EP3572539A1 - Procédé de fabrication d'un alliage nbti - Google Patents
Procédé de fabrication d'un alliage nbti Download PDFInfo
- Publication number
- EP3572539A1 EP3572539A1 EP18173614.1A EP18173614A EP3572539A1 EP 3572539 A1 EP3572539 A1 EP 3572539A1 EP 18173614 A EP18173614 A EP 18173614A EP 3572539 A1 EP3572539 A1 EP 3572539A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- melting
- electron beam
- nbti
- alloy
- arc
- 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.)
- Withdrawn
Links
- 239000000956 alloy Substances 0.000 title claims abstract description 61
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000002844 melting Methods 0.000 claims abstract description 109
- 230000008018 melting Effects 0.000 claims abstract description 108
- 238000010894 electron beam technology Methods 0.000 claims abstract description 60
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000000365 skull melting Methods 0.000 claims abstract description 20
- 230000006698 induction Effects 0.000 claims abstract description 18
- 239000000155 melt Substances 0.000 claims abstract description 17
- 238000007711 solidification Methods 0.000 claims abstract description 13
- 230000008023 solidification Effects 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000010936 titanium Substances 0.000 claims description 62
- 239000010955 niobium Substances 0.000 claims description 45
- 229910052719 titanium Inorganic materials 0.000 claims description 17
- 229910052758 niobium Inorganic materials 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 4
- 229910001275 Niobium-titanium Inorganic materials 0.000 claims description 3
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 claims description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 10
- 238000001704 evaporation Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000001307 helium Substances 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 239000002887 superconductor Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000829 induction skull melting Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 210000003625 skull Anatomy 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
-
- 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
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
-
- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- 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
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
Definitions
- the invention relates to a method for producing a niobium-titanium alloy (NbTi alloy) from niobium (Nb) and titanium (Ti).
- NbTi alloys for use as Type II superconductors are typically made by at least three times vacuum arc melting to achieve the necessary homogeneity and quality of the alloy. Such methods are known from JP H04-131 332 A and the JP H03-281 746 A known.
- the vapor pressure of Ti is about 0.05 mbar at 1900 ° C. and about 1 mbar at 2500 ° C. This results in a loss of Ti by evaporation of the Ti in a processing of the starting metals.
- the object of the invention is therefore to overcome the disadvantages of the prior art.
- an efficient and simple and inexpensive to implement method for the production of NbTi alloys is to be found, which enables the production of superconducting NbTi wires in high quality.
- the vacuum during electron beam melting in step B) has a maximum pressure of 10-3 mbar.
- the electron beam melting takes place in a high vacuum at a pressure of at most 10-4 mbar.
- the NbTi material is completely melted by electron beam melting, thereby completely alloying the Nb and Ti homogeneously with a maximum percentage deviation of the alloy composition of not more than +/- 1.5% nominal.
- the skull melting according to step A) is preferably realized by electron beam skull melting, induction skull melting or arc-skull melting.
- the arc melting, the vacuum induction melting or the Skull melting is performed only once and the electron beam melting is performed only once.
- step A) the metallic Ti is over-alloyed with an excess of between 1% by weight and 5% by weight compared to the desired NbTi alloy.
- the weight losses can be compensated for by evaporation of Ti during electron beam melting and optionally also during arc melting, vacuum induction melting or skull melting.
- the arc melting, the vacuum induction melting or the skull melting in step A) is carried out in an inert gas, in particular in helium (He) or argon (Ar).
- the arc melting, vacuum induction melting or Skull melting in step A) is carried out at a partial pressure between 20 mbar and 300 mbar of the inert gas.
- step A) arc melting is used and that the arc melting in step A) an electrode of Nb is used and Ti is supplied as granules or sponge or an electrode of plates welded together Nb and Ti or a compressed rod of Nb coated with Ti, or a rod of Ti covered with Nb or an electrode of a compressed mixture of particulate Nb and particulate Ti.
- the electrode and optionally the granules or sponge is melted with the arc and the mixture solidifies in a cooled arc melting crucible as the at least one alloyed body, in particular the at least one rod.
- the cooled arc melting crucible is a water-cooled copper arc melting crucible.
- the at least one alloyed body in particular the at least one rod, is melted with at least one electron beam from at least one electron beam gun and the melt is collected in a cooled electron beam melting crucible and solidifies.
- the cooled electron beam melting crucible is a water-cooled copper electron beam melting crucible.
- the cooled electron beam melting crucible preferably has a lowerable bottom.
- the NbTi alloy contains between 40% by weight and 60% by weight of Ti, preferably between 45% by weight and 50% by weight of Ti.
- NbTi47 alloy is produced.
- the chosen sequence makes it possible to homogenize the at least one alloyed body, in particular the at least one rod, strongly and to homogenize the melt produced in a melting process with the large but temporally short energy input during electron beam melting.
- the resulting unavoidable Ti evaporations are compensated by a superalloy.
- the NbTi alloy solidifies in a cylindrical form.
- Such cylindrical shapes in particular rods or rods, can be processed very well, for example, in connection to pull wires.
- the cylindrical shape has a diameter between 100 mm and 500 mm. Alternatively or additionally, it may be provided that the cylindrical shape has a length between 750 mm and 4000 mm.
- Cylindrical molds of such dimensions are also very well suited for further processing, for example to subsequently produce wires or rod material from the cylindrical molds.
- the arc melting, the vacuum induction melting or the Skull melting and the solidification of the mixture after the arc melting, the vacuum induction melting or the Skull melting continuously takes place, so that continuously new material is melted and the mixture on already solidified NbTi Material is frozen.
- the electron beam melting and the solidification of the melt take place continuously after the electron beam melting, so that melt continuously generated by the electron beam melting is solidified on already solidified NbTi alloy.
- the process can be used well for larger quantities on an industrial scale, without requiring large amounts of the mixture or the melt liquid or must be kept warm. This also avoids further evaporation of Ti and thus a change in the composition of the NbTi alloy.
- NbTi alloy prepared by a method according to the invention.
- the invention is based on the surprising finding that it is possible by arc melting, vacuum induction melting or skull melting and subsequent electron beam melting to produce high-quality NbTi alloys in only a few steps, which meets the requirements for producing superconducting wires and other components , By avoiding additional steps, a cost effective NbTi alloy can be provided. Two remelting processes suffice, where up to now more remelting processes have been used. In the process control according to the invention, the amount of evaporated Ti is very accurately predictable. The known evaporating titanium amount can thus be overcompensated or weighed out beforehand, and thus the losses of the Ti can be compensated well. As a result, an NbTi alloy can be produced with a relatively accurately predictable and readily adjustable composition. The micro-element distribution of such a molten block is equal to or even more homogeneous than that of a four-time vacuum arc-melted block.
- FIG. 1 shows a schematic representation of an arc melting plant 1 in cross section, which is suitable for performing a first part of a method according to the invention.
- a vacuum induction smelting plant or a Skull smelting plant may also be used.
- the arc melting is carried out in a pressure-tight and evacuatable chamber 2.
- the process can be carried out by evacuating and purging with a noble gas such as argon or helium, and then filling with an inert gas such as helium or argon in a protective gas atmosphere.
- the first part of the process according to the invention can also be carried out in the protective gas under a partial pressure of between 20 and 300 mbar.
- An electrode 4 is attached to a holder 6, which also serves the power supply.
- the electrode 4 is made of a core of Nb with two outer layers of Ti or coaxial of a core of Nb with an outer sheath of Ti.
- the electrode 4 can also be pressed from Nb and Ti particles. It is also possible to use an Nb electrode and continuously add the Ti in particulate form via a lateral access (not shown).
- the Ti in particulate form may be present, for example, as a Ti sponge.
- an electric voltage of about 28 V is applied and an arc is drawn or generated with an electric current between 4 kA and 6 kA, the electrode 4 (and optionally the separately supplied Ti particles ) melts.
- the selected current depends on the selected geometry of the electrode. For example, for the amperage between 4 kA and 6 kA given here by way of example, the electrode 4 can have a diameter of 100 mm which matches these current intensities and the arc melting crucible 8 has a diameter of 200 mm which matches these current intensities.
- arc melting crucible 8 for example, a water-cooled copper crucible can be used. In the arc melting crucible 8, a mixture 10 of the raw materials Nb and Ti is collected. The mixture 10 solidifies at the bottom of the arc melting crucible 8 (in FIG FIG. 1 below) and forms an alloyed body 14 of NbTi material.
- the NbTi material of the alloyed body 14 may include unfused Nb clusters.
- One or more alloyed bodies 14 can be produced, which are subsequently processed further with electron beam melts.
- the alloyed body 14 has a diameter of about 200 mm and a length of about 1600 mm and weighs about 300 kg.
- FIG. 2 which shows a schematic representation of an electron beam melting system 11 in cross section
- the alloyed body 14 produced in the first part of the method according to the invention is again melted into a vacuum chamber 12 of the electron beam melting system 11.
- the vacuum chamber 12 can be evacuated via a vacuum connection 13.
- a vacuum pump (not shown) is connected to the vacuum connection 13.
- two electron guns 16 are arranged in the vacuum chamber 12, with which a conical region (referred to herein as electron beam 17) is scanned, as is the case with Brownian tubes
- the intensity of the electron beam 17 in the region of the cone can be regulated by a suitable guidance of the electron beam 17 in order to adapt the electron beam melting to the alloyed body 14.
- the alloyed body 14 is inserted laterally horizontally. Likewise, with a suitable adaptation of the electron beams 17, it is possible to introduce the alloyed body 14 vertically from above, ie vertically. Below the alloyed body 14 is disposed a cooled electron beam melting crucible 18 made of copper with lowerable bottom 19 (preferably of inherent NbTi). The alloyed body 14 is melted with the electron beams 17, and the melt 20 dripping from the alloyed body 14 falls into the Electron beam melting crucible 18, where the melt 22 is collected and continuously solidified as the desired NbTi alloy 24 while the lowerable bottom 19 is driven down. The result is a rod made of NbTi.
- the alloyed body 14 is continuously advanced and optionally further alloyed body 14 are pushed.
- the Nb clusters still contained in the alloyed body 14 are completely melted during the electron beam melting, so that a homogeneous melt 22 and thus a homogeneous NbTi alloy 24 are produced after only one melting with the electron beams 17 of the alloyed body with arc melting.
- the NbTi alloy 24 solidifies in the electron beam melting crucible 18 and is continuously drawn down to form a cylindrical body of about 305 mm in diameter, about 2200 mm in length. For this purpose, several of the alloyed bodies 14 must be melted with the electron beam melts and solidified in the electron beam melting crucible 18.
- NbTi alloy prepared by the described method has the same micro-homogeneity and element distribution quality as an NbTi alloy of the same diameter produced by four times arc melting of 20 mm.
- an NbTi alloy prepared by the above-described inventive method and a conventional NbTi alloy prepared by four times vacuum arc melting (VAR) were examined by means of a scanning electron microscope.
- VAR vacuum arc melting
- FIG. 3 shows an energy dispersive X-ray analysis (EDX) generated by the scanning electron microscope (ESM) of the NbTi alloy obtained by a method according to the invention
- FIG. 4 Energy dispersive X-ray analysis (EDX) using the Scanning Electron Microscope (ESM) generates a NbTi alloy obtained by conventional vacuum arc melting four times for comparison FIG. 3
- Nb and Ti are contained in equal amounts, that is, the ratio of the integrals of the intensities of the secondary electrons in the regions typical for Nb and Ti is the same for both samples (see Figures 3 and 4 ).
- the two NbTi alloys have the same or at least very similar compositions.
- the inventive the NbTi alloy produced in the simpler manufacturing process has the same composition and quality as the NbTi alloy produced by four-time vacuum arc melting.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture And Refinement Of Metals (AREA)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP18173614.1A EP3572539A1 (fr) | 2018-05-22 | 2018-05-22 | Procédé de fabrication d'un alliage nbti |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP18173614.1A EP3572539A1 (fr) | 2018-05-22 | 2018-05-22 | Procédé de fabrication d'un alliage nbti |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP3572539A1 true EP3572539A1 (fr) | 2019-11-27 |
Family
ID=62222518
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP18173614.1A Withdrawn EP3572539A1 (fr) | 2018-05-22 | 2018-05-22 | Procédé de fabrication d'un alliage nbti |
Country Status (1)
| Country | Link |
|---|---|
| EP (1) | EP3572539A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113322386A (zh) * | 2021-04-19 | 2021-08-31 | 西部超导材料科技股份有限公司 | 一种大规格NbTi合金铸锭的制备方法 |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3268373A (en) | 1963-05-21 | 1966-08-23 | Westinghouse Electric Corp | Superconductive alloys |
| JPS60220844A (ja) | 1984-04-17 | 1985-11-05 | Sumitomo Chem Co Ltd | 伸張試験用試験片つかみ治具 |
| DE3518855A1 (de) | 1984-05-29 | 1985-12-05 | Toho Titanium Co., Ltd., Tokio/Tokyo | Abschmelzelektrode zur herstellung von niob-titan legierungen |
| US5013357A (en) * | 1989-10-26 | 1991-05-07 | Westinghouse Electric Corp. | Direct production of niobium titanium alloy during niobium reduction |
| EP0429019A1 (fr) * | 1989-11-20 | 1991-05-29 | Nkk Corporation | ProcédÀ© de fabrication d'un alliage à haute réactivité |
| JPH03281746A (ja) | 1990-03-29 | 1991-12-12 | Osaka Titanium Co Ltd | Ｎｂ―Ｔｉ合金の製造方法 |
| JPH04131332A (ja) | 1990-09-20 | 1992-05-06 | Osaka Titanium Co Ltd | Ｎｂ―Ｔｉ合金の製造方法 |
| EP0595877A1 (fr) | 1991-07-19 | 1994-05-11 | COMPOSITE MATERIALS TECHNOLOGY, Inc. | Procede de production d'alliages supraconducteurs |
| CN102660692A (zh) * | 2012-04-06 | 2012-09-12 | 宁夏东方钽业股份有限公司 | 超导NbTi合金的熔铸制造方法 |
| CN102965529A (zh) * | 2012-11-30 | 2013-03-13 | 上海大学 | 一种短流程钛合金Ti-Ni-Nb的制备方法 |
-
2018
- 2018-05-22 EP EP18173614.1A patent/EP3572539A1/fr not_active Withdrawn
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3268373A (en) | 1963-05-21 | 1966-08-23 | Westinghouse Electric Corp | Superconductive alloys |
| JPS60220844A (ja) | 1984-04-17 | 1985-11-05 | Sumitomo Chem Co Ltd | 伸張試験用試験片つかみ治具 |
| DE3518855A1 (de) | 1984-05-29 | 1985-12-05 | Toho Titanium Co., Ltd., Tokio/Tokyo | Abschmelzelektrode zur herstellung von niob-titan legierungen |
| US5013357A (en) * | 1989-10-26 | 1991-05-07 | Westinghouse Electric Corp. | Direct production of niobium titanium alloy during niobium reduction |
| EP0429019A1 (fr) * | 1989-11-20 | 1991-05-29 | Nkk Corporation | ProcédÀ© de fabrication d'un alliage à haute réactivité |
| JPH03281746A (ja) | 1990-03-29 | 1991-12-12 | Osaka Titanium Co Ltd | Ｎｂ―Ｔｉ合金の製造方法 |
| JPH04131332A (ja) | 1990-09-20 | 1992-05-06 | Osaka Titanium Co Ltd | Ｎｂ―Ｔｉ合金の製造方法 |
| EP0595877A1 (fr) | 1991-07-19 | 1994-05-11 | COMPOSITE MATERIALS TECHNOLOGY, Inc. | Procede de production d'alliages supraconducteurs |
| CN102660692A (zh) * | 2012-04-06 | 2012-09-12 | 宁夏东方钽业股份有限公司 | 超导NbTi合金的熔铸制造方法 |
| CN102965529A (zh) * | 2012-11-30 | 2013-03-13 | 上海大学 | 一种短流程钛合金Ti-Ni-Nb的制备方法 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113322386A (zh) * | 2021-04-19 | 2021-08-31 | 西部超导材料科技股份有限公司 | 一种大规格NbTi合金铸锭的制备方法 |
| CN113322386B (zh) * | 2021-04-19 | 2022-08-02 | 西部超导材料科技股份有限公司 | 一种大规格NbTi合金铸锭的制备方法 |
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