WO2015111361A1 - 窒素固溶チタン粉末材料、チタン素材及び窒素固溶チタン粉末材料の製造方法 - Google Patents
窒素固溶チタン粉末材料、チタン素材及び窒素固溶チタン粉末材料の製造方法 Download PDFInfo
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- WO2015111361A1 WO2015111361A1 PCT/JP2014/084530 JP2014084530W WO2015111361A1 WO 2015111361 A1 WO2015111361 A1 WO 2015111361A1 JP 2014084530 W JP2014084530 W JP 2014084530W WO 2015111361 A1 WO2015111361 A1 WO 2015111361A1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- 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
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- 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
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- 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
- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- 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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
-
- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C8/06—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
- C23C8/24—Nitriding
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- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/02—Nitrogen
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- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
- B22F2301/205—Titanium, zirconium or hafnium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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 nitrogen 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.
- Non-Patent Document 1 entitled “Effect of Nitrogen on Tension Deformation Behavior and Deformation Structure of Titanium” It describes that nitrogen is used as an element. Specifically, it describes that Ti-N alloys having various nitrogen concentrations are prepared by weighing sponge titanium and TiN powder to a predetermined composition and arc melting. In this case, both high strength and high ductility can be achieved if nitrogen atoms are uniformly dissolved in the Ti matrix.
- the diffusion of nitrogen atoms is significant, so the nitrogen atoms are concentrated at the top of the molten metal, and as a result, uniform dispersion of nitrogen is difficult with a large ingot. As a result, the ductility is significantly reduced.
- An object of the present invention is to provide a method for producing a nitrogen solid solution titanium powder material capable of uniformly diffusing nitrogen atoms in a matrix of Ti powder particles to cause solid solution.
- Another object of the present invention is to provide a titanium powder material and a titanium material having both high strength and high ductility by uniformly diffusing nitrogen atoms into a matrix of Ti powder particles to cause solid solution.
- the method for producing a nitrogen solid solution titanium powder material according to the present invention is to heat a titanium powder material made of titanium powder particles in an atmosphere containing nitrogen so that nitrogen atoms are dissolved in a matrix of titanium powder particles.
- the heating temperature for dissolving the nitrogen atoms in the matrix of titanium powder particles is preferably 400 ° C. or higher and 800 ° C. or lower.
- the nitrogen content of each titanium powder particle is preferably 0.1% to 0.65% on a mass basis.
- the nitrogen contents of the four types of pure titanium specified by the Japanese Industrial Standard (JIS) are as follows.
- JIS H 4600 1 type 0.03 mass% or less
- JIS H 4600 2 type 0.03 mass% or less
- JIS H 4600 3 class 0.05 mass% or less
- JIS H 4600 4 class 0.05 mass% or less
- the titanium material is formed into a predetermined shape using the above nitrogen solid solution titanium powder material.
- the titanium material is a pure Ti powder extrudate, the nitrogen content relative to the entire extrudate is 0.1% to 0.65% on a mass basis, and the elongation at break is 10% or more. .
- a method of solidifying the nitrogen solid solution titanium powder material to form a titanium material for example, compacting / sintering, hot extrusion, hot rolling, thermal spraying, metal injection molding, powder additive manufacturing, etc. are used.
- 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.
- Titanium powder material consisting of titanium powder particles is heated and held in an atmosphere containing nitrogen, so that nitrogen atoms are uniformly diffused and dissolved in the matrix of each titanium powder particle. A nitrogen solid solution titanium powder material is obtained.
- the heating conditions are, for example, as follows. Heating atmosphere: 100 vol. % N 2 gas Gas flow rate: 5 L / min. Heating temperature: 400-600 ° C Retention time: 1 to 2 hr.
- the nitrogen atoms are uniformly diffused and dissolved in the matrix of each titanium powder particle.
- a tubular heating furnace non-rotating type
- a rotary rotary kiln furnace may be used.
- Table 1 The results in Table 1 are in good agreement with the results of the differential thermogravimetric analyzer (TG-DTA).
- TG-DTA differential thermogravimetric analyzer
- the heating temperature is set to 400 ° C. (673 K) or higher. It is desirable to do. However, when the heating temperature exceeds 800 ° C., Ti powders are partially sintered, so a heating temperature of 800 ° C. or less is desirable.
- FIG. 3 is a diagram showing a change in the diffraction peak of Ti when a nitrogen solution heat treatment is performed. Specifically, nitrogen gas is supplied at 5 L / min. The pure Ti powder was heated for 1 hour and 2 hours at 600 ° C. (873 K) in the state of flowing at a flow rate of XRD (X-ray diffraction) analysis of the Ti powder.
- nitrogen gas is supplied at 5 L / min.
- the pure Ti powder was heated for 1 hour and 2 hours at 600 ° C. (873 K) in the state of flowing at a flow rate of XRD (X-ray diffraction) analysis of the Ti powder.
- the above sintered body was heated at 1000 ° C. for 5 minutes in an argon gas atmosphere, and immediately extruded under the condition of an extrusion ratio of 37 to produce an extruded material having a diameter of 7 mm.
- the extruded material using “3 hr heated Ti powder” nitrogen content: 0.668 mass%, oxygen content: 0.265 mass%) subjected to a nitrogen solution heat treatment for 3 hours
- the tensile strength ( UTS) increased to 1264 MPa and 0.2% yield strength (YS) increased to 1204 MPa
- the preferable lower limit of the nitrogen content is 0.1% by mass.
- the nitrogen content increases almost linearly with respect to the heat treatment time, and it can be seen that the amount of nitrogen contained in the Ti powder can be controlled by the heat treatment time.
- the oxygen content was almost constant without increasing and was not oxidized during the heat treatment.
- micro Vickers hardness (load 50 g) of this sintered body was measured. The results are shown in FIG.
- the oxygen gas ratio is 10 vol. Under the condition of% or less, the amount of oxygen does not increase remarkably, and it is recognized that only nitrogen atoms are dissolved in the Ti powder matrix. On the other hand, the oxygen gas ratio is 15 vol. If it exceeds%, the amount of oxygen also increases, indicating that both atoms of nitrogen and oxygen can be dissolved in the matrix of Ti powder. As described above, according to this production method, by adjusting the mixing ratio of the nitrogen gas amount and the oxygen gas amount in the heat treatment atmosphere, it is possible to produce a Ti powder in which not only nitrogen atoms but also oxygen atoms are dissolved.
- the present invention can be advantageously used to obtain a high-strength nitrogen solid solution titanium powder material and a titanium material that uniformly diffuse and dissolve in nitrogen in the matrix and maintain proper ductility.
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Abstract
Description
JIS H 4600 2種:0.03質量%以下
JIS H 4600 3種:0.05質量%以下
JIS H 4600 4種:0.05質量%以下
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。
チタン粉末粒子からなるチタン粉末材料を、窒素を含む雰囲気中で加熱して保持することにより、窒素原子を各チタン粉末粒子のマトリクス中に均一に拡散して固溶させ、最終的に目的とする窒素固溶チタン粉末材料を得る。
加熱雰囲気:100vol.%N2ガス
ガス流量:5L/min.
加熱温度:400~600℃
保持時間:1~2hr.
純Ti原料粉末を炉内に入れ、窒素ガスを150mL/min.の流量で流入させた状態で常温から800℃(1073K)まで昇温させたところ、400℃(673K)付近から重量増加が確認され、その後は温度上昇に伴って重量が顕著に増加した。その結果を図2に示す。図2中、TG(Thermogravimetry)は重量変化を示し、DTA(Differential Thermal Analysis)は発熱・吸熱挙動を示す。
管状加熱炉内で窒素ガスを5L/min.の流量で流入させた状態で、400℃(673K)、500℃(773K)、600℃(873K)の各温度で純Ti粉末を1時間加熱した後の窒素含有量および酸素含有量を測定した。その結果を表1に示す。
図3は、窒素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。具体的には、管状加熱炉内で窒素ガスを5L/min.の流量で流入させた状態で、600℃(873K)にて純Ti粉末を1時間、および2時間加熱した後のTi粉末のXRD(X線回折)分析を行った。
各Ti粉末を放電プラズマ焼結により成形固化し、熱間押出加工を施して直径φ7mmの押出材を作製した。
1時間の窒素固溶化熱処理を行って窒素含有量が0.290質量%になった「1hr加熱Ti粉末」、2時間の窒素固溶化熱処理を行って窒素含有量が0.479質量%になった「2hr加熱Ti粉末」、および窒素固溶化熱処理を行っていない「原料Ti粉末」(窒素含有量は0.018質量%)を用いた押出材について、強度を測定した。その結果を図5および表3に示す。
純Ti粉末(平均粒子径;28μm、純度>95%)を出発原料とし、管状炉内に窒素ガス(ガス流量;3L/min.)を流入させた状態でTi原料粉末を投入し、600℃にて10分~180分の窒素固溶加熱処理を行った。得られた各Ti粉末に含まれる窒素量および酸素量と、熱処理時間との関係を測定し、その結果を図6および表4に示す。
表4に記載の窒素含有Ti粉末を、放電プラズマ焼結(SPS)装置を用いて、加熱及び加圧して焼結体(直径40mm、厚み10mm)を作製した。
温度:1000℃
加圧力:30MPa
焼結時間:30分
真空度:6Pa
純Ti粉末(平均粒子径;28μm、純度>95%)を出発原料とし、管状炉内に窒素ガスと酸素ガスとの混合比を変えて流入させた状態で、Ti原料粉末を投入し、600℃にて60分の加熱処理を行った。得られた各Ti粉末に含まれる窒素量、酸素量を測定した。その結果を図8および表6に示す。
Claims (5)
- チタン粉末粒子からなるチタン粉末材料を、窒素を含む雰囲気中で加熱して前記チタン粉末粒子のマトリクス中に窒素原子を固溶させることを特徴とする、窒素固溶チタン粉末材料の製造方法。
- 前記窒素原子をチタン粉末粒子のマトリクス中に固溶するための加熱温度は、400℃以上800℃以下である、請求項1に記載の窒素固溶チタン粉末材料の製造方法。
- 請求項1または2に記載の方法によって製造された窒素固溶チタン粉末材料であって、
前記各チタン粉末粒子の窒素含有量は、質量基準で、0.1%~0.65%である、窒素固溶チタン粉末材料。 - 請求項3に記載の窒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窒素含有量が、質量基準で、0.1%~0.65%であり、
破断伸びが10%以上である、請求項4に記載のチタン素材。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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EP14879502.4A EP3097998B1 (en) | 2014-01-24 | 2014-12-26 | Process for producing powder material of solid solution of nitrogen in titanium |
US15/113,637 US10213837B2 (en) | 2014-01-24 | 2014-12-26 | Titanium powder containing solid-soluted nitrogen, titanium material, and method for producing titanium powder containing solid-soluted nitrogen |
JP2015558769A JP6261618B2 (ja) | 2014-01-24 | 2014-12-26 | チタン素材および窒素固溶チタン粉末材料の製造方法 |
BR112016016577-2A BR112016016577B1 (pt) | 2014-01-24 | 2014-12-26 | método para a produção de pó de titânio que contém um nitrogênio solubilizado sólido |
CN201480073907.9A CN106413944B (zh) | 2014-01-24 | 2014-12-26 | 固溶有氮的钛粉末材料、钛材以及固溶有氮的钛粉末材料的制备方法 |
MX2016009440A MX2016009440A (es) | 2014-01-24 | 2014-12-26 | Polvo de titanio que contiene nitrógeno en solución sólida, material de titanio, y método para producir polvo de titanio que contiene nitrógeno en solución sólida. |
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JP2014-011362 | 2014-01-24 | ||
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EP (1) | EP3097998B1 (ja) |
JP (1) | JP6261618B2 (ja) |
CN (1) | CN106413944B (ja) |
BR (1) | BR112016016577B1 (ja) |
MX (1) | MX2016009440A (ja) |
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US10213837B2 (en) | 2019-02-26 |
MX2016009440A (es) | 2016-10-28 |
CN106413944B (zh) | 2019-06-14 |
EP3097998A1 (en) | 2016-11-30 |
JP6261618B2 (ja) | 2018-01-17 |
CN106413944A (zh) | 2017-02-15 |
BR112016016577B1 (pt) | 2021-05-04 |
US20170008087A1 (en) | 2017-01-12 |
JPWO2015111361A1 (ja) | 2017-03-23 |
BR112016016577A2 (pt) | 2017-09-26 |
EP3097998A4 (en) | 2017-09-20 |
EP3097998B1 (en) | 2024-02-07 |
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