JP5400824B2 - Titanium plate with excellent press formability - Google Patents
Titanium plate with excellent press formability Download PDFInfo
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Description
本発明は、プレス加工等の成形性に優れたチタン板に関するものである。 The present invention relates to a titanium plate having excellent formability such as press working.
チタンは優れた耐食性並びに比強度を有することから、熱交換器、化学プラント部材、或いは海岸部の構造材等に広く採用されており、特に海水に対しては全く腐食しないことから海水熱交換器に採用されることが多い。中でも、プレート式熱交換器には板状に加工したチタン板が採用されており、伝熱効率向上のために表面を凹凸形状にプレス成形したチタン板が用いられている。また、近年は伝熱効率を更に向上させるため、チタン板を薄肉化させる、凹凸形状を複雑化させるといったニーズがあり、プレス成形等の成形性が更に優れたチタン板が開発されることが待望されているという背景もあり、プレス成形性に優れたチタン板に関しては、そのチタン板の材質等の構成並びにその成形加工技術に関する様々な提案がある。 Titanium has excellent corrosion resistance and specific strength, so it is widely used in heat exchangers, chemical plant members, coastal structural materials, etc., especially seawater, so it does not corrode at all. It is often adopted for. In particular, a plate-type heat exchanger employs a titanium plate processed into a plate shape, and a titanium plate whose surface is press-formed into an uneven shape is used to improve heat transfer efficiency. In recent years, in order to further improve the heat transfer efficiency, there is a need for thinning the titanium plate and complicating the uneven shape, and it is expected that a titanium plate having further excellent formability such as press molding will be developed. With respect to the titanium plate excellent in press formability, there are various proposals regarding the composition of the material of the titanium plate and the forming technique thereof.
チタンの材質面では、チタンの結晶構造が六方晶であるために異方性があることから、特許文献1として、通常の圧延方向と直角に圧延して、異方性を低減する方法が提案されている。しかしながら、この方法では、製造工程の途中で圧延方向を変更しなければならないため、生産性を落とさざるを得ないという実情があった。
Since the titanium crystal structure is hexagonal in terms of the material of titanium, there is anisotropy. Therefore,
成形加工技術の観点からは、表面潤滑の適正化等が検討されており、例えば、特許文献2として、板材の表面に潤滑剤キャリアの鉄、亜鉛合金層を形成させ、その後、リン酸亜鉛処理を行い、潤滑剤を塗布するという方法が提案されている。しかしながら、この方法では、潤滑剤処理に多数の工程が必要となり、その面で不効率な方法であった。 From the viewpoint of forming technology, optimization of surface lubrication has been studied. For example, as Patent Document 2, an iron or zinc alloy layer of a lubricant carrier is formed on the surface of a plate material, and then zinc phosphate treatment is performed. And a method of applying a lubricant has been proposed. However, this method requires many steps for the lubricant treatment, and is inefficient in that respect.
また、板材の表面潤滑性に着目した提案も多くあり、特許文献3および特許文献4として、板材の表面に酸化被膜を形成させたチタン板とその製造方法が、特許文献5として、板材の表面に窒素富化層を形成させたチタン板とその製造方法が、特許文献6として、板材の表面にTiC含有層を形成させたチタン板が、夫々提案されている。しかしながら、これらのチタン板やその製造方法では、板材の表面に被覆層を形成する必要があり、その製造工程が複雑であるという実情があった。 In addition, there are many proposals focusing on the surface lubricity of the plate material. Patent Documents 3 and 4 disclose a titanium plate having an oxide film formed on the surface of the plate material and a manufacturing method thereof as Patent Document 5 and the surface of the plate material. A titanium plate having a nitrogen-enriched layer formed thereon and a method for producing the same have been proposed as Patent Document 6, and a titanium plate having a TiC-containing layer formed on the surface of a plate material has been proposed. However, in these titanium plates and their manufacturing methods, it is necessary to form a coating layer on the surface of the plate material, and the manufacturing process is complicated.
また、チタンは優れた軽量性、耐食性並びに意匠性を有することから、マフラー等の二輪や四輪の部材にも適用されている。これらに適用するために、チタンには、張出し性、深絞り性、曲げ加工性、伸びフランジ性などの複雑で多様な加工に対応できる成形加工性が求められている。 Titanium is also applied to two-wheel and four-wheel members such as a muffler because it has excellent lightness, corrosion resistance, and design. In order to apply to these, titanium is required to have moldability that can cope with complicated and diverse processes such as stretchability, deep drawability, bending workability, and stretch flangeability.
本発明は、上記従来の問題を解決せんとしてなされたもので、プレス成形性に優れたうえに、伸びフランジ性にも優れたチタン板を提供することを課題とするものである。 The present invention has been made to solve the above-described conventional problems, and an object of the present invention is to provide a titanium plate that is excellent in press moldability and excellent in stretch flangeability.
請求項1記載の発明は、質量%で、Feを0.04〜0.10%、Oを0.07〜0.20%含有し、残部がTiおよび不可避的不純物であって、1/4t(tは板厚)部の圧延面における圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率が、30%以上であると共に、1/4t(tは板厚)部の1mm×1mmの平面内に存在する全結晶粒(α相)のうち、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率が90%以下であることを特徴とするプレス成形性に優れたチタン板である。
The invention according to
請求項2記載の発明は、1/4t(tは板厚)部の1mm×1mmの平面内に存在する結晶粒(α相)の平均結晶粒径が、20〜200μmである請求項1記載のプレス成形性に優れたチタン板である。 According to a second aspect of the present invention, the average crystal grain size of crystal grains (α phase) existing within a 1 mm × 1 mm plane of a 1/4 t (t is a plate thickness) portion is 20 to 200 μm. It is a titanium plate excellent in press formability.
本発明によると、プレス成形性に優れたチタン板を得ることができる。また、チタン本来の優れた耐久性はもとより、高い機械的強度に加えて、優れたプレス成形性並びに優れた伸びフランジ性を有しているので、プレート式熱交換器の構成材のほか、二輪・四輪部材、燃料電池のセパレーター、携帯電話機、モバイルパソコン、カメラのボディ、眼鏡フレーム等、高耐力で高度な成形性が要求される用途に広く適用することができる。 According to the present invention, a titanium plate excellent in press formability can be obtained. In addition to the excellent durability inherent in titanium, in addition to high mechanical strength, it has excellent press formability and excellent stretch flangeability. -Widely applicable to applications that require high strength and high formability, such as four-wheel members, fuel cell separators, mobile phones, mobile personal computers, camera bodies, and spectacle frames.
また、結晶粒(α相)の平均結晶粒径を、適切に制御することで、優れたプレス成形性を確保したうえで、且つ、伸びフランジ性に優れたチタン板とすることができる。 In addition, by appropriately controlling the average crystal grain size of the crystal grains (α phase), it is possible to obtain a titanium plate having excellent press formability and excellent stretch flangeability.
本発明者らは、プレス成形性に優れたうえに、伸びフランジ性にも優れたチタン板を得るために、鋭意、実験、研究を進めた。その結果、Feの含有量とOの含有量を規定したうえで、そのチタン板の1/4t(tは板厚)部の圧延面における圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率を、適切に制御すると共に、チタン板の1/4t(tは板厚)部の平面の1mm×1mm内に存在する結晶粒(α相)のうち、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率を適切に制御することで、プレス成形性に優れたうえに、伸びフランジ性にも優れたチタン板を得ることができることを見出し、本発明の完成に至った。 In order to obtain a titanium plate having excellent press formability and excellent stretch flangeability, the present inventors have intensively conducted experiments and research. As a result, the Fe content and the O content are defined, and {11-22} <11-23 at the time of rolling in the rolling surface of the 1/4 t (t is the plate thickness) portion of the titanium plate. > The crystal grain (α which is within 1 mm × 1 mm of the plane of the 1 / 4t (t is the plate thickness) portion of the titanium plate while appropriately controlling the area ratio of the Schmid factor of twin deformation of 0.47 or more. Phase), by appropriately controlling the area ratio occupied by the crystal grains whose c-axis angle with respect to the rolling direction is 70 to 90 °, the titanium plate has excellent press formability and excellent stretch flangeability The present invention was completed and the present invention was completed.
以下、本発明を実施形態に基づき詳細に説明する。 Hereinafter, the present invention will be described in detail based on embodiments.
本発明では、チタン板の成分組成と、そのチタン板の1/4t(tは板厚)部の圧延面における圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率、並びに、チタン板の1/4t(tは板厚)部の平面の1mm×1mm内に存在する結晶粒(α相)のうち、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率を規定するが、まず、成分組成について説明する。 In the present invention, the component composition of the titanium plate and the Schmid factor of {11-22} <11-23> twin deformation at the time of rolling in the rolling surface of the 1/4 t (t is the plate thickness) portion of the titanium plate. Is an area ratio of 0.47 or more, and the angle of the c-axis with respect to the rolling direction among crystal grains (α phase) existing within 1 mm × 1 mm of the plane of a 1/4 t (t is the plate thickness) portion of the titanium plate Defines the area ratio occupied by crystal grains of 70 to 90 °. First, the component composition will be described.
(成分組成)
純チタンは、不可避的不純物としてC、H、O、N、Fe等を微量に含有するが、本発明では、その中でも含有量が比較的多く、機械的性質に影響を及ぼすFeとOの含有量を規定した。
(Component composition)
Pure titanium contains a small amount of C, H, O, N, Fe, etc. as unavoidable impurities, but in the present invention, the content is relatively large, and the inclusion of Fe and O that affects mechanical properties. The amount was specified.
Feの含有量が0.10質量%を超えて多くなりすぎると、耐力が大きくなりすぎてプレス成形性および伸びフランジ性が低下する傾向がある。従って、Feの含有量の上限は0.10質量%とする。尚、Feの含有量の好ましい上限は0.08質量%であり、より好ましい上限は0.06質量%である。一方、Feの含有量が0.04質量%より少なくなると耐力が小さくなりすぎるので、Feの含有量の下限は0.04質量%とする。 If the Fe content exceeds 0.10 mass% and increases too much, the proof stress tends to be too high, and the press formability and stretch flangeability tend to decrease. Therefore, the upper limit of the Fe content is 0.10% by mass. In addition, the upper limit with preferable Fe content is 0.08 mass%, and a more preferable upper limit is 0.06 mass%. On the other hand, if the Fe content is less than 0.04% by mass, the yield strength becomes too small, so the lower limit of the Fe content is 0.04% by mass.
Oの含有量が0.20質量%を超えて多くなりすぎると、耐力が大きくなりすぎてプレス成形性および伸びフランジ性が低下する傾向がある。従って、Oの含有量の上限は0.20質量%とする。尚、Oの含有量の好ましい上限は0.16質量%であり、より好ましい上限は0.12質量%である。一方、Oの含有量が0.07質量%より少なくなると耐力が小さくなりすぎるので、Oの含有量の下限は0.07質量%とする。 If the O content exceeds 0.20% by mass, the proof stress tends to be too high, and the press formability and stretch flangeability tend to decrease. Therefore, the upper limit of the O content is 0.20% by mass. In addition, the upper limit with preferable content of O is 0.16 mass%, and a more preferable upper limit is 0.12 mass%. On the other hand, if the O content is less than 0.07% by mass, the yield strength becomes too small, so the lower limit of the O content is 0.07% by mass.
また、チタン板の1/4t(tは板厚)部の圧延面における圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率、並びに、チタン板の1/4t(tは板厚)部の平面の1mm×1mm内に存在する結晶粒(α相)のうち、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率の、規定理由は以下のとおりである。 Further, the area ratio of {11-22} <11-23> twinning deformation Schmid factor of 0.47 or more at the time of rolling in the rolling direction of the 1/4 t (t is the plate thickness) portion of the titanium plate, and Of the crystal grains (α phase) existing within 1 mm × 1 mm of the plane of the 1/4 t (t is the plate thickness) portion of the titanium plate, the crystal grains whose c-axis angle with respect to the rolling direction is 70 to 90 ° occupy The reason for defining the area ratio is as follows.
(圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率)
チタン板の1/4t(tは板厚)部の圧延面における、圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子(Schmid factor)が0.47以上の面積率が少なすぎると、チタン板の成形時に発生する変形双晶の頻度が少なくなりすぎて、本発明で意図する優れたプレス成形性を得られなくなってしまう。本発明で意図する優れたプレス成形性を確保するためには、前記した圧延方向引張時の{11−22}面のシュミット因子が0.47以上の面積率が30%以上でなければならない。好ましくはシュミット因子が0.47以上の面積率を35%以上、より好ましくはシュミット因子が0.47以上の面積率を40%以上とする必要がある。
(The area ratio of {11-22} <11-23> twinning deformation Schmid factor at the time of rolling in the rolling direction is 0.47 or more)
The area where the Schmid factor of the {11-22} <11-23> twin deformation during rolling in the rolling direction is 0.47 or more on the rolled surface of the 1/4 t (t is the plate thickness) portion of the titanium plate. If the rate is too small, the frequency of deformation twins generated at the time of forming the titanium plate becomes too low, and the excellent press formability intended in the present invention cannot be obtained. In order to ensure the excellent press formability intended in the present invention, the area ratio with the Schmid factor of the {11-22} plane at the time of pulling in the rolling direction of 0.47 or more must be 30% or more. Preferably, the area ratio with a Schmitt factor of 0.47 or more needs to be 35% or more, more preferably the area ratio with a Schmitt factor of 0.47 or more needs to be 40% or more.
(圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率)
チタン板の/4t(tは板厚)部の1mm×1mmの平面内に存在する全結晶粒(α相)のうち、図1に示す圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率が大きくなりすぎると、材料の異方性が大きくなりすぎ、等方的な変形を伴う伸びフランジ性が低下し、本発明で意図する伸びフランジ性が得られなくなってしまう。本発明で意図する伸びフランジ性を得るためには、前記した圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率が90%以下でなければならない。好ましくはその面積率を85%以下、より好ましくはその面積率を80%以下とする。
(Area ratio occupied by crystal grains whose c-axis angle with respect to the rolling direction is 70 to 90 °)
Of all crystal grains (α phase) existing in a 1 mm × 1 mm plane of a / 4t (t is the plate thickness) portion of the titanium plate, a crystal whose c-axis angle is 70 to 90 ° with respect to the rolling direction shown in FIG. If the area ratio occupied by the grains becomes too large, the anisotropy of the material becomes too large, the stretch flangeability accompanied by isotropic deformation is lowered, and the stretch flangeability intended in the present invention cannot be obtained. In order to obtain the stretch flangeability intended in the present invention, the area ratio occupied by the crystal grains having the c-axis angle of 70 to 90 ° with respect to the rolling direction must be 90% or less. The area ratio is preferably 85% or less, and more preferably the area ratio is 80% or less.
(結晶粒の平均結晶粒径)
以上が本発明で規定する必須要件であるが、更にチタン板の/4t(tは板厚)部の1mm×1mmの平面内に存在する結晶粒(α相)の平均結晶粒径を適切に制御することで、優れたプレス成形性を確保したうえで、且つ、伸びフランジ性に優れたチタン板とすることができる。
(Average crystal grain size of crystal grains)
The above is the essential requirement specified in the present invention, but the average grain size of crystal grains (α phase) existing in a 1 mm × 1 mm plane of the / 4t (t is the plate thickness) portion of the titanium plate is appropriately set. By controlling, it is possible to obtain a titanium plate having excellent press formability and excellent stretch flangeability.
チタン板の/4t(tは板厚)部の1mm×1mmの平面内に存在する結晶粒(α相)の平均結晶粒径が大きくなりすぎると、プレス成形後のチタン板の肌荒れが顕著になり、プレス成形品として外観上好ましくなくなる。従って、結晶粒(α相)の平均結晶粒径は、200μm以下とする。結晶粒(α相)の平均結晶粒径のより好ましい上限は150μm、更に好ましい上限は100μmである。一方、平均結晶粒径が小さくなりすぎると、チタン板の成形時に発生する変形双晶の頻度が少なくなりすぎて、十分な延性を確保できなくなり、本発明で意図する優れたプレス成形性を得られなくなってしまう。従って、結晶粒(α相)の平均結晶粒径は、20μm以上とする。結晶粒(α相)の平均結晶粒径のより好ましい下限は35μm、更に好ましい下限は50μmである。 When the average crystal grain size of the crystal grains (α phase) existing in a plane of 1 mm × 1 mm of the / 4t (t is the plate thickness) portion of the titanium plate becomes too large, the rough surface of the titanium plate after press forming becomes remarkable. Therefore, it is not preferable in appearance as a press-formed product. Therefore, the average crystal grain size of the crystal grains (α phase) is 200 μm or less. A more preferable upper limit of the average crystal grain size of the crystal grains (α phase) is 150 μm, and a more preferable upper limit is 100 μm. On the other hand, if the average crystal grain size is too small, the frequency of deformation twins generated during the formation of the titanium plate is too low, and sufficient ductility cannot be secured, and the excellent press formability intended in the present invention is obtained. It will not be possible. Therefore, the average crystal grain size of the crystal grains (α phase) is 20 μm or more. The more preferable lower limit of the average crystal grain size of the crystal grains (α phase) is 35 μm, and the more preferable lower limit is 50 μm.
(製造条件)
次に、本発明のチタン板の製造方法について説明する。通常のチタン板は、分塊圧延→熱間圧延→中間焼鈍→冷間圧延→最終焼鈍といった各工程間に、随時ブラスト、酸洗処理を入れて製造されるが、製造するチタン板の成分組成や各工程の設定条件によって、得られる物性や組織状態は変わるので、一連の製造工程として総合的に条件を選択して決定すべきであって、個々の工程毎に条件を厳密に設定することは必ずしも適切でない。
(Production conditions)
Next, the manufacturing method of the titanium plate of this invention is demonstrated. Ordinary titanium plates are manufactured by adding blasting and pickling treatment at any time between each process of lump rolling → hot rolling → intermediate annealing → cold rolling → final annealing, but the component composition of the titanium plate to be manufactured Since the physical properties and structure of the product to be obtained vary depending on the setting conditions of each process, the conditions should be selected and determined comprehensively as a series of manufacturing processes, and the conditions must be set strictly for each process. Is not necessarily appropriate.
しかしながら、本発明のチタン板を製造するための製造条件を、本発明者らが鋭意検討したところ、以下に示す製造条件を採用することで、本発明で意図するプレス成形性および伸びフランジ性に優れたチタン板を確実に製造することができることを確認した。 However, when the present inventors diligently examined the production conditions for producing the titanium plate of the present invention, by adopting the production conditions shown below, the press formability and stretch flangeability intended by the present invention are achieved. It was confirmed that an excellent titanium plate could be produced reliably.
その製造条件は、分塊圧延、熱間圧延、冷間圧延を全て同一方向で行うと共に、分塊圧延の1パスあたりの圧下率を5%以上、最終冷延率を70%以上、最終焼鈍温度を500〜750℃、最終焼鈍の保持時間を1時間以下とすることである。これらの条件を適切に組み合わせてチタン板を製造することで、本発明で意図するプレス成形性および伸びフランジ性に優れたチタン板を製造することができる。 The production conditions are that the partial rolling, hot rolling, and cold rolling are all performed in the same direction, the rolling reduction per pass of the partial rolling is 5% or more, the final cold rolling rate is 70% or more, and the final annealing. The temperature is 500 to 750 ° C., and the holding time of the final annealing is 1 hour or less. By producing a titanium plate by appropriately combining these conditions, a titanium plate excellent in press formability and stretch flangeability intended in the present invention can be produced.
以下、実施例を挙げて本発明をより具体的に説明するが、本発明はもとより下記実施例によって制限を受けるものではなく、本発明の趣旨に適合し得る範囲で適宜変更を加えて実施することも可能であり、それらは何れも本発明の技術的範囲に含まれる。 EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention is not limited by the following examples, and the present invention is implemented with appropriate modifications within a range that can meet the gist of the present invention. These are all included in the technical scope of the present invention.
本実施例では、まず、CCIM(コールドクルーシブル誘導溶解法)により表1に示す含有量でFe並びにOを含有するチタン鋳塊を鋳造した。残部はTiおよびC、H、N、等の不可避的不純物である。鋳塊の大きさはφ100mmの円柱形で、10kgである。この鋳塊を用いて表1に示す1パスあたりの圧下率で分塊圧延を行い、その後は放冷して厚み45mmの板形状の分塊圧延材を得た。更に、熱間圧延を実施し、スケール除去を行い厚み約5mmの熱延板を得た。 In this example, first, a titanium ingot containing Fe and O at the contents shown in Table 1 was cast by CCIM (cold crucible induction melting method). The balance is Ti and unavoidable impurities such as C, H, N, and the like. The size of the ingot is 10 kg in a cylindrical shape of φ100 mm. Using this ingot, the partial rolling was performed at the rolling reduction per pass shown in Table 1, and then the mixture was allowed to cool to obtain a plate-shaped partial rolled material having a thickness of 45 mm. Furthermore, hot rolling was performed, scale removal was performed, and a hot rolled sheet having a thickness of about 5 mm was obtained.
次いで、大気炉にて、700℃で5分間加熱してから空冷する焼鈍処理(中間焼鈍)を行った後、スケール除去を行った。次に、表1に示す冷延率で冷間圧延を行った後、真空焼鈍炉にて、表1に示す条件で加熱してから空冷する焼鈍処理(最終焼鈍)を行い、次いで、スキンパスを実施し、スケール除去を行って厚み0.5mmのチタン板を製造した。 Next, after performing an annealing treatment (intermediate annealing) in which air cooling was performed at 700 ° C. for 5 minutes in an atmospheric furnace, scale removal was performed. Next, after performing cold rolling at the cold rolling rate shown in Table 1, in the vacuum annealing furnace, it is heated under the conditions shown in Table 1 and then air-cooled (final annealing), and then the skin pass is performed. The scale was removed and a titanium plate having a thickness of 0.5 mm was manufactured.
本実施例では、製造した各チタン板の金属組織等の観察・測定と、耐力およびプレス成形性の評価を夫々下記の要領で行った。 In this example, observation and measurement of the metal structure and the like of each manufactured titanium plate and evaluation of proof stress and press formability were performed in the following manner.
本実施例では、電界放出型走査顕微鏡(Field Emission Scanning Electron Microscope:FESEM)(日本電子社製、JSM5410)に、後方錯乱電子回析像(Electron Back Scattering(Scattered) Pattern:EBSP)システムを搭載した結晶方位解析法によって金属組織の観察・測定を実施した。この測定方法を用いたのは、EBSP法は他の測定方法と比較して高分解能であり、高精度な測定ができるためである。まず、測定原理について説明する。 In this example, a field emission scanning electron microscope (FESEM) (manufactured by JEOL Ltd., JSM5410) is equipped with a back-scattered electron diffraction image (Electron Back Scattering (Scattered) Pattern system). The metal structure was observed and measured by the crystal orientation analysis method. This measurement method was used because the EBSP method has higher resolution than other measurement methods and can perform measurement with high accuracy. First, the measurement principle will be described.
EBSP法は、FESEMの鏡筒内にセットした試料に電子線を照射してスクリーン上にEBSPを投影する。これを高感度カメラで撮影して、コンピュータに画像として取り込む。この画像を解析して、既知の結晶系を用いたシミュレーションによるパターンとの比較によって、結晶の方位が決定される。算出された結晶の方位は3次元オイラー角として、位置座標(x、y)などと共に記録される。このプロセスが全測定点に対して自動的に行われるので、測定終了時には数万〜数十万点のデータを得ることができる。 In the EBSP method, an electron beam is irradiated onto a sample set in a lens barrel of FESEM to project EBSP on a screen. This is taken with a high-sensitivity camera and captured as an image on a computer. The orientation of the crystal is determined by analyzing this image and comparing it with a pattern obtained by simulation using a known crystal system. The calculated crystal orientation is recorded as a three-dimensional Euler angle together with position coordinates (x, y) and the like. Since this process is automatically performed for all measurement points, data of tens of thousands to hundreds of thousands of points can be obtained at the end of measurement.
このように、EBSP法には、X線回析法や透過電子顕微鏡を用いた電子線回析法よりも、観察視野が広く、数百個以上の多数の結晶粒に対する各種情報を、数時間以内で得ることができる利点がある。また、結晶粒毎の測定ではなく、指定した領域を一定間隔で走査して測定するために、測定領域全体を網羅した上記多数の測定ポイントに関する、上記各情報を得ることができる利点もある。尚、これらFESEMにEBSPシステムを搭載した結晶方位解析法の詳細は、神戸製鋼技報/Vol.52 No.2(Sep.2002)P66−70などに詳細に記載されている。 Thus, the EBSP method has a wider field of view than the X-ray diffraction method or the electron beam diffraction method using a transmission electron microscope, and can provide various information on hundreds of crystal grains for several hours. There are advantages you can get within. In addition, since the specified region is scanned at a fixed interval instead of the measurement for each crystal grain, there is an advantage that each of the above-mentioned information regarding the above-described many measurement points covering the entire measurement region can be obtained. Details of the crystal orientation analysis method in which the EBSP system is mounted on these FESEMs are described in Kobe Steel Technical Report / Vol. 52 no. 2 (Sep. 2002) P66-70 and the like.
(圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47 以上の面積率、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率)
チタン板の圧延面表面を機械研磨し、更に、バフ研磨に次いで電解研磨を行い、チタン板の表面から深さt/4(tは板厚)部の圧延面(チタン板の表面に平行な面であって、その板厚方向の深さt/4部の面)の結晶組織が観察できるように調整し、その圧延面における圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率、並びに、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率を、前記した測定により得た。測定エリアは1mm×1mmの平面内とし、測定ピッチは1μmとした。
(The area ratio occupied by the {11-22} <11-23> twin crystal deformation Schmid factor at the time of rolling in the rolling direction is 0.47 or more, and the crystal grains whose c-axis angle with respect to the rolling direction is 70 to 90 °. )
The surface of the rolled surface of the titanium plate is mechanically polished, followed by buffing and electrolytic polishing, and the rolled surface at a depth of t / 4 (t is the thickness) from the surface of the titanium plate (parallel to the surface of the titanium plate). The surface is adjusted so that the crystal structure of the surface (thickness t / 4 part depth in the plate thickness direction) can be observed, and {11-22} <11-23> The area ratio of the Schmid factor of crystal deformation of 0.47 or more and the area ratio occupied by the crystal grains having the c-axis angle of 70 to 90 ° with respect to the rolling direction were obtained by the above-described measurement. The measurement area was in a 1 mm × 1 mm plane, and the measurement pitch was 1 μm.
圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率は、測定した各測定点のシュミット因子が0.47以上の測定点の数を全測定点の数で割ることにより算出した。 The area ratio in which the Schmid factor of the {11-22} <11-23> twin deformation in the rolling direction tension is 0.47 or more is the number of measurement points having a Schmit factor of 0.47 or more at each measured measurement point. Calculated by dividing by the total number of measurement points.
圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率は、測定した各測定点のc軸の角度が70〜90°の数を全測定点の数で割ることにより算出した。 The area ratio occupied by the crystal grains having the c-axis angle of 70 to 90 ° with respect to the rolling direction was calculated by dividing the number of c-axis angles of 70 to 90 ° at each measured measurement point by the number of all measurement points. .
<結晶粒(α相)の平均結晶粒径>
結晶粒(α相)の平均結晶粒径は、チタン板の圧延面表面を機械研磨し、更に、バフ研磨に次いでエッチングを行い、チタン板の表面から深さt/4部の圧延面の結晶組織が観察できるように調整し、光学顕微鏡を用いて×100にて任意の3箇所を写真撮影し、得られた写真を元にJIS G 0551の切断法により粒度番号測定を実施し、その粒度番号をもとにα相の円相当平均粒径(直径)を計算により求めた。尚、粒度番号測定に用いた光学顕微鏡による観察領域は1mm×1mmとした。
<Average crystal grain size of crystal grains (α phase)>
The average crystal grain size of the crystal grains (α phase) is obtained by mechanically polishing the rolled surface of the titanium plate, further etching after buffing, and crystal of the rolled surface at a depth of t / 4 part from the surface of the titanium plate. Adjusted so that the structure can be observed, photographed any three locations at × 100 using an optical microscope, and performed particle size number measurement according to the cutting method of JIS G 0551 based on the obtained photograph. Based on the number, the circle equivalent average particle diameter (diameter) of the α phase was obtained by calculation. In addition, the observation area | region by the optical microscope used for the particle size number measurement was 1 mm x 1 mm.
<耐力の測定>
チタン板の耐力については、製造した各チタン板からJISZ2201に規定される13号試験片を作製し、この試験片について、JISZ2241に準拠する引張試験を行い、試験片の圧延方向の0.2%耐力(YS)を測定することで求めた。尚、試験片は、その長手方向(L方向)が圧延方向と一致するようにして採取した。また、試験速度(引張試験での歪み速度)は、0.3mm/minで一定とした。
<Measurement of yield strength>
Regarding the proof stress of the titanium plate, No. 13 test piece defined in JISZ2201 is prepared from each manufactured titanium plate, a tensile test based on JISZ2241 is performed on this test piece, and 0.2% in the rolling direction of the test piece. It calculated | required by measuring yield strength (YS). In addition, the test piece was extract | collected so that the longitudinal direction (L direction) might correspond with a rolling direction. The test speed (strain speed in the tensile test) was constant at 0.3 mm / min.
この試験で得られた試験片の圧延方向の0.2%耐力(YS)が200MPa以上のものを、高耐力であると評価した。 A test piece obtained in this test having a 0.2% yield strength (YS) in the rolling direction of 200 MPa or more was evaluated as having high yield strength.
<プレス成形性>
プレス成形性については、図2に示すような、V字形の溝を設けたプレート式熱交換器の熱交換部分をプレス成形することを模擬したプレス成形金型を用いてチタン板(試験体)のプレス成形を実施し、その評価を行った。プレス成形金型は、図1に示すように、成形部の大きさが100mm×100mmで、その表面には、ピッチ10mm、最大高さ4mmの平面V字形の平行する稜線部が6本形成されている。その各稜線部のR形状は、図2(a)の上から下に向かって順に、R=0.4、1.8、0.8、1.0、1.4、0.6の計6種類である。
<Press formability>
As for press formability, as shown in FIG. 2, a titanium plate (test body) using a press mold that simulates press forming of a heat exchange portion of a plate heat exchanger provided with a V-shaped groove. The press molding was carried out and evaluated. As shown in FIG. 1, the press-molding die has a size of a molding portion of 100 mm × 100 mm, and six parallel V-shaped parallel ridge portions having a pitch of 10 mm and a maximum height of 4 mm are formed on the surface. ing. The R shape of each ridge line portion is a total of R = 0.4, 1.8, 0.8, 1.0, 1.4, 0.6 in order from the top to the bottom of FIG. There are six types.
この成形金型を用いて80ton油圧プレス機によってプレス成形を実施した。具体的には、各試験体の表裏面に動粘度34mm2/s(40℃)のプレス油を塗布し、各試験体を、その圧延方向(L方向)が図2(a)の上下方向と一致するようにして下金型の上面に配置し、そのフランジ部を板押さえで拘束した後、プレス速度1mm/s、押し込み深さ3.4mmの条件でプレス成形を実施した。プレス成形性の評価は、プレス成形後に認められる割れの数で評価した。具体的な評価方法を以下に説明する。 Using this molding die, press molding was performed by an 80 ton hydraulic press. Specifically, press oil having a kinematic viscosity of 34 mm 2 / s (40 ° C.) is applied to the front and back surfaces of each test specimen, and each test specimen is rolled in the rolling direction (L direction) in the vertical direction of FIG. Was placed on the upper surface of the lower mold so as to coincide with the above, and the flange portion was constrained by a plate press, and then press molding was performed under the conditions of a press speed of 1 mm / s and an indentation depth of 3.4 mm. The press formability was evaluated by the number of cracks observed after press forming. A specific evaluation method will be described below.
プレス成形後の各試験体の図2(a)に示す稜線部と、測定位置A、B、C、C´、D、Eの一点鎖線との交点計36箇所について、割れの有無を目視で観察した。尚、測定位置C´は、図2(b)に示すように、隣接する稜線部の間に位置する谷部である。 The presence or absence of cracks is visually observed at 36 points of intersection between the ridge line portion shown in FIG. 2A of each test body after press molding and the one-dot chain lines of measurement positions A, B, C, C ′, D, and E. Observed. Note that the measurement position C ′ is a valley portion located between adjacent ridge line portions, as shown in FIG.
この目視において、割れの起点となる測定位置A、C、C´、Eについては、割れもくびれも認められなければ2点、くびれが認められれば1点、割れが認められれば0点とし、他の測定位置B、Dについては、割れもくびれも認められなければ1点、くびれが認められれば0.5点、割れが認められれば0点とし、更にその各点数に加工Rの逆数を掛けて割れの状態を数値化し、その合計値を求めた。その合計値を、完全に割れ、くびれが認められない場合を100として規格化した後、温度(T)、潤滑油の粘度(μ)、試験体の板厚(t)に依存する関数F(T,μ,t)、並びに、プレス金型の稜線の角度(α)、ピッチ(p)に依存する関数G(α,p)を掛け合わせて、成形性スコアとして算出した。尚、F並びにGは0〜1の値である。 In this visual inspection, the measurement positions A, C, C ′, and E, which are the starting points of cracking, are 2 points if neither cracking nor constriction is observed, 1 point if constriction is recognized, 0 point if cracking is recognized, For other measurement positions B and D, 1 point is given if neither cracking nor constriction is observed, 0.5 point if constriction is recognized, 0 point if cracking is observed, and the reciprocal of machining R is added to each point. Multiply it and digitize the state of the cracks and determine the total. After normalizing the total value as 100 when the case where cracks are not completely observed and constriction is observed, the function F () depends on the temperature (T), the viscosity of the lubricating oil (μ), and the plate thickness (t) of the specimen. T, μ, t) and the function G (α, p) depending on the angle (α) and pitch (p) of the ridge line of the press mold were multiplied to calculate the formability score. Note that F and G are values from 0 to 1.
以上の成形性スコアの算出方法は、下記式によって表すことができる。
成形性スコア=F×G×ΣE(ij)/R(j)/(ΣA,C,C´,E 2/R(j)+ΣB,D 1/R(j))×100
この式において、A、C、C´、Eの場合は、E(ij)=1.0×(割れくびれなし:2、くびれ:1、割れ0)として、また、B、Dの場合は、E(ij)=0.5×(割れくびれなし:2、くびれ:1、割れ0)として算出した。また、本実施例では、温度(T)、潤滑油の粘度(μ)、試験体の板厚(t)、プレス金型の稜線の角度(α)、およびプレス金型の稜線のピッチ(p)を一定としたため、F×Gを便宜的に1として成形性スコアを算出した。
The calculation method of the above moldability score can be represented by the following formula.
Formability score = F × G × ΣE (ij) / R (j) / (ΣA, C, C ′, E2 / R (j) + ΣB,
In this equation, in the case of A, C, C ′, E, E (ij) = 1.0 × (no cracking of the neck: 2, necking: 1, cracking 0), and in the case of B and D, E (ij) = 0.5 × (no cracking: 2, necking: 1, cracking 0). In this example, the temperature (T), the viscosity of the lubricating oil (μ), the thickness of the specimen (t), the angle of the ridge line of the press mold (α), and the pitch of the ridge line of the press mold (p ) Was constant, the moldability score was calculated with F × G as 1 for convenience.
この算出した成形性スコアが50点以上のものをプレス成形性に優れていると評価した。尚、表1には、成形性スコアが75点以上のものを◎、50点〜75点未満を○、50点未満を×として示す。 Those having a calculated moldability score of 50 or more were evaluated as being excellent in press moldability. In Table 1, those having a moldability score of 75 points or more are shown as ◎, 50 points to less than 75 points as ○, and less than 50 points as ×.
<伸びフランジ性>
チタン板の伸びフランジ性については、製造した各チタン板から70×70×0.5mmのブランクを切り出し、そのブランクの中心にφ10の孔を打ち抜きにより形成した後、打ち抜き時に生成されたバリが板上方になるようにしてダイスにセットし、下方から上方へ60°円錐パンチを押し上げる孔拡げ試験を実施することで求めた。
<Stretch flangeability>
Regarding the stretch flangeability of the titanium plate, a 70 × 70 × 0.5 mm blank is cut out from each manufactured titanium plate, a hole of φ10 is formed in the center of the blank by punching, and the burr generated at the time of punching is a plate. It was determined by carrying out a hole expansion test in which it was set on a die so as to face upward and a 60 ° conical punch was pushed upward from below.
試験では、孔の縁にクラックが生成されたことを目視により確認できた時点で速やかにパンチの押し上げを停止し、その時点での孔の直径を測定した後に、(試験後の孔の直径)/(試験前の孔の直径)という式より孔拡げ率λ(%)を算出した。この算出した孔拡げ率λが90%以上のものを伸びフランジ性に優れていると評価した。 In the test, when it was confirmed visually that a crack was generated at the edge of the hole, the punch was stopped immediately, and after measuring the diameter of the hole, the diameter of the hole after the test) The hole expansion rate λ (%) was calculated from the formula / (diameter of hole before test). Those having a calculated hole expansion ratio λ of 90% or more were evaluated as having excellent stretch flangeability.
<肌荒れ>
前記したプレス成形性の評価で、各試験体において、プレス成形後に割れが認められなかったV字形頂点部について、目視で肌荒れの状態を確認した。この確認により、V字形頂点部に、肌荒れが全く認められないものを○、明らかな凹凸が認められるものを×とし、○をプレス成形後も優れた外観であるとして評価した。
<Rough skin>
In the evaluation of the press formability described above, in each specimen, the rough surface state was visually confirmed for the V-shaped apex portion in which no crack was observed after press forming. Based on this confirmation, a case where no rough skin was observed at the V-shaped apex portion was evaluated as ◯, a case where clear unevenness was observed as ×, and ○ was evaluated as having an excellent appearance even after press molding.
以上の試験結果を表1に示す。 The test results are shown in Table 1.
No.1は、Feの含有量が下限の0.04質量%のもの、No.2は、Feの含有量が上限の0.10質量%のものであり、また、No.3は、Oの含有量が上限の0.20質量%のもの、No.4は、分塊圧延の1パスあたりの圧下率が下限に近いもの、No.5は、分塊圧延の1パスあたりの圧下率が9.2%と高いもの、No.6は、冷間圧延の最終冷延率が上限に近いもの(Oの含有量も下限に近い)、No.7は冷間圧延の最終冷延率が下限の70%のものである。これらNo.1〜7の成分組成は、全て本発明の要件を満足し、製造条件も好ましい条件である。
No. No. 1 has a lower Fe content of 0.04% by mass. No. 2 has an upper limit of Fe content of 0.10% by mass. No. 3 has an O content of 0.20% by mass of the upper limit. No. 4 is the one where the rolling reduction per pass of the ingot rolling is close to the lower limit. No. 5 has a high rolling reduction rate of 9.2% per pass of the ingot rolling. No. 6 shows that the final cold rolling ratio of cold rolling is close to the upper limit (the content of O is also close to the lower limit). 7 is 70% of the lower limit of the final cold rolling ratio of cold rolling. These No. The
これに対し、No.8は、Feの含有量が上限を超えるもの、No.9は、Oの含有量が上限を超えるもの、No.10は、分塊圧延の1パスあたりの圧下率が下限より低いもの、No.11は、冷間圧延の最終冷延率が下限より低いものであり、No.12は、結晶粒(α相)の平均結晶粒径が上限を上回るものであり、No.13は、FeとOの含有量が共に下限未満のものである。 In contrast, no. No. 8 has an Fe content exceeding the upper limit. No. 9 has an O content exceeding the upper limit. No. 10 has a rolling reduction per pass of the ingot rolling lower than the lower limit, No. 10 No. 11 has a cold rolling final cold rolling rate lower than the lower limit. No. 12 is the one in which the average crystal grain size of the crystal grains (α phase) exceeds the upper limit. No. 13 has both Fe and O contents less than the lower limit.
No.1〜7は、圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率という本発明で規定する要件も全て満足している。その結果、0.2%耐力(YS)は全て200MPa以上であり、プレス成形性の試験結果も○或いは◎で、孔拡げ率(伸びフランジ性)も90%以上である。すなわち、No.1〜7のチタン板は、高耐力でプレス成形性に優れたうえに、伸びフランジ性にも優れたチタン板であるということができる。
No. 1-7 are crystal grains having a {11-22} <11-23> twinning deformation Schmid factor of 0.47 or more and a c-axis angle of 70-90 ° with respect to the rolling direction when tensile in the rolling direction. All the requirements defined by the present invention, ie, the area ratio occupied by are satisfied. As a result, the 0.2% proof stress (YS) is all 200 MPa or more, the test result of press formability is also ◯ or ◎, and the hole expansion rate (stretch flangeability) is 90% or more. That is, no. It can be said that the
一方、No.9〜11、13は、0.2%耐力(YS)、プレス成形性、孔拡げ率のいずれか一つ以上で合格判定基準を満足しない結果となった。また、No.12は、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率が上限を超える結果となり、V字形頂点部に肌荒れが認められた。すなわち、本発明で規定する要件から外れるチタン板は、高耐力でプレス成形性に優れたうえに、伸びフランジ性にも優れたチタン板とはいえないことが分かる。 On the other hand, no. Nos. 9 to 11 and 13 did not satisfy the acceptance criteria with any one or more of 0.2% proof stress (YS), press formability, and hole expansion ratio. No. In No. 12, the area ratio occupied by the crystal grains having the c-axis angle of 70 to 90 ° with respect to the rolling direction exceeded the upper limit, and rough skin was observed at the V-shaped apex. That is, it can be seen that a titanium plate that deviates from the requirements defined in the present invention cannot be said to be a titanium plate that has high yield strength and excellent press formability and excellent stretch flangeability.
Claims (2)
1/4t(tは板厚)部の圧延面における圧延方向引張時の{11−22}<11−23>双晶変形のシュミット因子が0.47以上の面積率が、30%以上であると共に、
1/4t(tは板厚)部の1mm×1mmの平面内に存在する全結晶粒(α相)のうち、圧延方向に対するc軸の角度が70〜90°の結晶粒が占める面積率が90%以下であることを特徴とするプレス成形性に優れたチタン板。 In mass%, Fe is contained in 0.04 to 0.10%, O is contained in 0.07 to 0.20%, and the balance is Ti and inevitable impurities,
The area ratio of {11-22} <11-23> twin deformation with a Schmid factor of 0.47 or more at the time of rolling in the rolling direction of the 1/4 t (t is the plate thickness) portion is 30% or more. With
Of all the crystal grains (α phase) existing in a 1 mm × 1 mm plane of a 1/4 t (t is the plate thickness) portion, the area ratio occupied by the crystal grains whose c-axis angle with respect to the rolling direction is 70 to 90 ° A titanium plate excellent in press formability, characterized by being 90% or less.
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