CN101580960B - Method for preparing single crystal of titanium-nickel binary alloy - Google Patents
Method for preparing single crystal of titanium-nickel binary alloy Download PDFInfo
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- CN101580960B CN101580960B CN2009100230750A CN200910023075A CN101580960B CN 101580960 B CN101580960 B CN 101580960B CN 2009100230750 A CN2009100230750 A CN 2009100230750A CN 200910023075 A CN200910023075 A CN 200910023075A CN 101580960 B CN101580960 B CN 101580960B
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- titanium
- binary alloy
- nickel binary
- nickel
- single crystal
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- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000013078 crystal Substances 0.000 title claims abstract description 62
- 229910002056 binary alloy Inorganic materials 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 7
- 238000005242 forging Methods 0.000 claims abstract description 3
- 238000003466 welding Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims description 25
- 239000000446 fuel Substances 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000005266 casting Methods 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 6
- 238000005554 pickling Methods 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 238000007499 fusion processing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 238000004857 zone melting Methods 0.000 abstract description 6
- 238000009825 accumulation Methods 0.000 abstract 1
- 239000000155 melt Substances 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 230000009466 transformation Effects 0.000 description 5
- 229910010380 TiNi Inorganic materials 0.000 description 4
- 229910001566 austenite Inorganic materials 0.000 description 4
- 239000011324 bead Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000000113 differential scanning calorimetry Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 230000007334 memory performance Effects 0.000 description 1
- 229910001285 shape-memory alloy Inorganic materials 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for preparing a single crystal of titanium-nickel binary alloy. A polycrystal material stick of the titanium-nickel binary alloy is subjected to vacuum melting purification, forging and drawing; a polycrystal stick or single crystal stick of the titanium-nickel binary alloy, of which one end is cone-shaped, is taken as a seed crystal; after zone melting and accumulation welding, the melt of the polycrystal material stick of the titanium-nickel binary alloy is accumulated on the seed crystal of the polycrystal or the single crystal of the titanium-nickel binary alloy; and by gradually adjusting the downward movement speeds of both for matching and finally stabilizing the downward movement speeds, single crystals of the titanium-nickel binary single crystal in different sizes are prepared. The method and technical parameters provided by the invention can ensure the success rate of preparing the titanium-nickel binary single crystal to be higher, and the success rate is over 75 percent generally.
Description
Technical field
The present invention relates to a kind of preparation method of single crystal of titanium-nickel binary alloy, be specifically related to the method that a kind of zone melting method of piling prepares single crystal of titanium-nickel binary alloy.
Background technology
Titanium-nickel binary alloy is the most comprehensive, memory performance is best, practicality the is the strongest alloy material of research in the present shape memory alloy, and its single crystal is single because of organizing, stable performance, memory effect are remarkable, and the working reliability height demonstrates extraordinary development prospect.But since titanium-nickel binary alloy be easy to basic metal and rare gas element beyond any element react, and crystal grain is difficult to grow up, so the unusual difficulty of the preparation of single crystal, the domestic report of not succeeding in developing so far.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, proposes a kind of preparation method of single crystal of titanium-nickel binary alloy, to prepare the single crystal of titanium-nickel binary alloy of high transformation temperature.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of single crystal of titanium-nickel binary alloy is characterized in that preparation process is:
(1) preparation titanium-nickel binary alloy polycrystal raw material rod: the titanium-nickel binary alloy ingot casting behind induction melting, is thermally processed into titanium-nickel binary polycrystal raw material rod, obtains titanium-nickel binary alloy polycrystal raw material rod through forging, drawing, pickling and purification again;
(2) preparation seed crystal: adopt single crystal of titanium-nickel binary alloy rod identical or titanium-nickel binary alloy polycrystalline rod as seed crystal, be processed into an end of seed crystal coniform with fuel rod composition described in the step (1);
(3) will be processed into coniform less than an end of the titanium-nickel binary alloy polycrystal raw material rod of seed crystal diameter;
(4) by the molten method of piling in district, at first with seed crystal tip fusing and kept 3~10 minutes, then with the tip and the seed crystal welding of titanium-nickel binary alloy polycrystal raw material rod, in fusion process, the ratio that seed crystal is moved down speed and the downward input speed of titanium-nickel binary alloy fuel rod by
Progressively adjust to
And be stabilized in this velocity ratio
Drawing, final continuous growth goes out single crystal of titanium-nickel binary alloy; Wherein, D
EventuallyBe the final diameter of single crystal of titanium-nickel binary alloy, D
JustBe the diameter of titanium-nickel binary alloy polycrystal raw material rod, D
SeedBe the diameter of seed crystal,
Described in the above-mentioned steps (1) in the titanium-nickel binary alloy ingot casting atomic percent of nickel be 49.8at%-50.2at%.
The present invention compared with prior art has the following advantages: method provided by the invention and technical parameter can guarantee higher titanium-nickel binary single crystal preparation success ratio, and being generally power can reach more than 75%.
Below by embodiment, the present invention is described in further detail.
Embodiment
Embodiment 1
With TiNi
49.8at%The titanium-nickel binary alloy ingot casting is thermally processed into titanium-nickel binary polycrystal raw material rod behind induction melting.Through processing, pickling and purification, obtain titanium-nickel binary alloy polycrystal raw material rod: φ 7.8mm * 700mm.One terminal addition of this fuel rod is coniform, and the tip size of its circular cone is 1mm, bores high 15mm.The titanium-nickel binary alloy polycrystal raw material rod that adopts material of the same race is as seed crystal, be of a size of φ 18mm * 50mm, the one end be processed into coniform, the tip size of its circular cone is 2mm, bore high 15mm, the employing zone melting method is deposited on the polycrystalline seed crystal after the polycrystal raw material rod is melted.When melting begins, melt with the awl point of less power with seed crystal, its upper end, tapering is the bead shape, keeps 3 minutes.The decline fuel rod, the tip of fuel rod is fused in the blanking molten bath, regulate the lowering speed of fuel rod then, making the velocity ratio that moves down of fuel rod and seed crystal is 1, progressively regulate the speed than to 3.5, wherein compare final velocity from starting velocity is 10 minutes (adopting this velocity ratio thereafter) than elapsed-time standards always, obtains the titanium-nickel binary alloy finished product monocrystalline of φ 17.8mm * 200mm at last.Through Differential scanning calorimetry the transformation temperature of monocrystalline is tested, austenite end temp point can reach 130 ℃.
Embodiment 2
With TiNi
49.8at%The titanium-nickel binary alloy ingot casting is thermally processed into titanium-nickel binary polycrystal raw material rod behind induction melting.Through processing, pickling and purification, obtain titanium-nickel binary alloy polycrystal raw material rod: φ 8.3mm * 800mm.One terminal addition of this charge bar is coniform, and the tip size of its circular cone is 1mm, bores high 12mm.The single crystal of titanium-nickel binary alloy that adopts material of the same race is as seed crystal, be of a size of φ 20mm * 30mm, the one end be processed into coniform, the tip size of its circular cone is 2mm, bore high 15mm, the employing zone melting method is deposited on the polycrystalline seed crystal after the polycrystal raw material rod is melted.When melting begins, melt with the awl point of less power with seed crystal, its upper end, tapering is the bead shape, keeps 5 minutes.The decline fuel rod, the tip of fuel rod is fused in the blanking molten bath, regulate the lowering speed of fuel rod then, making the velocity ratio that moves down of fuel rod and seed crystal is 1, progressively regulate the speed than to 4, wherein compare final velocity from starting velocity is 10 minutes (adopting this velocity ratio thereafter) than elapsed-time standards always, obtains the titanium-nickel binary alloy finished product monocrystalline of φ 16mm * 300mm at last.Through Differential scanning calorimetry the transformation temperature of monocrystalline is tested, austenite end temp point can reach 127 ℃.
Embodiment 3
With TiNi
50.0at%The titanium-nickel binary alloy ingot casting is thermally processed into titanium-nickel binary polycrystal raw material rod behind induction melting.Through processing, pickling and purification, obtain titanium-nickel binary alloy polycrystal raw material rod: φ 15mm * 700mm.One terminal addition of this charge bar is coniform, and the tip size of its circular cone is 1mm, bores high 20mm.The single crystal of titanium-nickel binary alloy that adopts material of the same race is as seed crystal, be of a size of φ 20mm * 30mm, the one end be processed into coniform, the tip size of its circular cone is 1mm, bore high 15mm, the employing zone melting method is deposited on the polycrystalline seed crystal after the polycrystal raw material rod is melted.When melting begins, melt with the awl point of less power with seed crystal, its upper end, tapering is the bead shape, keeps 10 minutes.The decline fuel rod, the tip of fuel rod is fused in the blanking molten bath, regulate the lowering speed of fuel rod then, making the velocity ratio that moves down of fuel rod and seed crystal is 1, progressively regulate the speed than to 4, wherein compare final velocity from starting velocity is 10 minutes (adopting this velocity ratio thereafter) than elapsed-time standards always, obtains the titanium-nickel binary alloy finished product monocrystalline of φ 28mm * 150mm at last.Through Differential scanning calorimetry the transformation temperature of monocrystalline is tested, austenite end temp point can reach 105 ℃.
Embodiment 4:
With TiNi
50.2at%The titanium-nickel binary alloy ingot casting is thermally processed into titanium-nickel binary polycrystal raw material rod behind induction melting.Through processing, pickling and purification, obtain titanium-nickel binary alloy polycrystal raw material rod: φ 16mm * 900mm.One terminal addition of this charge bar is coniform, and the tip size of its circular cone is 1mm, bores high 20mm.The single crystal of titanium-nickel binary alloy that adopts material of the same race is as seed crystal, be of a size of φ 20mm * 30mm, the one end be processed into coniform, the tip size of its circular cone is 1mm, bore high 15mm, the employing zone melting method is deposited on the polycrystalline seed crystal after the polycrystal raw material rod is melted.When melting begins, melt with the awl point of less power with seed crystal, its upper end, tapering is the bead shape, keeps 10 minutes.The decline fuel rod, the tip of fuel rod is fused in the blanking molten bath, regulate the lowering speed of fuel rod then, making the velocity ratio that moves down of fuel rod and seed crystal is 1, progressively regulate the speed than to 4, wherein compare final velocity from starting velocity is 10 minutes (adopting this velocity ratio thereafter) than elapsed-time standards always, obtains the titanium-nickel binary alloy finished product monocrystalline of φ 30mm * 260mm at last.Through Differential scanning calorimetry the transformation temperature of monocrystalline is tested, austenite end temp point can reach 80 ℃.
Claims (2)
1. the preparation method of a single crystal of titanium-nickel binary alloy is characterized in that preparation process is:
(1) preparation titanium-nickel binary alloy polycrystal raw material rod: the titanium-nickel binary alloy ingot casting behind induction melting, is thermally processed into titanium-nickel binary polycrystal raw material rod, obtains titanium-nickel binary alloy polycrystal raw material rod through forging, drawing, pickling and purification again;
(2) preparation seed crystal: adopt single crystal of titanium-nickel binary alloy rod identical or titanium-nickel binary alloy polycrystalline rod as seed crystal, be processed into an end of seed crystal coniform with fuel rod composition described in the step (1);
(3) will be processed into coniform less than an end of the titanium-nickel binary alloy polycrystal raw material rod of seed crystal diameter;
(4) by the molten method of piling in district, at first with seed crystal tip fusing and kept 3~10 minutes, then with the tip and the seed crystal welding of titanium-nickel binary alloy polycrystal raw material rod, in fusion process, the ratio that seed crystal is moved down speed and the downward input speed of titanium-nickel binary alloy fuel rod by
Progressively adjust to
And be stabilized in this velocity ratio
Drawing, final continuous growth goes out single crystal of titanium-nickel binary alloy; Wherein, D
EventuallyBe the final diameter of single crystal of titanium-nickel binary alloy, D
JustBe the diameter of titanium-nickel binary alloy polycrystal raw material rod, D
SeedBe the diameter of seed crystal,
2. according to the preparation method of the described a kind of single crystal of titanium-nickel binary alloy of claim 1, it is characterized in that, described in the step (1) in the titanium-nickel binary alloy ingot casting atomic percent of nickel be 49.8at%-50.2at%.
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CN106381519B (en) * | 2016-09-27 | 2019-01-08 | 西北有色金属研究院 | A method of control large scale molybdenum niobium alloy monocrystal bar isodiametric growth |
CN109136806B (en) * | 2018-11-09 | 2020-12-25 | 中国石油大学(华东) | Preparation method of NiTi monocrystal in solid state by cyclic heat treatment |
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Non-Patent Citations (5)
Title |
---|
A.J.Wagoner Johnson等.Analysis of Multistep Transformations in Single-Crystal NiTi.《Metallurgical and Materials Transactions A》.2005,第36A卷第919-928页. * |
Pavel Lejcek and Jaromir Kopecek.Growth of Metallic Crystals by Floating Zone Technique with Optical Heating.《Materials Science Forum》.2007,第567-568卷第277-280页. * |
张清 等.大尺寸钼-铌合金单晶的研制.《稀有金属材料与工程》.2005,第34卷(第12期),第1948-1951页. * |
梁学磊 等.NiTi单晶的超声衰减研究.《中山大学学报(自然科学版)》.2001,第40卷(第A期),第238-239页. * |
王乐酉 等.TiNi单晶形状记忆合金制备及组织和性能研究.《稀有金属》.2008,第32卷(第3期),第279-283页. * |
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