WO2015105024A1 - チタン粉末材料、チタン素材及び酸素固溶チタン粉末材料の製造方法 - Google Patents
チタン粉末材料、チタン素材及び酸素固溶チタン粉末材料の製造方法 Download PDFInfo
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/80—After-treatment
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- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
- B22F2301/205—Titanium, zirconium or hafnium
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- B22F2302/25—Oxide
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- the present invention relates to a titanium powder material and a titanium material, and more particularly to a high-strength titanium powder material in which oxygen is dissolved, a titanium material, and a method for producing them.
- Titanium is a lightweight material with a specific gravity about half that of steel, and has excellent corrosion resistance and strength. Therefore, titanium, parts for aircraft, railway vehicles, motorcycles, automobiles, It is used for household appliances and building materials. It is also used as a medical material from the viewpoint of excellent corrosion resistance.
- titanium is used for a limited purpose because of its high material cost compared to steel materials and aluminum alloys.
- a titanium alloy has a high tensile strength exceeding 1000 MPa, but has a problem that ductility (breaking elongation) is not sufficient and plastic workability at room temperature or low temperature is poor.
- pure titanium has a high elongation at break exceeding 25% at room temperature and is excellent in plastic workability in a low temperature range, but has a low tensile strength of about 400 to 600 MPa. is there.
- Patent Document 1 proposes the following steps as a method for obtaining an oxygen solid solution titanium material.
- a step of preparing titanium powder and TiO 2 particles A step of adjusting the added amount of TiO 2 particles to 0.5% to 3.0% on a mass basis with respect to the entire mixed powder and mixing the titanium powder and TiO 2 particles.
- C Step of sintering the above mixture in a temperature range from 700 ° C. to less than the melting point of TiO 2 in a vacuum atmosphere to thermally decompose the TiO 2 particles, and dissociating the dissociated oxygen atoms in titanium. .
- the titanium material produced by the method disclosed in JP2012-241241, that is, the powder metallurgy method using TiO 2 particles, can maintain high strength and high ductility as compared with the melt-processed material. is there.
- the TiO 2 particles have a small particle size, it is easy to make an aggregate. Specifically, when the amount of TiO 2 particles added is increased, aggregates of TiO 2 particles are formed, and the decomposition of TiO 2 does not proceed completely, and the remaining TiO 2 particles start from breaking. As a result, ductility is reduced.
- An object of the present invention is to provide a method for producing an oxygen solid solution titanium powder material capable of dissolving a large amount of oxygen in the titanium powder material while maintaining proper ductility.
- Another object of the present invention is to provide a titanium powder material and a titanium material in which a large amount of oxygen is dissolved while maintaining proper ductility.
- the manufacturing method of the oxygen solid solution titanium powder material according to the present invention includes the following steps.
- B) The titanium powder material having the titanium oxide film is heated in an oxygen-free atmosphere to decompose the titanium oxide film formed on the surface of each titanium powder particle, and the dissociated oxygen atoms are A step of dissolving in a matrix of titanium powder particles.
- the amount of oxygen solid solution in the matrix of each titanium powder particle is increased by performing a plurality of cycles with the formation of the titanium oxide film and the subsequent decomposition of the titanium oxide film as one cycle.
- the heating temperature for forming the titanium oxide film is preferably 160 ° C. or higher and lower than 600 ° C., and the heating temperature for decomposing the titanium oxide film is preferably 450 ° C. or higher and below the melting point.
- the heat treatment that contributes to the formation of the titanium oxide film and the decomposition of the titanium oxide film is preferably carried out by containing the titanium powder material in a rotary kiln heating furnace.
- each titanium powder particle has an oxide film formed naturally in the atmosphere on the surface, and the amount of oxygen dissolved in the matrix of each titanium powder particle is greater than the amount of oxygen in the naturally formed oxide film. There are also many.
- the oxygen content of each titanium powder particle is preferably 0.4% to 4.7%, more preferably 1.15 to 1.9% on a mass basis.
- the titanium powder particles constituting the titanium powder material are made of pure titanium, and the average value of the micro Vickers hardness of the matrix of the titanium powder particles is 200 to 600.
- a titanium material molded into a predetermined shape using the oxygen solid solution titanium powder material described above is also an object of the present invention.
- the titanium material is a pure Ti powder extruded material, the oxygen content with respect to the whole extruded material is 1.2% by mass or more, and the elongation at break is 18% or more.
- FIG. 1 is a diagram schematically showing the features of the present invention. First, the outline of the invention will be described with reference to FIG. 1, and more detailed data will be described thereafter.
- titanium powder material A titanium powder material consisting of a large number of titanium powder particles is prepared.
- titanium powder particles may be either pure titanium powder particles or titanium alloy powder particles.
- Each titanium powder particle has an oxide film (natural oxide film) formed naturally in the atmosphere on the surface, but is a very thin film, and therefore the natural oxide film is not shown in FIG.
- the natural oxide film has a thickness of about 0.1 to 1 ⁇ m.
- the prepared titanium powder material is heated in an atmosphere containing oxygen to form a titanium oxide film on the surface of each titanium powder particle.
- the heat treatment that contributes to the formation of the titanium oxide film is preferably carried out by containing the titanium powder material in a rotary kiln heating furnace.
- the heating conditions are, for example, as follows.
- Heating atmosphere 10 vol. % O 2 -90 vol. % Ar mixed gas Mixed gas flow rate: 1 L / min. Heating temperature: 200 ° C Holding time: 30 min. Rotational speed: 20 rpm.
- the titanium oxide film is formed on the surface of each titanium powder particle by the above oxidation heat treatment.
- the reason why the rotary kiln heating furnace is used is to prevent titanium powder particles from being pre-sintered into a lump during oxidation heat treatment by applying rotation or vibration to the titanium powder material.
- the reason why argon gas is included is to prevent abnormal heat generation of the titanium powder material due to excessive oxygen.
- Titanium powder material having a titanium oxide film on its surface is heated in an oxygen-free atmosphere to decompose the titanium oxide film formed on the surface of each titanium powder particle, and the dissociated oxygen atoms are separated from each titanium powder. Solid solution in the matrix of particles.
- the heat treatment that contributes to the decomposition of the titanium oxide film is preferably carried out by accommodating the titanium powder material in a rotary kiln heating furnace.
- the oxidation heat treatment and solution heat treatment described above may be performed using the same rotary kiln heating furnace.
- the heating conditions are, for example, as follows.
- Heating atmosphere 100 vol. % Ar gas Gas flow rate: 1 L / min. Heating temperature: 600 ° C Holding time: 30 min. Or 60 min. Rotational speed: 20 rpm.
- the oxygen solution generated by the decomposition of the titanium oxide film is uniformly diffused into the matrix of each titanium powder particle by the above solution heat treatment and is dissolved. In this way, the target oxygen solid solution titanium powder material can be obtained.
- the oxygen-dissolved titanium powder material obtained as described above When the oxygen-dissolved titanium powder material obtained as described above is placed in the atmosphere, a natural oxide film is formed on the surface of each titanium powder particle.
- the amount of oxygen in the natural oxide film is at most about 0.2% by mass with respect to the entire titanium powder particles.
- the oxidation heat treatment and the solution heat treatment are performed by the method of the present invention, the amount of oxygen dissolved in the matrix of each titanium powder particle becomes larger than the amount of oxygen in the natural oxide film.
- FIG. 2 is a graph showing changes in the diffraction peak of Ti when pure titanium raw material powder is subjected to oxidation heat treatment and solution heat treatment.
- the Ti diffraction peak shifts to the low angle side, and when the solution heat treatment is further performed, the Ti diffraction peak significantly decreases to the low angle side. It is recognized that there is a shift.
- These peak shifts indicate that oxygen atoms were dissolved in the Ti substrate (matrix).
- a large amount of oxygen atoms contribute to the formation of the titanium oxide film, and a few oxygen atoms are dissolved in the Ti substrate. It can be seen that during the solution heat treatment, the titanium oxide film is decomposed and a large amount of oxygen atoms are dissolved in the Ti substrate.
- FIG. 3 is a diagram showing a change in the diffraction peak of TiO 2 when an oxidation heat treatment and a solution heat treatment are performed on a pure titanium raw material powder.
- a slight diffraction peak of TiO 2 is detected in the pure titanium raw material powder. This is because the pure titanium raw material powder has an oxide film (natural oxide film) formed naturally in the atmosphere. Since the titanium oxide film is formed on the powder particle surface during the oxidation heat treatment, the peak intensity of TiO 2 is high.
- the solution heat treatment it is recognized that the titanium oxide film is thermally decomposed and oxygen atoms are dissolved in the Ti base material, so that the TiO 2 peak disappears.
- Oxidative heat treatment heating atmosphere 10% O 2 + 90% Ar mixed gas (flow rate: 1 L / min.) Heating temperature: 200 ° C Holding time: 30 min. Rotational speed: 20 rpm. Solution heat treatment heating atmosphere: 100% Ar gas (flow rate: 1 L / min.) Heating temperature: 600 ° C Holding time: 30 min. Rotational speed: 20 rpm.
- the measurement results are shown in Table 1 and FIG.
- the column of the number of repetitions 0 is the oxygen amount and nitrogen amount of the pure titanium powder before the heat treatment. Oxygen is mainly contained in the natural oxide film.
- the oxygen content increases linearly in proportion to the number of repetitions of the above cycle, while the nitrogen content remains constant without change.
- the oxygen content of the titanium powder particles is increased to nearly 4.7%.
- the pure titanium raw material powder was subjected to an oxidation heat treatment, and further subjected to a solution heat treatment to measure how the micro Vickers hardness (Hv) changes.
- the measured sample was subjected to one cycle of oxidation heat treatment and solution heat treatment, and the oxygen content after the solution heat treatment was 1.18% by mass.
- the oxygen content in the Ti powder increases by increasing the number of cycles of oxidation / solution heat treatment.
- an extremely hard Ti powder having a substrate hardness exceeding 600 Hv requires high pressure when compression molding it, and at the same time, the powder becomes brittle and cracks are generated inside the powder molded body. A molded product cannot be obtained.
- the hardness of the pure Ti powder subjected to the oxidation / solution heat treatment according to the present invention is 200 to 600 Hv.
- Example 1 Pure Ti powder (average particle size: 28 ⁇ m, purity> 95%) is used as a starting material, and the oxidation heat treatment and solution heat treatment shown below are set as one cycle, and this is repeated up to 4 times to produce oxygen solid solution pure Ti powder. did.
- Oxidation heat treatment atmosphere 10% O 2 + 90% Ar mixed gas Temperature: 200 ° C. Holding time: 15 minutes Number of rotations: 20 rpm. Solution heat treatment atmosphere: 100% Ar gas Temperature: 600 ° C. Holding time: 30 minutes Number of rotations: 20 rpm.
- the oxygen content of each extruded material was analyzed and a tensile test was performed at room temperature to measure the tensile strength, proof stress, and elongation at break, and the dependency on the oxygen content was investigated.
- Table 3 shows the measurement results.
- FIG. 6 shows the comparison of tensile strength
- FIG. 7 shows the comparison of proof stress.
- the production method (direct oxidation solution heat treatment) according to the present invention, as the oxygen content increases, the tensile strength (UTS) and the yield strength (YS) both increase almost linearly, while the breaking elongation ( ⁇ ). However, it exhibited a sufficiently good ductility of 18.1% at an oxygen content of 1.66% by mass.
- a sample having an oxygen content of 0.21% by mass is an extruded material composed of pure titanium powder particles in which oxygen is not solid-solved, and is in the natural oxide film formed on the surface of each particle. It means that the amount of oxygen is about 0.21% by mass.
- the oxygen content of the sample subjected to the direct oxidation solution heat treatment is 0.42% or more.
- the material having an oxygen content of 1.24% by mass in the pure Ti powder extruded material by direct oxidation solution heat treatment and the oxygen content of 1.23% by mass in the pure Ti powder extruded material by adding TiO 2 particles The fracture starting point of the fracture surface after the tensile test with the material was observed with a scanning electron microscope (SEM). A photomicrograph is shown in FIG.
- fine dimples are confirmed and a uniform ductile fracture surface is exhibited.
- the material produced by the TiO 2 particle addition the presence of TiO 2 particles unreacted was observed at the origin of the fracture. That is, since the TiO 2 particles aggregated in the state of the Ti + TiO 2 mixed powder, unreacted TiO 2 became the starting point of fracture, and as a result, the elongation at break was significantly reduced.
- Example 2 The effect of heating temperature during oxidative heat treatment was investigated. Using the same pure Ti powder as before, 50 g of Ti powder was heated to a rotary kiln-type heat treatment furnace with oxygen + argon mixed gas (10% O 2 + 90% Ar / flow rate: 1 L / min.) Flowing at a heating temperature of 100 Ti powder was produced by changing the temperature to ⁇ 700 ° C. Note that the holding time at each temperature in the oxidation heat treatment is 1 hr, and the rotational speed is 20 rpm. It was.
- the temperature range suitable for the oxidation heat treatment of the Ti powder is 160 ° C. or more, and the oxidation heat treatment at less than 600 ° C. is effective for suppressing the partial melting of the Ti powder.
- Example 3 The influence of heating temperature during solution heat treatment was investigated.
- the oxidation heat treatment under the following conditions was performed on the pure Ti powder as before.
- Heating atmosphere 10% O 2 + 90% Ar mixed gas (flow rate: 1 L / min.) Heating temperature: 200 ° C Holding time: 30 min. Rotational speed: 20 rpm.
- the heating temperature was changed in the range of 300 to 800 ° C. in an argon gas atmosphere to produce Ti powder.
- the holding time at each temperature in the solution heat treatment was 1 hr, the argon gas flow rate: 1 L / min, and the rotation speed: 20 rpm.
- the weight of Ti powder to be charged into the heating furnace at one time was set to two conditions of 30 g and 150 g, and the influence of the input amount during the heat treatment was also investigated.
- heat treatment at 450 ° C. or higher is required to thermally decompose the oxide film TiO 2 formed by oxidation heat treatment and to dissolve oxygen atoms in the Ti substrate.
- a higher temperature of 550 ° C. or higher is desirable to stably and uniformly dissolve oxygen atoms completely.
- the present invention can be advantageously used to obtain a high-strength titanium powder material and a titanium material in which a large amount of oxygen is dissolved while maintaining proper ductility.
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Abstract
Description
(a)チタン粉末とTiO2粒子とを準備する工程。
(b)混合粉末全体に対してTiO2粒子の添加量が質量基準で0.5%~3.0%となるように調整してチタン粉末とTiO2粒子とを混合する工程。
(c)上記の混合物を、700℃からTiO2の融点未満の温度範囲で、かつ真空雰囲気中で焼結してTiO2粒子を熱分解させ、解離した酸素原子をチタン中に固溶させる工程。
(a)チタン粉末粒子からなるチタン粉末材料を、酸素を含む雰囲気中で加熱して上記チタン粉末粒子の表面にチタン酸化皮膜を形成する工程。
(b)上記チタン酸化皮膜を有するチタン粉末材料を、酸素を含まない雰囲気中で加熱して各チタン粉末粒子の表面に形成されたチタン酸化皮膜を分解し、その際に解離した酸素原子を各チタン粉末粒子のマトリクス中に固溶させる工程。
上記の特徴的な構成の作用効果または技術的意義については、以下の項目で説明する。
多数のチタン粉末粒子からなるチタン粉末材料を準備する。ここで「チタン粉末粒子」とは、純チタン粉末粒子またチタン合金粉末粒子のいずれであってもよい。各チタン粉末粒子は、大気中で自然に形成された酸化膜(自然酸化膜)を表面に有しているが、非常に薄い膜であるので、図1では自然酸化膜を図示していない。自然酸化膜の厚みは、0.1~1μm程度である。
準備したチタン粉末材料を、酸素を含む雰囲気中で加熱して各チタン粉末粒子の表面にチタン酸化皮膜を形成する。チタン酸化皮膜の形成に資する熱処理は、好ましくは、チタン粉末材料をロータリーキルン式加熱炉内に収容して行う。加熱条件は、例えば、以下の通りである。
混合ガス流量:1L/min.
加熱温度:200℃
保持時間:30min.
回転数:20rpm.
表面にチタン酸化皮膜を有するチタン粉末材料を、酸素を含まない雰囲気中で加熱して各チタン粉末粒子の表面に形成されたチタン酸化皮膜を分解し、その際に解離した酸素原子を各チタン粉末粒子のマトリクス中に固溶させる。チタン酸化皮膜の分解に資する熱処理は、好ましくは、チタン粉末材料をロータリーキルン式加熱炉内に収容して行う。前述した酸化熱処理および固溶化熱処理を同一のロータリーキルン式加熱炉を用いて行ってもよい。加熱条件は、例えば、以下の通りである。
ガス流量:1L/min.
加熱温度:600℃
保持時間:30min.または60min.
回転数:20rpm.
酸化熱処理の時間を増大しても酸素固溶量は増加しない。その理由は、チタン粉末粒子表面に形成されるチタン酸化皮膜がバリアとなり、更なる酸化反応が進行しないからである。チタン粉末粒子のマトリクス中に固溶する酸素の量を増加するには、酸化熱処理時間を増やすのではなく、チタン酸化皮膜形成のための酸化熱処理、および引き続いてのチタン酸化皮膜分解のための固溶化熱処理を1サイクルとして複数回のサイクルを行うことが望ましい。
図2は、純チタン原料粉末に対して酸化熱処理および固溶化熱処理を行った場合のTiの回折ピークの変化を示す図である。図2から明らかなように、純チタン原料粉末に対して酸化熱処理を行うとTiの回折ピークが低角度側にシフトし、さらに固溶化熱処理を行うとTiの回折ピークが顕著に低角度側にシフトしていることが認められる。これらのピークのシフトは、Tiの素地(マトリクス)中に酸素原子が固溶したことを示すものである。酸化熱処理時には、多量の酸素原子がチタン酸化皮膜の形成に寄与し、僅かの酸素原子がTiの素地中に固溶する。固溶化熱処理時には、チタン酸化皮膜が分解し、多量の酸素原子がTiの素地中に固溶していることがわかる。
下記の条件の酸化熱処理および固溶化熱処理を1サイクルとし、このサイクルを4回繰り返して純チタン粉末中の酸素量および窒素量を測定した。使用した純チタン粉末は、平均粒子径が28μm、純度が95%を超えるものであった。
加熱雰囲気:10%O2+90%Ar混合ガス(流量:1L/min.)
加熱温度:200℃
保持時間:30min.
回転数:20rpm.
固溶化熱処理
加熱雰囲気:100%Arガス(流量:1L/min.)
加熱温度:600℃
保持時間:30min.
回転数:20rpm.
純チタン原料粉末に対して、酸化熱処理を行い、さらに固溶化熱処理を行って、マイクロビッカース硬さ(Hv)がどのように変化するかを測定した。測定した試料は、酸化熱処理および固溶化熱処理のサイクルを1回施したものであり、固溶化熱処理後の酸素含有量が1.18質量%になるものであった。
純Ti粉末(平均粒子径;28μm、純度>95%)を出発原料とし、下記に示す酸化熱処理および固溶化熱処理を1サイクルとし、これを最高4回まで繰り返して酸素固溶純Ti粉末を作製した。
雰囲気:10%O2+90%Ar混合ガス
温度:200℃
保持時間:15分
回転数:20rpm.
固溶化熱処理
雰囲気:100%Arガス
温度:600℃
保持時間:30分
回転数:20rpm.
酸化熱処理時の加熱温度の影響を調査した。これまでと同様の純Ti粉末を用いて、ロータリーキルン式熱処理炉に酸素+アルゴン混合ガス(10%O2+90%Ar/流量;1L/min.)を流入した状態でTi粉末50gを加熱温度100~700℃に変化させてTi粉末を作製した。なお、酸化熱処理における各温度での保持時間はいずれも1hrとし、回転数を20rpm.とした。
固溶化熱処理時の加熱温度の影響を調査した。これまでと同様に純Ti粉末に対して、下記の条件の酸化熱処理を行った。
加熱温度:200℃
保持時間:30min.
回転数:20rpm.
Claims (10)
- チタン粉末粒子からなるチタン粉末材料を、酸素を含む雰囲気中で加熱して前記粉末粒子の表面にチタン酸化皮膜を形成する工程と、
前記チタン酸化皮膜を有する前記チタン粉末材料を、酸素を含まない雰囲気中で加熱して前記各チタン粉末粒子の表面に形成されたチタン酸化皮膜を分解し、その際に解離した酸素原子を前記各チタン粉末粒子のマトリクス中に固溶させる工程と、を備える、酸素固溶チタン粉末材料の製造方法。 - 前記チタン酸化皮膜の形成および引き続いての前記チタン酸化皮膜の分解を1サイクルとして複数回のサイクルを行うことによって、前記各チタン粉末粒子のマトリクス中への酸素固溶量を増加する、請求項1に記載の酸素固溶チタン粉末材料の製造方法。
- 前記チタン酸化皮膜を形成するための加熱温度は、160℃以上600℃未満であり、
前記チタン酸化皮膜を分解するための加熱温度は、450℃以上で融点以下である、請求項1または2に記載の酸素固溶チタン粉末材料の製造方法。 - 前記チタン酸化皮膜の形成およびチタン酸化皮膜の分解に資する熱処理は、前記チタン粉末材料をロータリーキルン式加熱炉内に収容して行う、請求項1~3のいずれかに記載の酸素固溶チタン粉末材料の製造方法。
- 請求項1~4のいずれかに記載の方法によって製造された酸素固溶チタン粉末材料であって、
前記各チタン粉末粒子は、大気中で自然に形成された酸化膜を表面に有しており、
前記各チタン粉末粒子のマトリクス中に固溶した酸素量は、前記自然形成酸化膜中の酸素量よりも多いことを特徴とする、酸素固溶チタン粉末材料。 - 前記各チタン粉末粒子の酸素含有量は、質量基準で、0.4%~4.7%である、請求項5に記載の酸素固溶チタン粉末材料。
- 前記各チタン粉末粒子の酸素含有量は、質量基準で、1.15~1.9%である、請求項6に記載の酸素固溶チタン粉末材料。
- 前記チタン粉末粒子は純チタンからなり、
前記チタン粉末粒子のマトリクスのマイクロビッカース硬さの平均値は、200~600である、請求項5~7のいずれかに記載の酸素固溶チタン粉末材料。 - 請求項5~8のいずれかに記載の酸素固溶チタン粉末材料を用いて所定の形状に成形したチタン素材。
- 当該チタン素材は純Ti粉末押出材であり、
押出材全体に対する酸素含有量が1.2質量%以上であり、
破断伸びが18%以上である、請求項9に記載のチタン素材。
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JP2018104778A (ja) * | 2016-12-27 | 2018-07-05 | 勝義 近藤 | 焼結刃物素材およびその製造方法 |
WO2022202740A1 (ja) * | 2021-03-26 | 2022-09-29 | 国立研究開発法人物質・材料研究機構 | 超臨界水利用装置用チタン合金 |
WO2024077526A1 (zh) * | 2022-10-12 | 2024-04-18 | 清华大学 | 纯钛制件及其制备方法 |
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Publication number | Publication date |
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EP3093085A4 (en) | 2017-09-20 |
JP6054553B2 (ja) | 2016-12-27 |
JPWO2015105024A1 (ja) | 2017-03-23 |
CN105899314B (zh) | 2017-12-15 |
EP3093085B1 (en) | 2022-04-27 |
EP3093085A1 (en) | 2016-11-16 |
CN105899314A (zh) | 2016-08-24 |
US20160332233A1 (en) | 2016-11-17 |
US10307824B2 (en) | 2019-06-04 |
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