JPH0347930A - Production of nb-ti alloy - Google Patents
Production of nb-ti alloyInfo
- Publication number
- JPH0347930A JPH0347930A JP1182235A JP18223589A JPH0347930A JP H0347930 A JPH0347930 A JP H0347930A JP 1182235 A JP1182235 A JP 1182235A JP 18223589 A JP18223589 A JP 18223589A JP H0347930 A JPH0347930 A JP H0347930A
- Authority
- JP
- Japan
- Prior art keywords
- mixture
- semi
- molten
- alloy
- semimolten
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 229910001069 Ti alloy Inorganic materials 0.000 title description 2
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 21
- 239000000956 alloy Substances 0.000 claims abstract description 21
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000007711 solidification Methods 0.000 claims abstract description 3
- 230000008023 solidification Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 19
- 239000010936 titanium Substances 0.000 claims description 14
- 229910020012 Nb—Ti Inorganic materials 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 8
- 239000010955 niobium Substances 0.000 claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 3
- 239000012768 molten material Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 8
- 230000006698 induction Effects 0.000 abstract description 7
- 238000005204 segregation Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 10
- 238000010894 electron beam technology Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野］ 本発明はＮ ｂ −Ｔ ｉ系合金の製造方法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for manufacturing an Nb-Ti alloy.
Ｃ従来の技術〕
従来、超電導材料などとして利用されるＮｂＴｉ系合金
のインゴントは、以下のような方法により製造されてい
る。すなわち、
イ）第２図に示すように、細いニオブ棒と細いチタン棒
を所望組成比、例えば、５Ｑｗｔ％： ５０１１ｔ％に
なるように束ねて混合体（１）を構成し、この混合体（
１）と水冷鋳型（２）を真空容器（３）中にセツトシ、
電源（４）を操作して混合体（１）と水冷鋳型（２）と
の間でアク（５）を発生させ、その熱で混合体（１）を
溶融して形成された合金ドロップ（６）を水冷鋳型（２
）中のプール部（７）に落下させ、凝固させて合金イン
ゴット（８）を形成するアーク溶解法。C. Prior Art Conventionally, ingons of NbTi-based alloys used as superconducting materials have been manufactured by the following method. That is, a) As shown in Fig. 2, thin niobium rods and thin titanium rods are bundled in a desired composition ratio, for example, 5Qwt%: 5011t% to form a mixture (1), and this mixture (
Set 1) and water-cooled mold (2) in a vacuum container (3),
The power source (4) is operated to generate scum (5) between the mixture (1) and the water-cooled mold (2), and the heat melts the mixture (1) to form an alloy drop (6). ) into a water-cooled mold (2
) into a pool (7) and solidified to form an alloy ingot (8).
口）上述の混合体に電子ビームを照射し、その熱で混合
体を溶融して形成された合金ドロップを水冷鋳型中のプ
ール部に落下させ、凝固させて合金インゴットを形成す
る電子ビーム溶解法。(1) An electron beam melting method in which the above-mentioned mixture is irradiated with an electron beam and the mixture is melted by the heat, and the formed alloy drop is dropped into a pool in a water-cooled mold and solidified to form an alloy ingot. .
ハ）ニオブ粉とチクンわ）より圧縮混合体を形成し、真
空容器中で加熱圧縮し、冷却して合金インゴ・ノドを形
成する粉末法。c) A powder method in which a compressed mixture is formed from niobium powder and chikunwa), heated and compressed in a vacuum container, and cooled to form an alloy ingot.
しかしながら、上述のＮｂ−Ｔｉ系合金の製造方法には
次のような問題点があった。すなわら、イ）アーク溶解
法では、プール部の鋳型近傍と中央部間に大きな温度勾
配が生しるため、Ｔｉが偏析し、インゴット外周部では
Ｔｉ温度が高く、結晶粒が大きくなる。However, the above-mentioned method for manufacturing the Nb-Ti alloy has the following problems. In other words, (a) in the arc melting method, a large temperature gradient occurs between the vicinity of the mold and the center of the pool, so Ti segregates, and the Ti temperature is high at the outer periphery of the ingot, resulting in large crystal grains.
口）電子ビーム溶解法では、高真空を動作要件とするた
め、Ｔｉの歩留りが悪く、またプール部の温度勾配によ
りインゴット外周部ではＴｉｆｉ度が高く、結晶粒が大
きくなる。In the electron beam melting method, since a high vacuum is required for operation, the yield of Ti is poor, and the Tifi degree is high in the outer peripheral part of the ingot due to the temperature gradient in the pool part, resulting in large crystal grains.
ハ）粉末法では、Ｔｉ濃度に大きな変動は生しないが、
ボイドが多く、結晶粒については、混粒や粗大粒が多く
なる。C) Although the powder method does not cause large fluctuations in Ti concentration,
There are many voids, and the crystal grains include many mixed grains and coarse grains.
本発明は上記問題点を解決したＮｂ−Ｔｉ系合金の製造
方法を提供するもので、少なくとも純ニオブと純チタン
の二種類の原料を混合して混合体を形成する工程と、該
混合体を圧縮して圧縮体を形成する工程と、該圧縮体を
加熱してその一部分を半溶融体とし、該半溶融体部と非
半溶融体部とを相対的に回転させる工程と、前記半溶融
体部を圧縮体中で移動させ、冷却し凝固させる工程とを
有することを第１発明とし、半溶融体部と非半溶融体部
の相対的回転速度が１１００ｒｐ以上であることを第２
発明とし、半溶融体部の凝固速度が１℃／ｍｉｎ以上で
あることを第３発明とするものである。The present invention provides a method for producing a Nb-Ti alloy that solves the above-mentioned problems, and includes at least a step of mixing two types of raw materials, pure niobium and pure titanium, to form a mixture; a step of compressing to form a compressed body; a step of heating the compressed body to make a part of it into a semi-molten body; and a step of relatively rotating the semi-molten body part and the non-semi-molten body part; The first invention includes a step of moving the body part in a compressed body, cooling and solidifying the body part, and the second invention is that the relative rotational speed of the semi-molten body part and the non-semi-molten body part is 1100 rpm or more.
A third aspect of the present invention is that the solidification rate of the semi-molten portion is 1° C./min or more.
本発明は最近開発された半凝固加工法を応用したもので
ある。半凝固加工法は、溶融状態の金属と固体化した金
属が共存した状態で、機械的に強力にかくはんすること
により、生成する樹枝状晶を破壊して金属の粒子と液体
が混在するスラリーを造り、それを成形加工する方法で
ある。半凝固加工法により製造された合金は、偏析など
の欠陥がなく、結晶粒が微細化しているという特徴があ
る。The present invention applies a recently developed semi-solid processing method. In the semi-solid processing method, molten metal and solidified metal coexist and are mechanically stirred strongly to destroy the generated dendrites and create a slurry containing a mixture of metal particles and liquid. It is a method of making and molding it. Alloys manufactured using the semi-solid processing method are free from defects such as segregation and have fine grains.
上述のように、純ニオブと純チタンを混合して形成され
た圧縮体を加熱して部分的に半溶融体とし、半溶融体部
と非半溶融体部を相対的に回転させると、ＮｂＴｉのス
ラリーが作られる。この際に、回転速度を１１００ｒｐ
以上にすると結晶粒を１胴以下に微細化することができ
る。また、半溶融体部を移動させ、冷却する際に、冷却
速度をビＣ／ｍｉｎ以上にすることにより、さらに結晶
粒を微細化することができる。この冷却速度を下部ると
粒は粗大化するが偏析は少ない状態となる。しかし結晶
粒の粗大化は後の加工性を阻害するため好ましくない。As mentioned above, when a compressed body formed by mixing pure niobium and pure titanium is heated to partially become a semi-molten body, and the semi-molten body part and the non-semi-molten body part are relatively rotated, NbTi slurry is made. At this time, increase the rotation speed to 1100 rpm.
If the amount is above, the crystal grains can be made finer than one grain. In addition, when moving and cooling the semi-molten material, the crystal grains can be further refined by setting the cooling rate to at least BiC/min. When the cooling rate is lowered, the grains become coarser, but there is less segregation. However, coarsening of crystal grains is not preferable because it impairs subsequent workability.
以下、図面に示した実施例に基づいて本発明を説明する
。The present invention will be described below based on embodiments shown in the drawings.
第１図は本発明にがかる一実施例の説明図であり、真空
容器（１３）中に混合体（１１）が、上端を回転軸（１
２’）に固定し下端を回転方向が逆の回転軸（１２）に
連結してセットされている。この混合体（１１）は、２
００メツシユのニオブとスポンジチタンをＮ ｂ−４６
，５ｗｔ％Ｔｉになるように配合し、直径１００ＩＩＩ
ＩＩｌφの円柱状に圧縮して冷間成型し、次いで、７
ｔｏｎＯ熱間静水圧機中で１６５０°Ｃ，１０分間保持
後冷却し、大気中に取出したものである。真空容器（１
３）中にセットされた混合体（１１）の周囲には固定し
た誘導コイル（１４）が配置されている。この誘導コイ
ル（１４）に通電し、誘導コイル（１４）近傍の混合体
（１１）を１９８９°Ｃになるまで加熱して半溶融体と
し、上部回転軸（１２’）を回転し、下部の回転軸（１
２）を逆方向に１ ｒｐｎ＋で回転させる。誘導コイル
（１４）と、半溶融体部（１５）は一定位置に保たれ凝
固した合金が水冷管（１６）により冷却されて下方に引
き下げられる。FIG. 1 is an explanatory diagram of an embodiment according to the present invention, in which a mixture (11) is placed in a vacuum container (13) with its upper end connected to a rotating shaft (1).
2'), and the lower end is connected to a rotating shaft (12) whose rotation direction is opposite. This mixture (11) has 2
00 mesh niobium and sponge titanium Nb-46
, 5 wt% Ti, diameter 100III
Compressed and cold-molded into a cylinder of IIlφ, then 7
After being held at 1650°C for 10 minutes in a tonO hot isostatic pressure machine, it was cooled and taken out into the atmosphere. Vacuum container (1
3) A fixed induction coil (14) is placed around the mixture (11) set in the container. The induction coil (14) is energized, the mixture (11) near the induction coil (14) is heated to 1989°C to form a semi-molten substance, the upper rotating shaft (12') is rotated, and the lower Rotating axis (1
2) is rotated in the opposite direction at 1 rpn+. The induction coil (14) and the semi-molten body part (15) are kept at a fixed position, and the solidified alloy is cooled by the water-cooled tube (16) and pulled downward.
以上のようにして製造されたＮｂ−Ｔｉ合金インゴット
試料と、従来のアーク溶解法および熱間静水圧処理を３
時間施した粉末法により製造されたインゴット試料につ
いて、その検査結果を第１表に示す。The Nb-Ti alloy ingot sample produced as described above was subjected to conventional arc melting method and hot isostatic pressure treatment.
Table 1 shows the test results for the ingot samples produced by the powder method that were subjected to the test.
この結果より、本実施例の試料のＴｉ濃度は外周部と中
央部では七んと変わらず、偏析が生しておらず、従来の
アーク法および粉末法より改善されていることがわかる
。また、結晶粒の大きさについては、本実施例において
回転速度を１ｏＯｒｐｒｎ以上、冷却速度を１℃／ｍｉ
ｎ以上にすることにより、結晶粒の大きさは１＋ｎｍ以
下となり、回転速度および冷却速度を上げるほど結晶粒
が小さくなることがわかる。さらに、アーク法および粉
末法ではボイド′が発生するが、本実施例ではボイドが
見出されなかった。From this result, it can be seen that the Ti concentration of the sample of this example is the same at 7 between the outer periphery and the center, no segregation occurs, and is improved over the conventional arc method and powder method. Regarding the size of crystal grains, in this example, the rotation speed was set to 1 oOrprn or more, and the cooling rate was set to 1°C/mi.
It can be seen that by setting the value to be n or more, the size of the crystal grains becomes 1+nm or less, and the crystal grains become smaller as the rotation speed and cooling rate are increased. Furthermore, although voids occur in the arc method and the powder method, no voids were found in this example.
次に、他の実施例として、Ｎｂ ３１１ｔ％Ｔｉにな
るように配合した混合体を用い、他は前記実施例と同一
条件で製造したＮｂ−Ｔｉ合金インゴット試料について
、電子ビーム法および粉末法によるインゴット試料との
比較データを第２表に示す。Next, as another example, a Nb-Ti alloy ingot sample manufactured under the same conditions as in the previous example, using a mixture containing Nb 311t%Ti, was subjected to electron beam method and powder method. Comparison data with ingot samples are shown in Table 2.
第２表の結果からも、本実施例のＮｂ−Ｔｉ合金インゴ
ットは、従来の製造方法により製造されたインゴットに
比較して、Ｔｉの偏析がなくなり、結晶粒は微細化し、
ボイドはなくなるという優れた性質を示している。The results in Table 2 also show that in the Nb-Ti alloy ingot of this example, Ti segregation was eliminated and the crystal grains were refined, compared to ingots manufactured by conventional manufacturing methods.
It shows the excellent property of eliminating voids.
以上説明したように本発明によれば、純ニオブと純チタ
ンの原料を混合して圧縮体を形成し、次いで、該圧縮体
を加熱してその一部分を半溶融体とし、半溶融体部と非
半溶融体部とを相対的に回転させ、次いで、半溶融体部
を圧縮体中で移ｖＪさせ、冷却し凝固させるため、Ｔｉ
の偏析がなく、結晶粒が微細化され、ボイドのないＮｂ
−Ｔｉ合金インゴットが得られるという優れた効果があ
る。As explained above, according to the present invention, raw materials of pure niobium and pure titanium are mixed to form a compressed body, and then the compressed body is heated to make a part of it into a semi-molten body, and a semi-molten body part is formed. Ti
Nb with no segregation, fine grains, and no voids
-There is an excellent effect that a Ti alloy ingot can be obtained.
Ｎｂ−Ｔｉ系合金としてＴａ、Ｈｆ、Ｚｒなどの第３．
第４元素を添加したものにも同様に適用できるものであ
る。Third types of Nb-Ti alloys such as Ta, Hf, Zr, etc.
It can be similarly applied to those to which a fourth element is added.
第１図は本発明にかかるＮｂ−Ｔｉ系合金の製造方法の
一実施例の説明図、第２図は同製造方法の−従来例の説
明図である。
１．１１・・・混合体、 ２・・・水冷鋳型、真空容器
、 ４・・・電源、 ５−アーク、金ドロップ、 ７
・・・プール部、 ８・・・イ１２、１２’・・・回
転軸、 １４・・・誘導コイル、溶融体部、 １６・・
・水冷管。FIG. 1 is an explanatory diagram of an embodiment of the method for manufacturing an Nb-Ti alloy according to the present invention, and FIG. 2 is an explanatory diagram of a conventional example of the same manufacturing method. 1.11...Mixture, 2...Water-cooled mold, vacuum container, 4...Power source, 5-Arc, gold drop, 7
... Pool part, 8... A12, 12'... Rotating shaft, 14... Induction coil, molten body part, 16...
・Water cooling pipe.
Claims (3)
混合して混合体を形成する工程と、該混合体を圧縮して
圧縮体を形成する工程と、該圧縮体を加熱してその一部
分を半溶融体とし、該半溶融体部と非半溶融体部とを相
対的に回転させる工程と、前記半溶融体部を圧縮体中で
移動させ、冷却し凝固させる工程とを有することを特徴
とするＮｂ−Ｔｉ系合金の製造方法。(1) A step of mixing at least two types of raw materials, pure niobium and pure titanium, to form a mixture, a step of compressing the mixture to form a compressed body, and a step of heating the compressed body to form a part thereof. is a semi-molten body, the process includes a step of relatively rotating the semi-molten body part and a non-semi-molten body part, and a process of moving the semi-molten body part in a compressed body, cooling and solidifying it. A method for producing a featured Nb-Ti alloy.
００ｒｐｍ以上であることを特徴とする請求項１記載の
Ｎｂ−Ｔｉ系合金の製造方法。(2) The relative rotational speed of the semi-molten part and the non-semi-molten part is 1
2. The method for producing a Nb-Ti alloy according to claim 1, wherein the speed is 00 rpm or more.
とを特徴とする請求項１記載のＮｂ−Ｔｉ系合金の製造
方法。(3) The method for producing a Nb-Ti alloy according to claim 1, wherein the solidification rate of the semi-molten material is 1° C./min or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1182235A JP2583313B2 (en) | 1989-07-14 | 1989-07-14 | Method for producing Nb-Ti alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1182235A JP2583313B2 (en) | 1989-07-14 | 1989-07-14 | Method for producing Nb-Ti alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0347930A true JPH0347930A (en) | 1991-02-28 |
| JP2583313B2 JP2583313B2 (en) | 1997-02-19 |
Family
ID=16114709
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1182235A Expired - Lifetime JP2583313B2 (en) | 1989-07-14 | 1989-07-14 | Method for producing Nb-Ti alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2583313B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703757A (en) * | 2012-05-18 | 2012-10-03 | 宁夏东方钽业股份有限公司 | Corrosion resistant niobium-titanium alloy, and method for manufacturing plates and pipes with the same |
| CN109694136A (en) * | 2018-12-29 | 2019-04-30 | 苏州凯虹高分子科技有限公司 | A kind of scale inhibition pipe and its production technology |
-
1989
- 1989-07-14 JP JP1182235A patent/JP2583313B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703757A (en) * | 2012-05-18 | 2012-10-03 | 宁夏东方钽业股份有限公司 | Corrosion resistant niobium-titanium alloy, and method for manufacturing plates and pipes with the same |
| CN109694136A (en) * | 2018-12-29 | 2019-04-30 | 苏州凯虹高分子科技有限公司 | A kind of scale inhibition pipe and its production technology |
| CN109694136B (en) * | 2018-12-29 | 2022-05-10 | 苏州凯虹高分子科技有限公司 | Scale inhibition pipe and production process thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2583313B2 (en) | 1997-02-19 |
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