CN110923508A - A kind of NiTiHfSc high temperature shape memory alloy and preparation method thereof - Google Patents
A kind of NiTiHfSc high temperature shape memory alloy and preparation method thereof Download PDFInfo
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- 229910001285 shape-memory alloy Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000010891 electric arc Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 37
- 239000000956 alloy Substances 0.000 abstract description 37
- 230000009466 transformation Effects 0.000 abstract description 12
- 238000011084 recovery Methods 0.000 abstract description 9
- 230000007704 transition Effects 0.000 abstract description 6
- 230000003446 memory effect Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 238000000265 homogenisation Methods 0.000 abstract description 2
- 229910000734 martensite Inorganic materials 0.000 description 14
- 238000003723 Smelting Methods 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 6
- 230000035882 stress Effects 0.000 description 5
- 238000009760 electrical discharge machining Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 2
- 229910010380 TiNi Inorganic materials 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910001000 nickel titanium Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- 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
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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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
- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
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Abstract
本发明提供的是一种NiTiHfSc高温形状记忆合金及制备方法。一、称取Ti、Ni、Hf和Sc；二、在非自耗真空电弧炉内，将原料熔炼成铸锭；三、将铸锭放入真空炉中进行均匀化处理；四、将铸锭真空炉中进行固溶处理，得化学式为Tix‑ aNiyHfzSca的高温形状记忆合金，其中x+y+z＝100，y＝50～51，z＝15～25，a＝0～1.5，其余为x。本发明解决了现有TiNiHf合金加工性能差、形状恢复率低，相变热循环稳定性差的问题。本发明工艺简单,所得产物的相变温度较高，相变热循环稳定性佳，形状记忆效应良好，是一种有应用前景的形状记忆合金。本发明用于制备形状记忆合金。
The invention provides a NiTiHfSc high temperature shape memory alloy and a preparation method. 1. Weigh Ti, Ni, Hf and Sc; 2. Melt the raw materials into ingots in a non-consumable vacuum arc furnace; 3. Put the ingots into the vacuum furnace for homogenization; 4. Put the ingots into Solution treatment is carried out in a vacuum furnace to obtain a high temperature shape memory alloy with the chemical formula Ti x - a Ni y Hf z Sc a , wherein x+y+z=100, y=50～51, z=15～25, a= 0～1.5, the rest are x. The invention solves the problems that the existing TiNiHf alloy has poor processing performance, low shape recovery rate and poor thermal cycle stability of phase transformation. The invention has the advantages of simple process, high phase transition temperature, good phase transition thermal cycle stability and good shape memory effect, and is a promising shape memory alloy. The present invention is used to prepare shape memory alloys.
Description
Technical Field
The invention relates to a shape memory alloy, in particular to a high-temperature shape memory alloy. The invention also relates to a preparation method of the shape memory alloy.
Background
The shape memory alloy is a metal intelligent material integrating sensing and driving. The martensite phase transition temperature of the traditional shape memory alloy, such as TiNi binary alloy, is lower than 100 ℃, and the requirement of high-temperature occasions, such as fire alarms, automobiles, nuclear reactors and the like, can not be met. Heretofore, the TiNi-based high-temperature shape memory alloy mainly includes ti (nix) (X ═ Pd, Pt, Au) alloy and ni (tix) (X ═ Hf, Zr) alloy. The ti (nix) (X ═ Pd, Pt, Au) alloy contains a large amount of noble metal elements, which results in an expensive alloy and failure to achieve practical engineering applications. Zr is less effective than Hf in increasing the martensitic transformation temperature of the alloy, and the shape recovery characteristics of the NiTiZr alloy are inferior to that of the NiTiHf alloy. Therefore, the NiTiHf alloy is a high-temperature shape memory alloy with great development prospect. However, the thermal cycle stability of the martensitic transformation of the NiTiHf high-temperature shape memory alloy is poor, for example, the martensitic transformation temperature of the NiTiHf alloy is reduced by 14-25 ℃ after 10 thermal cycles. In addition, the low critical slip stress of NiTiHf high temperature shape memory alloys results in poor shape recovery characteristics of the alloys. NiTiHf high-temperature shape memory alloy is high in brittleness, so that the critical sliding stress of the alloy is difficult to improve in a plastic processing mode. Aging can also increase the critical slip stress of the alloy, but is only applicable to Ni-rich NiTiHf alloys. The Ni-rich NiTiHf alloy still has poor workability. Alloying is another effective means for improving the critical sliding stress of the NiTiHf high-temperature shape memory alloy. For example, Pd is added into NiTiHf alloy to raise the yield strength of the alloy. However, Pd is expensive. The poor shape recovery characteristics of NiTiHf alloy greatly restrict the practical engineering application of the alloy. Therefore, the need for other alloy elements to prepare the high temperature shape memory alloy with high strength, high shape recovery and excellent cold and hot processing ability is still needed.
Disclosure of Invention
The invention aims to provide the NiTiHfSc high-temperature shape memory alloy with good phase change thermal cycling stability and high shape recovery rate. The invention also aims to provide a preparation method of the NiTiHfSc high-temperature shape memory alloy.
The purpose of the invention is realized as follows:
the chemical formula of the NiTiHfSc high-temperature shape memory alloy is Tix-aNiyHfzScaWherein x + y + z is 100, y is 50-51, z is 15-25, a is 0-1.5, and the rest is x.
The preparation method of the NiTiHfSc high-temperature shape memory alloy comprises the following steps:
step one, according to the mass ratio of Ti: ni: hf: weighing Ti, Ni, Hf and Sc according to the proportion of y to z to a, wherein x + y + z is 100, y is 50-51, z is 15-25, and a is 0-1.5;
step two, putting the raw materials weighed in the step one into a non-consumable vacuum arc furnace, and vacuumizing to ensure that the vacuum degree of the back bottom reaches 2 multiplied by 10-2～2×10-3Pa, then introducing high-purity argon to the pressure in the furnace of 300-500Pa, smelting the raw materials into a button-shaped ingot by using a high-temperature electric arc, then overturning, and repeatedly smelting for 6-8 times;
step three, putting the button-shaped cast ingot obtained in the step two into a vacuum furnace, and vacuumizing to ensure that the vacuum degree reaches 4 multiplied by 10-2Pa, keeping the temperature at 900-1100 ℃ for 3h to obtain Tix-aNiyHfzScaHigh temperature shape memory alloys.
The invention solves the problems of poor martensite phase transformation thermal cycle stability and poor shape recovery characteristic of the NiTiHf high-temperature shape memory alloy, and high cost or narrow application range of the existing means.
Generally, the addition of Sc to NiTi-based alloys will lower the martensitic transformation temperature. According to the invention, the contents of the NiTiHf alloy component and the Sc element are adjusted, so that the addition of the Sc element can improve the martensitic transformation temperature of the NiTiHf alloy, and the NiTiHf alloy can still be used as a high-temperature shape memory alloy. In addition, Sc element has large chemical activity, and part of Sc element reacts with residual oxygen in the vacuum furnace during smelting to form fine Sc2O3The particles can achieve the effect of strengthening the second phase. Meanwhile, part of Sc element is dissolved in the matrix to play a role in solid solution strengthening. Therefore, the Sc element is added into the NiTiHf alloy, and the critical slip stress of the alloy can be improved without reducing the phase transition temperature of the alloy, so that the aim of improving the shape recovery characteristic of the alloy is fulfilled. More importantly, the Sc element can greatly improve the NiTiHf alloy martensite phase transformationThermal cycling stability of (a). The preparation method is simple, and the prepared alloy has good phase-change thermal cycle stability and high shape recovery rate, and is a novel high-temperature shape memory alloy with application prospect.
The method is used for preparing the NiTiHfSc high-temperature shape memory alloy.
Drawings
FIG. 1 is Ti prepared in example one28.7Ni50.3Hf15Sc1Back-scattered electron images of the alloy;
FIG. 2 is Ti prepared in example one28.7Ni50.3Hf15Sc1A DSC curve of the alloy;
FIG. 3 is Ti prepared in example one28.7Ni50.3Hf15Sc1Change of martensite phase transformation after 10 times of alloy thermal cycle
FIGS. 4 a-4 c are Ti prepared in example one28.7Ni50.3Hf15Sc1Image of alloy one-way shape memory effect.
Detailed Description
The chemical formula of the TiNiHfSc shape memory alloy is Tix-aNiyHfzScaWherein x + y + z is 100, y is 50-51, z is 15-25, a is 0-1.5, and the rest is x.
Ti of the inventionx-aNiyHfzScaThe preparation method of the shape memory alloy comprises the following steps:
weighing Ti, Ni, Hf and Sc according to the mass ratio of (x-a) y: z: a, wherein x + y + z is 100, y is 50-51, z is 15-25, a is 0-1.5, and the balance is x;
secondly, putting the Ni, Ti, Hf and Sc weighed in the step one into a non-consumable vacuum arc furnace, vacuumizing to enable the degree of vacuum of the back bottom to reach 2 x 10-2～2×10-3Pa, then introducing high-purity argon until the pressure in the furnace is 300Pa, smelting raw materials of Ni, Ti, Hf and Sc into an ingot by using high-temperature electric arc, then overturning, and repeatedly smelting for 6-8 times;
thirdly, putting the cast ingot obtained in the second step into a vacuum furnace, and pumpingVacuum to make vacuum degree reach 4X 10-2Pa, keeping the temperature at 960-1200 ℃ for 6-8 h;
fourthly, carrying out hot extrusion on the ingot casting processed in the third step at 850-950 ℃ to obtain a bar material with the diameter of about 2-3 cm, putting the bar material into a vacuum furnace, vacuumizing to enable the vacuum degree to reach 2 x 10-2Keeping the temperature of the mixture Pa at 800-1000 ℃ for 1-2 h to obtain Tix-aNiyHfzScaHigh temperature shape memory alloys.
The purity of Ni, Ti, Hf and Sc in the first step is not lower than 99.9%.
Ti obtained by the above method28.7Ni50.3Hf15Sc1The high-temperature shape memory alloy has good thermal cycle stability and shape memory effect, and the martensite phase transformation starting temperature is about 217.37 ℃; can completely meet the application requirement of the high-temperature shape memory alloy.
The invention is described in more detail below by way of example.
The first embodiment is as follows:
this example is a Ti28.7Ni50.3Hf15Sc1The preparation method of the shape memory alloy comprises the following steps:
firstly, according to the mass ratio of 28.7: 50.3: 15: 1, weighing Ni, Ti, Hf and Sc with the purity of 99.9 percent;
secondly, putting the Ni, Ti, Hf and Sc weighed in the step one into a non-consumable vacuum arc furnace, vacuumizing to enable the degree of vacuum of the back bottom to reach 2 x 10-3Pa, then filling high-purity argon with the purity of 99.9 percent until the pressure in the furnace is 300Pa, and smelting the raw materials of Ni, Ti, Hf and Sc into cast ingots by utilizing high-temperature electric arcs;
thirdly, putting the button-shaped cast ingot obtained in the second step into a vacuum furnace, and vacuumizing to ensure that the vacuum degree reaches 2 multiplied by 10-2Pa, keeping the temperature at 980 ℃ for 8h for homogenization treatment to obtain Ti28.7Ni50.3Hf15Sc1A high temperature shape memory alloy;
ti prepared from example one by spark erosion cutting28.7Ni50.3Hf15Sc1Cutting a cuboid with a length of 20mm, a width of 20mm and a thickness of 1.3mm from the high-temperature shape memory alloy, grinding the cut trace on the surface with sand paper, polishing to obtain a backscattered electron image, and observing the sample, wherein FIG. 1 is the backscattered electron image of the sample, wherein the white contrast phase is Hf-rich phase, and the black contrast phase is Sc2O3The gray contrast phase is the matrix.
Ti prepared from example one by spark erosion cutting28.7Ni50.3Hf15Sc1A rectangular parallelepiped of 3mm in length, 1.5mm in width and about 30mg in weight was cut out of the high temperature shape memory alloy, the surface of the cut was polished with sandpaper, and the phase change behavior was measured on a Perkin-Elmer Diamond DSC, and FIG. 2 is a DSC curve of the sample showing the martensite phase transition onset temperature (M)s) The temperature was 217.37 ℃. It can be seen that the phase transition temperature is higher than Ti29.7Ni50.3Hf15High temperature shape memory alloy (163.73 deg.C). FIG. 3 shows a sample of Ti28.7Ni50.3Hf15Sc1The martensite phase transformation temperature of the alloy is reduced by 8.15 ℃ in 10 times of thermal cycles after the alloy is subjected to the martensite phase transformation change for 10 times of thermal cycles. The martensite phase transformation thermal cycle stability of the visible sample is superior to that of Ti29.7Ni50.3Hf15And (3) alloying.
Ti prepared from example one by spark erosion cutting28.7Ni50.3Hf15Sc1Cutting 35mm long strip of 0.5mm thickness from the high temperature shape memory alloy, grinding surface cutting trace with sand paper, bending the strip by bending mold with 6% deformation, and heating to 350 deg.C. FIGS. 4 a-4 c are prepared Ti28.7Ni50.3Hf15Sc1The one-way shape memory effect picture of the alloy is heated and then the deformation is completely recovered.
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Cited By (2)
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| CN115261674A (en) * | 2021-04-29 | 2022-11-01 | 西安交通大学 | High-phase-change latent heat titanium-nickel-based shape memory alloy and preparation method thereof |
| CN115927915A (en) * | 2022-11-30 | 2023-04-07 | 西安赛特思迈钛业有限公司 | Ti-Ni-Zr shape memory alloy and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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Application publication date: 20200327 |