JP4886514B2 - Nickel-based semi-finished product having a cubic recrystallized texture, its production method and use - Google Patents
Nickel-based semi-finished product having a cubic recrystallized texture, its production method and use Download PDFInfo
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- JP4886514B2 JP4886514B2 JP2006525826A JP2006525826A JP4886514B2 JP 4886514 B2 JP4886514 B2 JP 4886514B2 JP 2006525826 A JP2006525826 A JP 2006525826A JP 2006525826 A JP2006525826 A JP 2006525826A JP 4886514 B2 JP4886514 B2 JP 4886514B2
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- 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
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
Description
本発明は、立方体再結晶集合組織を有するニッケル系の半製品及びその製造方法に関する。 The present invention relates to a nickel-based semi-finished product having a cubic recrystallization texture and a method for producing the same.
この半製品は、例えば高度に微細構造の配向を有する物理化学的被覆用の基材として使用可能である。このような基材は、例えば高温超電導の分野で使用されるようなセラミック被覆用の支持体として適している。この使用は、この場合、超伝導磁石、変圧器、モーター、断層撮影装置又は超伝導電流路において行われる。 This semi-finished product can be used, for example, as a substrate for physicochemical coating with a highly microstructured orientation. Such a substrate is suitable as a support for ceramic coatings, such as those used in the field of high temperature superconductivity. This use takes place in this case in superconducting magnets, transformers, motors, tomography devices or superconducting current paths.
面心立方格子を有する多結晶金属、例えばニッケル、銅及びアルミニウムは、予め圧延によって著しく冷間加工された後に、後続する再結晶時に立方体層（Wuerfellage）を有する特徴的な集合組織を形成することができることは公知である（G. Wassermann著：Texturen metallischer Werkstoffe, Springer, Berlin, 1939）。このように集合組織形成された金属ベルト、特にニッケルベルトは、金属被覆、セラミック緩衝層及びセラミック超伝導層用の基材としても使用される（US 5,741, 377）。支持体材料としてのこのような金属ベルトの適性は、集合組織形成の達成可能な程度及び被覆方法を作業する温度の範囲内での前記集合組織の安定性に決定的に依存する。 Polycrystalline metals with face-centered cubic lattice, such as nickel, copper and aluminum, form a characteristic texture with a cubic layer (Wuerfellage) upon subsequent recrystallization after being significantly cold worked beforehand by rolling. (G. Wassermann: Texturen metallischer Werkstoffe, Springer, Berlin, 1939). The metal belts, in particular nickel belts, that are textured in this way are also used as substrates for metal coatings, ceramic buffer layers and ceramic superconducting layers (US 5,741, 377). The suitability of such a metal belt as a support material depends critically on the achievable degree of texture formation and the stability of the texture within the temperature range at which the coating process is operated.
Ｎｉ−Ｃｒ、Ｎｉ−Ｃｒ−Ｖ、Ｎｉ−Ｃｕ及び類似の合金からなる高温超電導体を製造するための既に集合組織形成された半製品は公知である（US 5,964, 966; US 6,106, 615）。 Already textured semi-finished products for producing high temperature superconductors made of Ni-Cr, Ni-Cr-V, Ni-Cu and similar alloys are known (US 5,964, 966; US 6,106, 615). .
この目的のためにＭｏ及びＷを有するＮｉ合金も公知である（DE 100 05 861 C1）
この公知の半製品は次の欠点を有する：
− ニッケルは冷間加工及び焼き鈍しによる再結晶化の後に、粗大な結晶粒構造を形成する傾向が強く、前記の粗大な結晶粒構造は高度な立方体集合組織の達成に不利である、
− 冷間加工されたＮｉ−ベルトは、特に高温（８００〜１１５０℃）での熱処理による再結晶化の際に粒界溝を形成する傾向が強い、
− 前記粒界溝は高度な二軸の立方体集合組織の形成を著しく阻害する、
− 粒界溝を有する支持体材料は、エピタキシャル層析出のための、例えば緩衝層及び超伝導層のための基材としてあまり適していない。
Ni alloys with Mo and W are also known for this purpose (DE 100 05 861 C1).
This known semi-finished product has the following disadvantages:
-Nickel has a strong tendency to form a coarse grain structure after recrystallization by cold working and annealing, which is disadvantageous for achieving a high cubic texture;
-Cold-worked Ni-belts have a strong tendency to form intergranular grooves, especially during recrystallization by heat treatment at high temperatures (800-1150 ° C),
-The grain boundary grooves significantly inhibit the formation of a highly biaxial cubic texture;
-Support materials with intergranular grooves are not very suitable as substrates for epitaxial layer deposition, for example for buffer layers and superconducting layers.
本発明の根底をなす課題は、高度に微細構造の配向を有する物理化学的被覆用の基材として使用するための改善された使用特性を有するニッケル系の半製品を開発することであった。特に、前記半製品は、高度でかつ熱安定性の立方体集合組織を有するのが好ましくかつ粒界溝の形成は十分に抑制されるのが好ましい。前記の課題中には、前記半製品の製造方法の開発も含まれる。 The problem underlying the present invention was to develop a nickel-based semi-finished product with improved use characteristics for use as a substrate for physicochemical coatings having a highly microstructured orientation. In particular, the semi-finished product preferably has an advanced and heat-stable cubic texture, and the formation of grain boundary grooves is preferably sufficiently suppressed. The above-mentioned problems include development of a method for manufacturing the semi-finished product.
前記課題は、半製品の材料がマイクロアロイの範囲内でＡｇ添加物を含有し、Ａｇ添加物が最大で０．３Ａｔｏｍ％であることにより解決される。 This problem is solved by the fact that the semi-finished material contains an Ag additive in the range of microalloy and the Ag additive is at most 0.3 Atom%.
本発明の有利な実施態様の場合には、前記Ｎｉ合金は合金元素としてＭｏ及び／又はＷを含有することができる。 In a preferred embodiment of the invention, the Ni alloy can contain Mo and / or W as alloying elements.
前記半製品上には、本発明により、＞９０％の集合組織割合を有する、立方体集合組織形成されたＮｉＯ層が存在することができる。この層は拡散バリアとして適していて、特に酸化条件下で質的に高い価値の被覆の製造を可能にする。 On the semi-finished product, according to the present invention, there can be a NiO layer formed with a cubic texture having a texture ratio of> 90%. This layer is suitable as a diffusion barrier and enables the production of qualitatively high value coatings, especially under oxidizing conditions.
本発明によるＡｇ添加物を用いて、高度な立方体集合組織の形成は促進されかつ半製品のＮｉ表面上での粒界溝の熱による形成は抑制される。更に、Ａｇ添加物は、半製品上に高度な立方体集合組織を備えたＮｉＯ層を成長させることを可能にする。 With the Ag additive according to the present invention, the formation of a high degree of cubic texture is promoted and the formation of grain boundary grooves on the Ni surface of the semi-finished product is suppressed. Furthermore, the Ag additive makes it possible to grow NiO layers with a high cubic texture on the semi-finished product.
本発明による半製品の製造方法は、まず、機械的合金を含めた溶融冶金的又は粉末冶金的な方法で、最大で０．３Ａｔｏｍ％のマイクロアロイの範囲内でＡｇ添加物を含有している工業的純度のＮｉ又はＮｉ合金からなる半製品を製造することを特徴とする。その後で、この半製品は熱間加工し、引き続き高度な冷間加工により＞８０％の厚さの減少率でベルト又は平面ワイヤに加工される。最後に、この半製品を焼き鈍して再結晶させて立方体集合組織を達成する。 The method for producing a semi-finished product according to the present invention is first a melt metallurgical or powder metallurgical method including a mechanical alloy, and contains an Ag additive within a range of a maximum of 0.3 Atom% microalloy. A semi-finished product made of industrially pure Ni or Ni alloy is produced. This semi-finished product is then hot worked and subsequently processed into belts or planar wires with a thickness reduction of> 80% by advanced cold working. Finally, the semi-finished product is annealed and recrystallized to achieve a cubic texture.
この再結晶させる焼き鈍しの後又はその間に、こうして製造された半製品は、本発明の場合に立方体集合組織形成されたＮｉＯ層を成長させる目的で酸化性の雰囲気中で熱処理することができる。 After or during this recrystallization annealing, the semi-finished product thus produced can be heat-treated in an oxidizing atmosphere for the purpose of growing a NiO layer having a cubic texture in the present invention.
前記半製品は、本発明の場合に、高度な微細構造の配向を有する物理化学的被覆用の基材として、特にワイヤ状の又はベルト状の高温超電導体の製造のために使用することができる。 Said semi-finished products can be used in the case of the present invention as a substrate for physicochemical coating with a high microstructure orientation, in particular for the production of wire-like or belt-like high-temperature superconductors. .
本発明を、次に本発明の成果のある試験を示す実施例を用いて更に詳説する。この試験結果の一部を図１及び２及び下記の表１に示す。 The invention will now be described in further detail with reference to examples illustrating the successful testing of the invention. Some of the test results are shown in FIGS. 1 and 2 and Table 1 below.
実施例１
Ｎｉ純度９９．９Ａｔｏｍ％の工業的純度のニッケルを、銀０．０１Ａｔｏｍ％を合金して金型に注ぎ込んだ。インゴットを１０００℃で四角形寸法（２２×２２）ｍｍ２の寸法に圧延し、均質に焼き鈍し、急冷した。引き続き、この四角形材料を切削により仕上げ加工して、圧延による引き続く冷間加工のために無欠陥の表面を得た。この冷間加工は、８０％を越えて厚さを減少させる圧下率で実施され、この場合９９．６％で実施される。生じるニッケルベルトは、８０μｍの厚さを有し、かつ高度に圧延により集合組織形成されていた。その後に、５５０℃で酸化しないガス雰囲気中で３０分間の焼き鈍し処理を行った。
Example 1
Nickel with an industrial purity of Ni purity 99.9 Atom% was poured into a mold after alloying 0.01 Atom% of silver. The ingot was rolled at 1000 ° C. to a square dimension (22 × 22) mm 2 , annealed homogeneously and quenched. Subsequently, this square material was finished by cutting to obtain a defect-free surface for subsequent cold working by rolling. This cold working is performed at a reduction rate that reduces the thickness by more than 80%, in this case 99.6%. The resulting nickel belt had a thickness of 80 μm and was highly textured by rolling. Thereafter, annealing was performed for 30 minutes in a gas atmosphere that was not oxidized at 550 ° C.
この結果は、図１による写真からも明らかなように、極めて鋭い再結晶集合組織であった。立方体層を有するクリスタリットの割合は９８％であり、小角度粒界の割合は同様に９８％であった。Ｘ線回折の場合の（１１１）極の強度の半値幅はＦＷＨＭ＝４．４°であった。 This result was an extremely sharp recrystallized texture, as is apparent from the photograph according to FIG. The proportion of crystallite having a cubic layer was 98% and the proportion of small angle grain boundaries was 98% as well. The half width of the intensity of the (111) pole in the case of X-ray diffraction was FWHM = 4.4 °.
実施例２
Ｎｉ純度９９．９Ａｔｏｍ％の工業的純度のニッケルを、銀０．０１Ａｔｏｍ％を合金して真空誘導炉中で融解させて、金型に注ぎ込んだ。インゴットを１０００℃で四角形寸法（２２×２２）ｍｍ２の寸法に圧延し、均質に焼き鈍し、急冷した。引き続き、この四角形材料を切削により仕上げ加工して、圧延による引き続く冷間加工のために無欠陥の表面を得た。この冷間加工を、８０％を越えて厚さを減少させる圧下率で実施し、この場合９９．６％で実施した。生じるニッケルベルトは、８０μｍの厚さを有し、かつ高度に圧延により集合組織形成されていた。その後に、５５０℃で還元性のガス雰囲気中で３０分間の焼き鈍し処理を行った。
Example 2
Nickel having an industrial purity of Ni purity 99.9 Atom% was alloyed with 0.01 Atom% silver, melted in a vacuum induction furnace, and poured into a mold. The ingot was rolled at 1000 ° C. to a square dimension (22 × 22) mm 2 , annealed homogeneously and quenched. Subsequently, this square material was finished by cutting to obtain a defect-free surface for subsequent cold working by rolling. This cold working was carried out at a reduction rate that reduced the thickness by more than 80%, in this case 99.6%. The resulting nickel belt had a thickness of 80 μm and was highly textured by rolling. Thereafter, annealing was performed at 550 ° C. in a reducing gas atmosphere for 30 minutes.
この結果はほとんど完全な立方体再結晶集合組織であった。引き続き、このベルトを純粋な酸素ガス中で１１５０℃で５分間の酸化を行った。 The result was almost a complete cubic recrystallization texture. Subsequently, this belt was oxidized in pure oxygen gas at 1150 ° C. for 5 minutes.
生じたニッケル酸化物層は立方体集合組織を有し、その際、結晶粒の９７％は立方体層を有していた。この集合組織はニッケルベルトの集合組織に対して４５°回転していた（図２参照）。（１１１）極のこのＦＷＨＭ値は６．２°であった。 The resulting nickel oxide layer had a cubic texture, with 97% of the grains having a cubic layer. This texture was rotated by 45 ° with respect to the texture of the nickel belt (see FIG. 2). This FWHM value of the (111) pole was 6.2 °.
実施例３
工業的純度のニッケルを、銀０．１％を合金して融解させ、金型に注ぎ込んだ。インゴットを１１００℃で四角形寸法（２２×２２）ｍｍ２の寸法に圧延し、均質に焼き鈍し、急冷した。引き続き、この四角形材料を切削により仕上げ加工して、圧延による引き続く冷間加工のために無欠陥の表面を得た。この冷間圧延を、８５％の厚さ減少の圧下率で実施した。生じたニッケルベルトは３ｍｍの厚さを有し、引き続き８５０℃で３０分間の焼き鈍し処理を行って再結晶させた。その後、この表面を清浄化し、このベルトを８０μｍの厚さに冷間加工した。引き続き、８５０℃で４５分間、還元性の雰囲気中で焼き鈍して立方体集合組織を作成した。
Example 3
Industrial purity nickel was melted by alloying with 0.1% silver and poured into a mold. The ingot was rolled at 1100 ° C. to a square dimension (22 × 22) mm 2 , annealed homogeneously and quenched. Subsequently, this square material was finished by cutting to obtain a defect-free surface for subsequent cold working by rolling. This cold rolling was performed at a reduction rate of 85% thickness reduction. The resulting nickel belt had a thickness of 3 mm and was subsequently recrystallized by annealing at 850 ° C. for 30 minutes. The surface was then cleaned and the belt was cold worked to a thickness of 80 μm. Subsequently, a cube texture was prepared by annealing in a reducing atmosphere at 850 ° C. for 45 minutes.
実施例４
工業的純度のニッケル粉末を、タングステン粉末４．０Ａｔｏｍ％及び銀粉末０．１Ａｔｏｍ％の添加下で粉末冶金的に加工した。この場合、プレス成形、熱処理、熱間加工の後に、（１２×１２）ｍｍ２の棒材が得られた。この表面を切削により仕上げ加工して、圧延による引き続く冷間加工のために無欠陥の表面を得た。この冷間圧延は（１０×１０）ｍｍ２の寸法から出発して厚さ８０μｍの仕上がり寸法になるまで実施した。前記ベルトの縁部領域を除去して廃棄した。この得られたニッケルベルトを、引き続きまず５５０℃で還元性の雰囲気中で３０分間焼き鈍し処理を行って再結晶させた。その後、このベルトを還元性の雰囲気中で１１００℃で８分間の第２の焼き鈍しで処理して、熱的に高負荷可能な立方体層を調節した。
Example 4
Industrial purity nickel powder was processed powder metallurgically with the addition of 4.0 Atom% tungsten powder and 0.1 Atom% silver powder. In this case, a bar of (12 × 12) mm 2 was obtained after press molding, heat treatment and hot working. This surface was finished by cutting to obtain a defect-free surface for subsequent cold working by rolling. This cold rolling was carried out starting from a dimension of (10 × 10) mm 2 until a finished dimension of 80 μm thickness was obtained. The belt edge area was removed and discarded. The obtained nickel belt was first annealed at 550 ° C. in a reducing atmosphere for 30 minutes and recrystallized. Thereafter, this belt was treated in a reducing atmosphere at a second annealing at 1100 ° C. for 8 minutes to adjust a cubic layer capable of being thermally highly loaded.
次に記載する表１は、番号５及び６の支持体の値で、ＦＷＨＭ（１１１）値に関して先行技術（支持体番号１〜４）と比較して本発明によるＡｇ添加の有利な影響を示した。
Table 1 described below shows the beneficial effects of Ag addition according to the present invention compared to the prior art (
Claims (5)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10342965A DE10342965A1 (en) | 2003-09-10 | 2003-09-10 | Nickel-based semifinished product with a recrystallization cube texture and process for its production |
| DE10342965.4 | 2003-09-10 | ||
| PCT/EP2004/052083 WO2005024077A1 (en) | 2003-09-10 | 2004-09-08 | Nickel-based semifinished product having a cube recrystallization texture, corresponding method of production and use |
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| Publication Number | Publication Date |
|---|---|
| JP2007505215A JP2007505215A (en) | 2007-03-08 |
| JP4886514B2 true JP4886514B2 (en) | 2012-02-29 |
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| JP2006525826A Expired - Fee Related JP4886514B2 (en) | 2003-09-10 | 2004-09-08 | Nickel-based semi-finished product having a cubic recrystallized texture, its production method and use |
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| Country | Link |
|---|---|
| US (1) | US20070062613A1 (en) |
| EP (1) | EP1664361A1 (en) |
| JP (1) | JP4886514B2 (en) |
| KR (1) | KR101231936B1 (en) |
| CN (1) | CN100523238C (en) |
| DE (1) | DE10342965A1 (en) |
| WO (1) | WO2005024077A1 (en) |
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| DE102004060900A1 (en) * | 2004-12-14 | 2006-06-29 | Leibniz-Institut Für Festkörper- Und Werkstoffforschung Dresden E.V. | Nickel-based semi-finished product with cube texture and process for its production |
| DE102005013368B3 (en) * | 2005-03-16 | 2006-04-13 | Leibniz-Institut Für Festkörper- Und Werkstoffforschung Dresden E.V. | Making nickel-based blank with cubic recrystallization structure for use as backing for high temperature superconductor, employs silver micro-alloying and specified thermal and mechanical treatments |
| KR100691061B1 (en) * | 2005-08-30 | 2007-03-09 | 엘에스전선 주식회사 | Substrate for superconducting wire and fabrication method thereof and superconducting wire |
| JP5330725B2 (en) * | 2008-03-31 | 2013-10-30 | 古河電気工業株式会社 | Superconducting wire substrate and manufacturing method thereof |
| DE102008001005B4 (en) | 2008-04-04 | 2011-06-22 | Karlsruher Institut für Technologie, 76131 | A method for producing a composite layer with epitaxially grown layers of a magnetic shape memory material and composite layer with epitaxial layers of a magnetic shape memory material and its use |
| CN103194704B (en) * | 2013-04-18 | 2015-04-08 | 重庆大学 | Preparation method of low-cost nickel baseband with high cube texture content |
| CN105209188B (en) | 2013-06-07 | 2017-10-13 | Vdm金属有限公司 | The method for preparing metal foil |
| JP6388925B2 (en) | 2013-06-07 | 2018-09-12 | ファオデーエム メタルズ ゲゼルシャフト ミット ベシュレンクテル ハフツングＶＤＭ Ｍｅｔａｌｓ ＧｍｂＨ | Metal foil manufacturing method |
| CN105220017A (en) * | 2015-11-13 | 2016-01-06 | 无锡清杨机械制造有限公司 | A kind of nickel alloy wire and production method thereof |
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| US2570355A (en) * | 1949-04-09 | 1951-10-09 | Low Sidney | Metal alloy |
| US5584908A (en) * | 1994-11-14 | 1996-12-17 | Sherritt Inc. | Micron-sized nickel metal powder and a process for the preparation thereof |
| US5741377A (en) * | 1995-04-10 | 1998-04-21 | Martin Marietta Energy Systems, Inc. | Structures having enhanced biaxial texture and method of fabricating same |
| US5964966A (en) * | 1997-09-19 | 1999-10-12 | Lockheed Martin Energy Research Corporation | Method of forming biaxially textured alloy substrates and devices thereon |
| US6120624A (en) * | 1998-06-30 | 2000-09-19 | Howmet Research Corporation | Nickel base superalloy preweld heat treatment |
| DE10005861C2 (en) * | 1999-04-03 | 2002-05-08 | Dresden Ev Inst Festkoerper | Nickel-based metallic material and process for its production |
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2003
- 2003-09-10 DE DE10342965A patent/DE10342965A1/en not_active Withdrawn
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2004
- 2004-09-08 JP JP2006525826A patent/JP4886514B2/en not_active Expired - Fee Related
- 2004-09-08 US US10/571,245 patent/US20070062613A1/en not_active Abandoned
- 2004-09-08 EP EP04787109A patent/EP1664361A1/en not_active Withdrawn
- 2004-09-08 CN CNB2004800259519A patent/CN100523238C/en not_active Expired - Fee Related
- 2004-09-08 KR KR1020067004924A patent/KR101231936B1/en not_active IP Right Cessation
- 2004-09-08 WO PCT/EP2004/052083 patent/WO2005024077A1/en active Application Filing
Also Published As
| Publication number | Publication date |
|---|---|
| KR101231936B1 (en) | 2013-02-08 |
| KR20060119955A (en) | 2006-11-24 |
| EP1664361A1 (en) | 2006-06-07 |
| CN1849403A (en) | 2006-10-18 |
| WO2005024077A1 (en) | 2005-03-17 |
| WO2005024077B1 (en) | 2005-08-25 |
| US20070062613A1 (en) | 2007-03-22 |
| DE10342965A1 (en) | 2005-06-02 |
| JP2007505215A (en) | 2007-03-08 |
| CN100523238C (en) | 2009-08-05 |
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