced by plasma arc melting of a pure titanium under an Ar atmosphere containing 20 vol% of H 2 .
  • Non-Patent Literature 2 describes that oxygen concentration decreases from initial oxygen concentration of 0.23 mass% to 0.09 mass%.
  • Non-Patent Literature 1 describes that an ICP analysis method is used as an oxygen analysis method. However, there is no suggestion about specific experimental conditions on which the data was obtained. Typically in the ICP analysis method, it is difficult to precisely analyze oxygen concentration in a sample due to existence of oxygen atoms contained in water molecules used for producing a solution for quantitative analysis.
  • Non-Patent Literature 2 also shows a graph illustrating a change with time of oxygen concentration in a sample. Considering the inclination of the illustrated graph, it is difficult to expect further effect of reducing oxygen.
  • An object of the present invention is to provide a method for refining a titanium material in which contained oxygen and further hydrogen can be surely removed from a titanium material made of a pure titanium, a titanium alloy or an intermetallic compound containing titanium as one of main components.
  • the method for refining a titanium material according to the present invention preferably further includes a heat treatment step of retaining the titanium material for 15 minutes or more under the condition of a degree of vacuum of 1 ⁇ 10 -2 to 1 ⁇ 10 -4 Pa and a retention temperature of 600 to 1,200°C after termination of the second melting step, thereby removing hydrogen from the titanium material.
  • contained oxygen and further hydrogen can be removed from a titanium material made of a pure titanium, a titanium alloy or an intermetallic compound containing titanium as one of main components.
  • the present inventors conducted earnest investigations in order to find out a method for refining a titanium material in which light elements or particularly oxygen contained in a titanium material containing, as its main component, titanium, which is very likely to be combined with light elements such as oxygen, nitrogen, etc., can be surely removed from the titanium material.
  • oxygen contained in the titanium material can be surely removed by performing a first melting step of melting the titanium material under a noble gas atmosphere containing a certain amount of hydrogen so as to introduce hydrogen, and successively a second melting step of melting the titanium material under a noble gas atmosphere so as to remove contained oxygen from the titanium material together with the hydrogen introduced in the first step.
  • the hydrogen introduced into the titanium material in order to remove the contained oxygen can be surely removed by performing a heat treatment step of retaining the titanium material under a certain condition after the second melting step. It is considered that in a case where the heat treatment step is carried out, the hydrogen that cannot be quite removed in the second melting step can be surely removed.
  • the reason why the oxygen contained in the titanium material can be removed from the titanium material together with the hydrogen introduced in the first melting step is because the introduced hydrogen functions as a deoxidizer.
  • the titanium material used in the method for refining a titanium material of the present invention contains any one of a pure titanium, a titanium alloy, and an intermetallic compound of titanium (an intermetallic compound containing titanium as one of main components).
  • the pure titanium include commercially pure titanium of JIS titanium 1, JIS titanium 2, JIS titanium 3, and JIS titanium 4.
  • alloy elements contained in the titanium alloy include Al, V, Mo, Cr, Zr, Sn, Si, Cu, Nb, Fe, Ni, Ta, Ag, Pd, C, and N.
  • Examples of the intermetallic compound include TiAl and NiTi.
  • the titanium content of the titanium material is 45 mass% or higher.
  • the lower limit of the titanium content of a typical titanium material is such a degree. If the titanium content of a material is too low, the material cannot be regarded as a titanium material.
  • the method for refining titanium of the present invention includes at least a first melting step and a second melting step. Each of the first melting step and the second melting step is carried out once to several times. In addition, a heat treatment step may be carried out after termination of the second melting step. The refining method will be separated into the first melting step, the second melting step and the heat treatment step below, and each of the steps will be described in detail.
  • the first melting step is a step for introducing hydrogen into the titanium material.
  • the first melting step is a pretreatment step for removing oxygen from the titanium material.
  • the techniques shown in previously-described Non-Patent Literature 1 and Non-Patent Literature 2 suggest that oxygen can be reduced in a case where a step corresponding to the first melting step is carried out.
  • oxygen cannot be removed from the titanium material only by the first melting step.
  • oxygen cannot be removed satisfactorily from the titanium material only by performing the first melting step.
  • the titanium material is melted under a noble gas atmosphere containing 5 to 70 vol% of hydrogen, for example, by use of a plasma arc melting furnace, thereby introducing hydrogen into a melt of the titanium material.
  • the melting in the first melting step is preferably performed by plasma arc melting.
  • the titanium material is melted by plasma arc melting
  • heating and hydrogen introduction can be attained concurrently as long as hydrogen is mixed into plasma gas.
  • an apparatus or the like for introducing hydrogen gas must be prepared separately from a heat source, and thus the manufacturing cost increases.
  • the reason why the noble gas atmosphere containing 5 to 70 vol% (5 vol% or higher and 70 vol% or lower) of hydrogen is used as the atmosphere in the first melting step is as follows. If the hydrogen concentration exceeds 70 vol% particularly in the case of the plasma arc melting, energy necessary for ionization increases, and arc extinguishing often occurs due to increase in voltage, so that a plasma arc is hardly generated. On the other hand, if the hydrogen concentration is less than 5 vol%, sufficient hydrogen cannot be introduced into the melt of the titanium material.
  • the lower limit of the hydrogen content may be preferably 10 vol% or higher, and more preferably 15 vol% or higher.
  • the upper limit of the hydrogen content may be preferably 60 vol% or lower, and more preferably 50 vol% or lower.
  • the noble gas atmosphere containing 5 to 70 vol% of hydrogen is used as the atmosphere in the first melting step
  • an Ar atmosphere can be used as the insert gas atmosphere by way of example. Further, deoxidation can be attained in principle even when the atmosphere in the first melting step is an He atmosphere, an Ne atmosphere, or the like.
  • the amount of heat inputted in the first melting step is not particularly stipulated in the present invention, it is preferably set within a range of 15 to 200 kW/kg (15 kW/kg or more and 200 kW/kg or less). If the inputted amount of heat is less than 15 kW/kg, necessary amount of heat for melting titanium cannot be secured. On the other hand, if the inputted amount of heat exceeds 200 kW/kg, a volatilization loss of titanium occurs.
  • the melting retention time in the first melting step is set within a range of 0.3 to 3.6 ks (5 to 60 minutes).
  • the lower limit of the melting retention time is more preferably set at 0.6 ks (10 minutes), and the upper limit thereof is more preferably 1.8 ks (30 minutes). If the melting retention time is less than 0.3 ks (5 minutes), sufficient hydrogen for deoxidation cannot be introduced. On the other hand, if the melting retention time exceeds 3.6 ks (60 minutes), both the heat loss and the volatilization loss of titanium merely increase.
  • the first melting step is typically carried out only once. However, the first melting step may be carried out again after the second melting step is carried out. Further, the first melting step may be carried out successively and repeatedly two or more times. Whether the first melting step is carried out once or a plurality of times may be determined based on a criterion that the oxygen concentration has been reduced to 80% or lower in comparison with that before the treatment.
  • the second melting step is a step of removing oxygen contained in the titanium material from the melt of the titanium material together with the hydrogen introduced into the titanium material in the first melting step.
  • the melting in the first melting step is preferably carried out by plasma arc melting.
  • the melting in the second melting step is also preferably carried out by plasma arc melting.
  • the temperature of the melt in a case where the titanium material is melted by plasma arc melting, the temperature of the melt can be increased to be higher than by another process. In a case of melting other than the plasma arc melting, it is expected that the deoxidation efficiency is slightly lowered due to a temperature fall.
  • a noble gas atmosphere of Ar, He, Ne or the like is used as the atmosphere in the second melting step.
  • the atmosphere in the first melting step is set as the Ar atmosphere containing 5 to 70 vol% of hydrogen
  • an Ar atmosphere being the same kind of noble gas as in the first melting step is preferably used in the second melting step, in view of efficiency.
  • another noble gas such as He, Ne or the like may be used as the atmosphere in the second melting step, in the same manner as in the first melting step.
  • the oxygen contained in the titanium material can be surely removed from the melt of the titanium material together with the hydrogen introduced into the titanium material in the first melting step.
  • the atmosphere is set as the noble gas atmosphere not containing hydrogen, an extremely small amount of lower than 5 vol% of hydrogen may be contained as long as it gives no influence to the removal of hydrogen and oxygen from the melt of the titanium material.
  • the amount of heat inputted in the second melting step is preferably set within a range of 15 to 200 kW/kg in the same manner as in the first melting step. If the inputted amount of heat is less than 15 kW/kg, necessary amount of heat for melting titanium cannot be secured. On the other hand, if the inputted amount of heat exceeds 200 kW/kg, a volatilization loss of titanium occurs.
  • the melting retention time in the second melting step is set within a range of 0.3 to 3.6 ks (5 to 60 minutes) in the same manner as the melting retention time in the first melting step.
  • the lower limit of the melting retention time is more preferably set at 0.6 ks (10 minutes), and the upper limit thereof is more preferably set at 1.8 ks (30 minutes). If the melting retention time is less than 0.3 ks (5 minutes), sufficient time for deoxidation cannot be secured. On the other hand, if the melting retention time exceeds 3.6 ks (60 minutes), both the heat loss and the volatilization loss of titanium merely increase.
  • the second melting step is typically carried out only once in the same manner as the first melting step. However, the second melting step may be carried out a plurality of times in the same manner as the first melting step. In a case where the second melting step is carried out a plurality of times, a combination of the first melting step and the second melting step may be regarded as one set and performed a plurality of times, or only the second melting step may be carried out a plurality of times after termination of the first melting step. Whether the second melting step is carried out only once or a plurality of times may be determined based on a criterion that the hydrogen concentration has been reduced to 5.0 ⁇ 10 -2 mass% or lower.
  • the heat treatment step is carried out after termination of the second melting step.
  • the titanium material is retained for 0.9 ks (15 minutes) or more under the condition of a degree of vacuum of 1 ⁇ 10 -2 to 1 ⁇ 10 -4 Pa and a retention temperature of 600 to 1,200°C.
  • the heat treatment step does not have to be always carried out. However, in a case where the heat treatment step is carried out, the hydrogen which cannot be quite removed in the second melting step can be surely removed.
  • the heat treatment step is carried out by use of a vacuum heat treatment furnace or the like.
  • the degree of vacuum is set within a range of 1 ⁇ 10 -2 to 1 ⁇ 10 -4 Pa.
  • the reason why the upper limit of the degree of vacuum is set at 1 ⁇ 10 -4 Pa is because a degree of vacuum exceeding 1 ⁇ 10 -4 Pa is preferable only for the sake of dehydrogenation but it is inefficient to take a long time to exhaust the gas to the aforementioned degree of vacuum.
  • the reason why the lower limit of the degree of vacuum is set at 1 ⁇ 10 -2 Pa is because in a case of a degree of vacuum less than 1 ⁇ 10 -2 Pa, an oxide film is formed in the titanium surface and the removal of hydrogen is impeded by the oxide film.
  • the retention temperature in the heat treatment step is set at 600 to 1,200°C.
  • the reason why the lower limit of the retention temperature is set at 600°C is because if the retention temperature is lower than 600°C, the diffusion rate of hydrogen in the solid titanium material becomes so low that it takes a long time to remove hydrogen, which is inefficient.
  • the reason why the upper limit of the retention temperature is set at 1,200°C is because, if the retention temperature is higher than 1,200°C, the formation of an oxide film in the titanium surface becomes active and the time required for cooling increases.
  • the retention time in the heat treatment step is set at 0.9 ks (15 minutes) or more. If the retention time is less than 0.9 ks (15 minutes), it is highly likely that the hydrogen which cannot be quite removed from the titanium material in the second melting step cannot be removed. In a case where the retention time is set at 0.9 ks (15 minutes) or more, the hydrogen which cannot be quite removed from the titanium material in the second melting step can be surely removed.
  • the hydrogen can be removed from the titanium material more surely. However, it is considered that substantially all the hydrogen in the titanium material can be removed in the retention time of about 3.6 ks (60 minutes).
  • a titanium material commercially pure titanium: melting material made of CP titanium
  • the first melting step and the second melting step in a plasma arc melting furnace and the heat treatment step in a vacuum heat treatment furnace were carried out sequentially in accordance with testing conditions.
  • a hearth used for melting the titanium material was shaped into a semisphere having a diameter of 80 mm.
  • the titanium melt mass (sample mass) being 250 g
  • the titanium material was put onto the hearth so as to reach a height of about 25 mm.
  • a titanium melt mass (sample mass) being 500 g
  • the titanium material was put onto the hearth so as to reach a height of about 40 mm.
  • the melting power of a plasma arc in the first melting step was set at 70 V and 500 A
  • the melting power in the second melting step was set at 50 V and 450 A.
  • the melting time was set within a range of 0.3 to 3.6 ks (5 to 60 minutes), and the flow rate was set at 30 L/min.
  • the melting time was set within a range of 0.3 to 3.6 ks (5 to 60 minutes), and the flow rate was set at 20 L/min.
  • the amount of heat inputted in the first melting step and the second melting step was 114 kW/kg, and the furnace pressure was 1 atm.
  • an Ar atmosphere in which 30 vol% of hydrogen had been mixed was used as the atmosphere in the first melting step.
  • an Ar atmosphere (pure Ar atmosphere) in which no hydrogen had been mixed was used.
  • a sample having been subjected to the melting steps was placed on an Al 2 O 3 boat on which a Ti sheet was laid, and evacuated to 7.0 ⁇ 10 -3 Pa by a vacuum pump. After that, the temperature was increased to 1,023 K (750°C) while the vacuum state (7.0 ⁇ 10 -3 Pa) was retained, and then retained for a retention time of 3.6 ks (60 minutes).
  • Example 1 Item Sample mass [g] First melting step Second melting step Heat treatment step Oxygen density [mass%] Hydrogen density [mass%] Note time [min] times time [min] times yes/no before treatment after treatment after treatment Comp.
  • Example 1 250 15 1 - - - 0.105 0.254 6.80 ⁇ 10 -1 Comp.
  • Example 2 250 15 1 - - yes 0.105 0.107 1.89 ⁇ 10 -3 Comp.
  • Example 3 250 15 2 - - yes 0.105 0.099 2.24 ⁇ 10 -3 Comp.
  • Example 4 250 30 1 - - - - 1.57 1.55 4.93 ⁇ 10 -1 Comp.
  • Example 5 250 30 1 - - yes 1.57 1.48 2.09 ⁇ 10 -3
  • Example 1 250 30 1 20 1 - 0.105 0.049 1.07 ⁇ 10 -2
  • Example 2 250 30 1 20 1 yes 0.105 0.059 1.84 ⁇ 10 -3
  • Example 3 250 5 1 20 1 - 0.105 0.049 8.25 ⁇ 10 -3
  • Example 4 250 15 1 20 1 - 0.105 0.061 1.01 ⁇ 10 -2
  • Example 5 250 15 2 20 1 - 0.105 0.057 1.27 ⁇ 10 -2 sample reversed
  • Example 6 250 15 2 20 1 yes 0.105 0.045 7.80 ⁇ 10 -4 sample reversed
  • Example 7 250 30 1 20 1 - 0.105 0.021 9.28 ⁇ 10 -3 cooled gradually
  • Example 8 250 30 2 20 2 - 0.105 0.040 7.89 ⁇ 10 -3 sample reversed
  • Example 9 250 30 2 20 2 yes 0.105 0.043 2.16 ⁇ 10 -3 sample reversed
  • Example 10 250 5 3 10 3 - 0.105 0.077 3.52 ⁇ 10 -2
  • Example 5 the sample was reversed between the first melting steps performed twice such that the first melting step, sample reversing, the first melting step ... were performed sequentially.
  • Example 8 the sample was reversed at the time of repeating of the series of steps such that the first melting step, the second melting step, sample reversing, the first melting step ... were performed sequentially.
  • Example 7 The gradually cooling in Example 7 was carried out by decreasing a current value from 450 A at a rate of 50 A per 20 seconds in the second melting step, and turning off the plasma as soon as the current value reached 50 A.
  • the hydrogen introduced into the titanium material in the first melting step functions as a deoxidizer in the second melting step such that oxygen contained in the titanium material is removed from the titanium material together with the hydrogen.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
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Claims (2)

  1. Procédé de raffinage d'une matière de titane, dans lequel l'oxygène contenu dans une matière de titane constituée de titane pur, d'un alliage de titane ou d'un composé intermétallique contenant du titane comme un des composants principaux est éliminé, la teneur en titane de la matière de titane faisant 45% en masse ou plus, le procédé comprenant:
    un première étape de fusion où l'on fait entrer en fusion la matière de titane sous atmosphère de gaz noble contenant de 5 à 70% en volume d'hydrogène, introduisant ainsi de l'hydrogène dans une fusion de la matière de titane; et
    une deuxième étape de fusion où l'on fait entrer en fusion la matière de titane dans laquelle de l'hydrogène a été introduit à la première étape de fusion sous atmosphère de gaz noble contenant moins de 5% en volume d'hydrogène, éliminant de ce fait l'oxygène contenu dans la matière de titane de la fusion de la matière de titane avec l'hydrogène,
    dans lequel la durée de rétention de la fusion dans la première et la deuxième étape de fusion est réglée dans l'intervalle entre 0,3 et 3,6 ks, et
    dans lequel chacune de la première étape de fusion et de la deuxième étape de fusion est réalisée au moins une fois.
  2. Procédé de raffinage d'une matière de titane selon la revendication 1, comprenant en outre une étape de traitement thermique où l'on retient la matière de titane pendant 15 minutes ou plus sous la condition d'un degré de vide de 1×10-2 à 1×10-4 Pa et d'une température de rétention allant de 600 à 1200°C à la fin de la deuxième étape de fusion, éliminant ainsi l'hydrogène de la matière de titane.
EP18874635.8A 2017-10-31 2018-10-29 Procédé de purification de matériau à base de titane Active EP3705588B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2017210129A JP6816339B2 (ja) 2017-10-31 2017-10-31 チタン素材の脱酸方法
PCT/JP2018/040049 WO2019088007A1 (fr) 2017-10-31 2018-10-29 Procédé de purification de matériau à base de titane

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EP3705588A1 EP3705588A1 (fr) 2020-09-09
EP3705588A4 EP3705588A4 (fr) 2021-03-10
EP3705588B1 true EP3705588B1 (fr) 2023-05-31

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US (1) US20200239979A1 (fr)
EP (1) EP3705588B1 (fr)
JP (1) JP6816339B2 (fr)
CN (1) CN111279000B (fr)
RU (1) RU2738280C1 (fr)
WO (1) WO2019088007A1 (fr)

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KR101435481B1 (ko) * 2014-02-12 2014-08-28 한국지질자원연구원 Ｔｉ―Ｍｏ 합금 스크랩을 이용한 3원계 티타늄 합금 분말의 제조방법
CN104694705B (zh) * 2015-02-06 2016-08-31 中南大学 一种深度脱氧装置及其应用
CN105779699B (zh) * 2016-03-28 2019-01-11 上海大学 利用溶解气体上浮法去除金属夹杂物的方法及增压真空感应炉精炼装置
JP6281598B2 (ja) 2016-05-26 2018-02-21 横浜ゴム株式会社 空気入りタイヤ

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CN111279000A (zh) 2020-06-12
EP3705588A1 (fr) 2020-09-09
EP3705588A4 (fr) 2021-03-10
JP2019081926A (ja) 2019-05-30
CN111279000B (zh) 2022-02-25

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