CN113718155B - High entropy high strength (TiHfX)50（NiCu）50Shape memory alloy and preparation method thereof - Google Patents
High entropy high strength (TiHfX)50（NiCu）50Shape memory alloy and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- 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
- C22B9/16—Remelting metals
- C22B9/20—Arc remelting
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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
- 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
- C22F1/006—Resulting in heat recoverable alloys with a memory effect
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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
Abstract
The invention relates to the technical field of shape memory alloys, in particular to a high-entropy high-strength (TiHfX)50（NiCu）50Shape memory alloy and a preparation method thereof. Provided by the invention (TiHfX)50（NiCu）50The high-entropy high-strength memory alloy comprises the following chemical components in atomic percentage: 33-37% of Ti, 42-46% of Ni, 8-12% of Hf, 4-8% of Cu and 3-7% of X, wherein X is one of Y, Zr, Nb, Al, Co and Mn. The alloy is prepared by the following method: the Ti, Ni, Hf, Cu and X raw materials in the component ratio are placed in a vacuum arc melting furnace and repeatedly melted to obtain an alloy ingot, and the as-cast high-entropy memory alloy has both high strength and good memory performance. The high-entropy memory alloy prepared by the invention has high strength and good memory performance, the preparation process is very simple, the alloy only needs to be subjected to arc melting and compression memory training, and heat treatment and plastic deformation processing are not needed, so that the high-entropy memory alloy is easy to operate and has a very good application prospect.
Description
Technical Field
The invention belongs to the technical field of alloy materials and preparation thereof, and particularly relates to a high-entropy high-strength (TiHfX)50(NiCu)50Shape memory alloy and a preparation method thereof.
Background
The high-entropy alloy breaks through the traditional alloy design method by a brand-new thought, and provides a more unique and wide visual angle and space for developing novel materials and improving the traditional alloy. The concept of "high entropy" is widely integrated into the research of various novel high-performance materials, and shows great potential in the aspect of improving the mechanical and physicochemical properties of the materials. In 2014, Ukrainian scholars combined "high-entropy alloy" with "shape memory", formally proposed high-entropy shape memory alloy (G.S. Firstov, et al.high-temperature shape memory alloy definitions, Materials Science and Engineering A,2004,378:2-10), provided new application prospects for high-entropy alloy, and provided new research ideas for development of novel memory alloys. In China, Wuyuan et al, Beijing university of science and technology, also reported that the content of the Chinese herbal medicine is high in patent CN105296836B granted in 2017Design and preparation method of entropy memory alloy. However, these early high entropy alloys were defined as alloys having a mixed entropy above 1.5R or alloy constituents that satisfied 5-35 atomic percent. In recent years, research in the field of high-entropy alloys is rapidly developed, the definition of the high-entropy alloys is continuously expanded, and the mixed entropy value and the component range of the high-entropy alloys are not limited to the above range any more, namely the mixed entropy value of the alloys can be lower than 1.5R, and the components of the components can be lower than 5% or higher than 35%, so that the development of more high-entropy alloys with excellent performance is possible. For example, Ti proposed by Wang et al of Beijing university of science and technology50Zr20Hf15Al10Nb5And Ti49Zr20Hf15Al10Nb6High-entropy memory alloys with a mixed entropy of 1.33R and 1.35R, respectively, and a composition of constituent Ti of up to 50% (Lu Wang, et al. Superelastic effect in Ti-rich high-entropy alloy strain-induced texture transformation, script Material, 2019,162: 112-; ti proposed by Chen et al of Taiwan university40Zr10Ni40Co5Cu5The mixed entropy of the high-entropy alloy is 1.28R, and the components of Ti and Ni are both as high as 40% (Chih-Hsean Chen, et al40Zr10Ni40Co5Cu5multi-principal element alloy, script material, 2020,186: 127-; ti proposed by Rajeshwar of national research university of Russian Bilogorod38Zr25Hf25Ta10Sn2And Ti38Zr25Hf25Ta7Sn5The high entropy alloy has a mixed entropy of 1.37R and 1.39R, respectively, 38% of Ti component and only 2% of Sn component (Rajeshwar R, et al. Exceptionllyhigh strain-modifying and reduction product to transformation induced plasticity effect in Ti-rich high-entropy alloys, Scientific Reports,2020,10: 13293).
At present, most of the publicly reported non-high-entropy superelasticity shape memory alloys need processing processes such as rolling, drawing, aging and the like, and the production and processing processes are complex. Reported high entropy memory alloy systems are Ti-Zr-Hf-Co-Ni-Cu, Ti-Zr-Hf-Ni-Pd, Ti-Zr-Hf-Ni-Cu-Pd, Ti-Zr-Hf-Al-Cu-Nb, Ti-Zr-Hf-Nb-Ta-Sn, etc. Among them, Ti-Zr-Hf-Co-Ni-Cu series high entropy memory was proposed first, the alloy has memory property, and can fully recover 1.63% of prestrain (G.S. Firstov, et al.high entropy shape memory alloys, Materials Today: Proceedings,2015,2: S499-S503); the Ti-Zr-Hf-Ni-Cu high-entropy alloy has superelasticity in the range of 185-285 ℃, and can completely recover 4% of prestrain at room temperature (Shaohui Li, et al. A high-entropy high-temperature sheath alloy with large and complex superelastic recovery, Materials Research Letters,2021,9: 263-269). Ti-Zr-Hf-Ni-Pd and Ti-Zr-Hf-Ni-Cu-Pd are high temperature memory alloys, have a transition temperature of 500 ℃ or higher, do not have memory properties at room temperature, and are very high in cost due to the addition of a noble metal Pd (1℃ Demiran, et al. Ultra-high temperature multiple-component shape memory alloys, script Material 2019, 158: 83-87; 2D. Piorunek, et al. chemical composition, microstructural and structural transformation in high temperature shape memory alloys, Intermetallics,2020,122: 106792). Ti-Zr-Hf-Al-Nb system proposed by Wang of Beijing university of science and technology is beta titanium alloy, the maximum recoverable strain is 5.2%, the complete recoverable strain is 4%, but the strength and the critical stress are only 900MPa and 480 MPa; the Ti-Zr-Hf-Nb-Ta-Sn series is also a beta titanium alloy, and the maximum recoverable strain can reach 3.8% (J.J.Gao, et al Synthesis and characterization of a new TiZrHfNbTaSn high-entry alloy ex-situ superior modifier, script Material, 2021,198: 113824).
The memory alloys reported so far have the following problems: (1) the existing high-entropy and non-high-entropy shape memory alloys have complex preparation processes, and most of the high-entropy and non-high-entropy shape memory alloys need plastic processing such as rolling and drawing and heat treatment processes such as homogenization, aging, quenching and the like. For example, Ti-Zr-Hf-Ni-Cu-Pd needs to be subjected to heat treatment for 100 hours, and Ti-Zr-Hf-Al-Cu-Nb and Ti-Zr-Hf-Nb-Ta-Sn series high-entropy alloys are subjected to cold rolling, homogenization, aging, water quenching treatment and the like. (2) The existing high-entropy and non-high-entropy shape memory alloy can not have both high strength and high recoverable strain. For example, the recoverable strain of Ti-Zr-Hf-Co-Ni-Cu is only 1.63%, and the recoverable strain of Ti-Zr-Hf-Ni-Cu system is 4%. The Ti-Zr-Hf-Al-Cu-Nb system beta titanium alloy can recover the strain to 5.2 percent, but has low strength and critical stress. (3) Some of the existing high-entropy and non-high-entropy shape memory alloys contain noble metals, and the cost of the alloys is too high.
In summary, various problems of the existing shape memory alloy still remain to be solved, the preparation process needs to be further simplified, and the performance of the alloy needs to be adjusted by more optimized alloy component combination, so that the application range of the alloy is further expanded.
Disclosure of Invention
In view of the problems of the prior art, the invention provides a high-entropy high-strength (TiHfX)50(NiCu)50The shape memory alloy and the preparation method thereof have good comprehensive performance and have good shape memory effect and high strength in a special component range.
In order to achieve the purpose, the invention adopts the following technical scheme:
high entropy and high strength (TiHfX)50(NiCu)50A shape memory alloy, the alloy comprising the following chemical composition in atomic percent: 33 to 37 percent of Ti, 42 to 46 percent of Ni, 8 to 12 percent of Hf, 4 to 8 percent of Cu and 3 to 7 percent of X, wherein the alloy element X is one of Y, Zr, Nb, Al, Co and Mn.
Preferably, the sum of the atomic percentages of the three elements Ti, Hf and X is equal to the sum of the atomic percentages of the two elements Ni and Cu, and the sum is 50%.
High entropy and high strength (TiHfX)50(NiCu)50A method of making a shape memory alloy, said method comprising the steps of:
1) material preparation and smelting: mixing the raw materials Ti, Ni, Hf, Cu and X according to atomic percentage, putting the mixture into a vacuum arc melting furnace, vacuumizing the furnace, filling argon to prevent oxidation in the alloy melting process, continuously melting for more than 2 minutes in a molten state for more than 6 times repeatedly to uniformly mix the alloy components to obtain the as-cast high-entropy high-strength (TiHfX)50(NiCu)50A shape memory alloy;
2) note the bookMemory training: the (TiHfX) obtained in the step 1)50(NiCu)50And cutting the shape memory alloy cast ingot into a required columnar sample, and then performing cyclic compression memory training to obtain the columnar high-entropy high-strength shape memory alloy with the recovery rate of 100%.
Preferably, in the step 1), the vacuum degree of the vacuum arc melting furnace is less than 10-3Pa, the melting current is 100-350A.
Further preferably, in the step 1), the melting state is continued for 2 minutes or more for each pass.
Preferably, in the step 1), after argon is filled, the pressure in the smelting furnace is-0.06 MPa, arc striking is carried out, and the current is increased to 250-350A; the turnover is realized by a manipulator, and the repeated remelting time is more than 6 times.
Further preferably, in the step 1), when X ═ Y, the melting current is 220-. In the step 2), the 100% recovery of 6% pre-strain can be realized when the training frequency is more than 5 times, and the pre-strain has the post-training output stress strength of 1578 MPa.
Further preferably, in the step 1), when X ═ Zr, the melting current is 180-. In the step 2), the 100% recovery of 6% pre-strain can be realized when the training times are more than 7 times, and the pre-strain has 1040MPa of post-training output stress strength.
Further preferably, in the step 1), when X ═ Al, the melting current is 150-. In the step 2), the 100% recovery of 6% pre-strain is realized when the training times are more than 5 times, and the pre-strain has the output stress strength of 1944MPa after training.
Further preferably, in the step 1), when X ═ Co, the melting current is 200-. In the step 2), the 100% recovery of 6% pre-strain is realized when the training times are more than 5 times, and the pre-strain has the output stress strength of 1945MPa after training.
Further preferably, in the step 1), when X ═ Mn, the melting current is 260-. In the step 2), the 100% recovery of 6% pre-strain can be realized when the training times are more than 5 times, and the 100% recovery has 2070MPa of post-training output stress strength.
Preferably, in the step 2), the height of the columnar sample is 6mm, the diameter of the columnar sample is 3mm, the prestrain of the cyclic compression memory training is 4-8%, and the cycle number is 5-20.
Preferably, in the step 1), the as-cast state high-entropy high-strength (TiHfX)50(NiCu)50The compressive strength of the shape memory alloy is 1832-2552MPa, and the recoverable strain is 4.61-8.81%.
Preferably, in the step 2), the recovery rate of the 6% pre-strain of the columnar high-entropy high-strength shape memory alloy can reach 100%, and the maximum output stress strength after the 6% pre-strain training is 1040-2070 MPa.
The invention has the following beneficial effects:
1) the high-entropy high-strength shape memory alloy disclosed by the invention has high strength and excellent memory performance. The compression strength of the as-cast high-entropy memory alloy is 1832-2552MPa, and the recoverable strain is 4.61-8.81%. After 5-20 times of compression training, the recovery rate of the columnar high-entropy shape memory alloy can reach 100% and has excellent stability, 6% of pre-strain can be completely recovered, and the maximum output stress strength after training is 1040-2070 MPa.
2) The invention introduces the expanded definition of the high-entropy alloy into the development of a novel high-strength superelasticity shape memory alloy, designs an alloy with equal atomic ratio of Ti-like elements (Ti, Hf, X) and Ni-like elements (Ni, Cu) on the basis of the TiNi memory alloy, and breaks the component limitation of 5-35% of the traditional high-entropy alloy elements by partial components. Therefore, the alloy can not only ensure good memory performance, but also play a role in improving the mechanical property of the material by the high entropy effect. In the preferable X element, the addition of rare earth Y can improve the recoverable strain and superelasticity of the alloy within a certain range; the plasticity and the toughness of the alloy can be improved by adding Zr, the phase transition temperature of the alloy is effectively adjusted, and the shape memory effect of the alloy is improved; the addition of Nb can improve the toughness and recoverable strain of the alloy and promote the precipitation of omega phase to improve the stability; the oxidation resistance of the alloy can be improved by adding the Al element; the addition of Co element can properly reduce the transformation temperature, is a strong stabilizer of B2 austenite, and can stabilize martensite and austenite; the addition of Mn can replace Ti and Ni, and has good promotion effect on the exertion of high entropy effect.
3) The invention has low cost and simple process. The invention relates to (TiHfX)50(NiCu)50The alloy is used as a base, the components and the performance of the alloy are optimized and adjusted by changing the X element into Y, Zr, Nb, Al, Co, Mn and the like, and the alloy is not added with noble metals such as Pd, Pt, Au and the like and has lower cost. In addition, the preparation process is simple, the alloy only needs to be subjected to arc melting and compression memory training, and does not need to be subjected to heat treatment such as homogenization, aging, quenching and the like and plastic deformation processing such as rolling, drawing and the like, so that the process can be further simplified, and the processing cost can be reduced. Therefore, the invention has potential application value.
Drawings
FIG. 1 is a microstructure view of alloy 1 prepared in example 1 of the present invention;
FIG. 2 is a compressive stress-strain curve for alloy 1 prepared in example 1 of the present invention;
FIG. 3 is a graph of 2-15% cyclic compressive stress strain for alloy 1 prepared in example 1 of the present invention;
FIG. 4 is a 20 cycle 6% training compression curve for alloy 1 prepared in example 1 of the present invention;
FIG. 5 is a microstructure view of alloy 2 prepared in example 2 of the present invention;
FIG. 6 is a compressive stress-strain curve for alloy 2 prepared in example 2 of the present invention;
FIG. 7 is a 2-15% cyclic compressive stress strain curve for alloy 2 prepared in example 2 of the present invention;
FIG. 8 is a 20 cycle 6% training compression curve for alloy 2 prepared in example 2 of the present invention;
FIG. 9 is a microstructure view of alloy 3 prepared in example 3 of the present invention;
FIG. 10 is a graph of the compressive stress strain for alloy 3 prepared in example 3 of the present invention;
FIG. 11 is a graph of 2-10% cyclic compressive stress strain for alloy 3 prepared in example 3 of the present invention;
FIG. 12 is a 20 cycle 6% training compression curve for alloy 3 prepared in example 3 of the present invention;
FIG. 13 is a compressive stress-strain curve for alloy 4 prepared in example 4 of the present invention;
FIG. 14 is a graph of 2-8% cyclic compressive stress strain for alloy 4 prepared in example 4 of the present invention;
FIG. 15 is a compression curve of alloy 4 prepared in example 4 of the present invention for 20 cycles of 6% training
FIG. 16 is a graph of the compressive stress strain for alloy 5 prepared in example 5 of the present invention;
FIG. 17 is a graph of 2-8% cyclic compressive stress strain for alloy 5 prepared in example 5 of the present invention;
FIG. 18 is a 15 pass 6% cycle training compression curve for alloy 5 prepared in example 5 of the present invention
FIG. 19 is a compressive stress-strain curve for alloy 6 prepared in example 6 of the present invention;
FIG. 20 is a graph of 2-10% cyclic compressive stress strain for alloy 6 prepared in example 6 of the present invention;
FIG. 21 is a 20-pass 6% cycle training compression curve for alloy 6 prepared in example 6 of the present invention.
The specific implementation mode is as follows:
the invention is further described below with reference to the accompanying drawings.
Example 1
Using high-purity metals of Ti, Ni, Hf, Cu and Y as raw materials, cleaning them by using alcohol, then using the cleaned high-purity metals of Ti, Ni, Hf, Cu and Y as alloy 1 according to the atomic ratio of 35%, 44% Ni, 10% Hf, 6% Cu and 5% Y, placing the raw materials in a vacuum arc furnace, vacuumizing to 9.5X 10%-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 220-280A, and keeping the smelting current for more than 2 minutes in the molten state of the alloy to ensure that all metals are completely melted together. Will get by the manipulatorThe obtained alloy ingot is turned over and repeatedly smelted for 6 times, so that the raw material components are uniform, and the as-cast high-entropy Ti-Ni-Hf-Cu-Y shape memory alloy is obtained.
The microstructure of the resulting alloy 1 is shown in FIG. 1; the alloy 1 is subjected to a press-breaking experiment, as shown in FIG. 2, the compressive strength is 2115MPa, and the breaking strain is 30.96%; alloy 1 was subjected to 2-15% precompression test, as shown in FIG. 3, with a recovery of 42-48% and a maximum recoverable strain of 6.65%, where the superelastic strain was 0.50-2.83%; alloy 1 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, and after more than 20 times of cyclic compression memory training with pre-compression of 6%, the recovery rate can reach 100% after the cycle number is more than 5 times, wherein the super-elastic strain is 1.28-2.83%, the output stress intensity after training can reach 1578MPa, and the stress-strain curve of the compression memory training is shown in figure 4.
Example 2
Using high-purity metals of Ti, Ni, Hf, Cu and Zr as raw materials, cleaning with alcohol, then using the cleaned raw materials as alloy 2 according to the atomic ratio of 35% of Ti, 44% of Ni, 10% of Hf, 6% of Cu and 5% of Zr, placing the raw materials in a vacuum arc furnace, vacuumizing to 9.5X 10-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 180-240A, and keeping the smelting current for more than 2 minutes in the molten state of the alloy to ensure that all metals are completely melted together. And overturning the obtained alloy ingot by using a manipulator, and repeatedly smelting for 6 times to ensure that the raw material components are uniform, thereby obtaining the as-cast high-entropy Ti-Ni-Hf-Cu-Zr shape memory alloy.
The microstructure of the resulting alloy 2 is shown in FIG. 5, which shows a compressive strength of 2498MPa and a breaking strain of 33.41%, as shown in FIG. 6; alloy 2 was subjected to 2-15% precompression test, as shown in FIG. 7, with a recovery of 50-78% and a maximum recoverable strain of 8.81%, where the superelastic strain was 4.95%; alloy 2 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, and after more than 20 times of cyclic compression memory training with pre-pressing of 6%, the recovery rate can reach 100% after the cycle number is more than 7 times, wherein the super-elastic strain is 2.57-3.35%, the output stress intensity reaches 1040MPa, and the stress-strain curve of the compression memory training is shown in figure 8.
Example 3
Using high-purity metals Ti, Ni, Hf, Cu and Nb as raw materials, cleaning with alcohol, mixing them according to the atomic ratio of 35% Ti, 44% Ni, 10% Hf, 6% Cu and 5% Nb to obtain alloy 3, placing the raw materials in vacuum arc furnace, vacuumizing to 9.5X 10-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 180-320A, and keeping the smelting current for more than 2 minutes in the molten state of the alloy to ensure that all metals are completely melted together. And overturning the obtained alloy ingot by using a manipulator, and repeatedly smelting for 6 times to ensure that the raw material components are uniform, thereby obtaining the as-cast high-entropy Ti-Ni-Hf-Cu-Nb shape memory alloy.
The microstructure micrograph of the obtained alloy 3 is shown in fig. 9, and the alloy 3 is subjected to a press-fracture experiment, as shown in fig. 10, wherein the compressive strength is 1832MPa, and the fracture strain is 9.46%; alloy 3 was subjected to 2-10% precompression test, as shown in FIG. 11, with a recovery of 50-75% and a maximum recoverable strain of 5.98%, where the superelastic strain was 0.21-1.90%. Alloy 3 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, and after more than 20 times of cyclic compression memory training with pre-pressing of 6%, the recovery rate can reach 100% after the cycle number is more than 4 times, wherein the super-elastic strain is 1.16-2.77%, the output stress intensity reaches 1276MPa, and the stress-strain curve of the compression memory training is shown in figure 12.
Example 4
Using high-purity metals Ti, Ni, Hf, Cu and Al as raw materials, cleaning with alcohol, using cleaned high-purity metals Ti, Ni, Hf, Cu and Al as alloy 4 according to the atomic ratio of 35%, 44% Ni, 10% Hf, 6% Cu and 5% Al, placing the raw materials in a vacuum arc furnace, vacuumizing to 9.5X 10-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 150-220A, and keeping the smelting current for more than 2 minutes in the molten state of the alloy to ensure that all metals are completely melted together. And overturning the obtained alloy ingot by using a manipulator, and repeatedly smelting for 6 times to ensure that the raw material components are uniform, thereby obtaining the as-cast high-entropy Ti-Ni-Hf-Cu-Al shape memory alloy.
The alloy 4 was subjected to a press-break test, as shown in fig. 13, and had a compressive strength of 2552MPa and a strain at break of 12.40%; alloy 4 was subjected to 2-6% precompression test, as shown in FIG. 14, with a recovery of 75-77% and a maximum recoverable strain of 4.61%, where the superelastic strain was 0.16-0.91%; alloy 4 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, and after more than 20 times of cyclic compression memory training with pre-compression of 6%, the recovery rate can reach 100% after the cycle number is more than 4 times, wherein the super-elastic strain is 1.16-1.69%, the output stress strength can reach 1944MPa, and the stress-strain curve of the compression memory training is shown in figure 15.
Example 5
Using high-purity metals of Ti, Ni, Hf, Cu and Co as raw materials, cleaning them with alcohol, then using alloy 5 according to the atomic ratio of 35% of Ti, 44% of Ni, 10% of Hf, 6% of Cu and 5% of Co, placing the raw materials in vacuum arc furnace, vacuumizing to 9.5X 10-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 200-260A, and keeping the smelting current for more than 2 minutes in the molten state of the alloy to ensure that all metals are completely melted together. And overturning the obtained alloy ingot by using a manipulator, and repeatedly smelting for 6 times to ensure that the raw material components are uniform, thereby obtaining the as-cast high-entropy Ti-Ni-Hf-Cu-Co shape memory alloy.
Example 6
Using high-purity metals of Ti, Ni, Hf, Cu and Mn as raw materials, cleaning them with alcohol, mixing them according to the atomic ratio of 35% of Ti, 44% of Ni, 10% of Hf, 6% of Cu and 5% of Mn and making them be alloy 6, placing the raw materials in vacuum arc furnace, vacuumizing to 9.5X 10-3Below Pa, filling argon to-0.06 MPa, then striking arc, controlling the smelting current at 260-350A, melting the alloyThe state lasts more than 2 minutes, and the metals are ensured to be completely melted together. And overturning the obtained alloy ingot by using a manipulator, and repeatedly smelting for 6 times to ensure that the raw material components are uniform, thereby obtaining the as-cast high-entropy Ti-Ni-Hf-Cu-Mn shape memory alloy.
The alloy 6 was subjected to a press-break test, as shown in fig. 19, and had a compressive strength of 2388MPa and a strain at break of 12.80%; alloy 1 was subjected to 2-10% precompression test, as shown in FIG. 20, with a recovery of 42-69% and a maximum recoverable strain of 6.86%, where the superelastic strain was 0.39-2.37%; alloy 6 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, and after more than 20 times of cyclic compression memory training with pre-compression of 6%, the recovery rate can reach 100% after the cyclic times is more than 3 times, wherein the super-elastic strain is 1.25-1.85%, the stress can reach 2070MPa, and the stress-strain curve of the compression memory training is shown in figure 21.
Comparative example 1
Using high-purity metals of Ti, Ni, Hf, Cu and Cr as raw materials, cleaning them with alcohol, mixing them according to the atomic ratio of 35% of Ti, 44% of Ni, 10% of Hf, 6% of Cu and 5% of Cr and using alloy 7, placing the raw materials in vacuum arc furnace, vacuumizing to 9.5X 10-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 350A and keeping the smelting current for more than 2 minutes in the molten state of the alloy, and ensuring that all metals are completely melted together. And overturning the obtained alloy ingot by using a manipulator, and repeatedly smelting for 6 times to ensure that the raw material components are uniform, thereby obtaining the as-cast high-entropy Ti-Ni-Hf-Cu-Cr shape memory alloy.
The compressive strength of the obtained alloy 7 in an as-cast state is 1890MPa, and the fracture strain is 10.40 percent; the maximum recovery rate in the as-cast state is 82%, the maximum recoverable strain is 6.55%, and the super elasticity is 2.27%; alloy 7 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, and the second circulating alloy is broken by pressing through the circulating compression memory training with the prepressing rate of 6 percent and cannot be completely recovered.
Comparative example 2
Using high-purity metals of Ti, Ni, Hf, Cu and V as raw materials, cleaning the raw materials by alcohol, then using the cleaned raw materials and mixing them according to the atomic ratio of 35% of Ti, 44% of Ni, 10% of Hf, 6% of Cu and 5% of V as alloy 8Placing in a vacuum arc furnace, vacuumizing to 9.5 × 10- 3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 350A and keeping the smelting current for more than 2 minutes in the molten state of the alloy, and ensuring that all metals are completely melted together. And overturning the obtained alloy ingot by using a manipulator, and repeatedly smelting for 6 times to ensure that the raw material components are uniform, thereby obtaining the as-cast high-entropy Ti-Ni-Hf-Cu-V shape memory alloy.
The obtained alloy 8 had an as-cast compressive strength of 2170MPa and a fracture strain of 10.35%; the maximum recovery rate in the cast state is 62 percent, and the maximum recoverable strain is 6.23 percent; alloy 8 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, and the second time of cyclic alloy is broken by pressing through cyclic compression memory training with the prepressing of 6 percent and can not be completely recovered.
Comparative example 3
Using high-purity metals of Ti, Ni, Hf, Cu and Y as raw materials, cleaning them with alcohol, then using alloy 9 according to the atomic ratio of 39% Ti, 44% Ni, 10% Hf, 6% Cu and 1% Y, placing the raw materials in vacuum arc furnace, vacuumizing to 9.5X 10-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 350A and keeping the smelting current for more than 2 minutes in the molten state of the alloy, and ensuring that all metals are completely melted together. Turning over the obtained alloy ingot by using a manipulator, and repeatedly smelting for 6 times to ensure that the raw material components are uniform; cutting the obtained alloy into small blocks by adopting a wire, placing the small blocks in a vacuum heat treatment furnace, vacuumizing to-0.05 MPa, introducing argon, carrying out homogenization treatment at 900 ℃ for 2h, and rapidly quenching in an ice-water mixture to obtain the Ti-Ni-Hf-Cu-Y shape memory alloy.
The obtained alloy 9 has a complex process, the maximum recoverable strain is 7.92 percent, the recovery rate is 72 percent, and the compressive strength is only 1471 MPa; alloy 9 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, the recovery rate reaches 100% after 20 times of pre-pressing and 7% of cyclic compression training, but the maximum output stress after training is lower and is only 986 MPa.
Comparative example 4
High-purity metals of Ti, Ni, Hf, Cu and Zr are used as raw materials, after being cleaned by alcohol, the raw materials are cleaned according to the atomic ratio of 35 percent of Ti, 35 percent of Ni,10 percent of Hf, 6 percent of Cu and 14 percent of Zr are mixed to form alloy 10, the raw materials are placed in a vacuum arc furnace and are vacuumized to 9.5 multiplied by 10-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 350A and keeping the smelting current for more than 2 minutes in the molten state of the alloy, and ensuring that all metals are completely melted together. The obtained alloy ingot is turned over by a manipulator and repeatedly smelted for 6 times, so that the raw material components are uniform, and the as-cast high entropy (TiHfZr) is obtained59(NiCu)41A shape memory alloy.
The compressive strength of the obtained alloy 10 in an as-cast state is 1322MPa, and the fracture strain is 8.94%; the maximum recovery rate of the cast state is 51 percent, and the maximum recoverable strain is 4.10 percent; the alloy 10 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by a wire, and the second circular alloy is broken by the circular compression memory training with the prepressing rate of 6 percent and cannot be completely recovered.
Comparative example 5
Using high-purity metals of Ti, Ni, Hf, Cu and Zr as raw materials, cleaning with alcohol, then using alloy 11 as the raw materials according to the atomic ratio of 20% Ti, 20% Ni, 20% Hf, 20% Cu and 20% Zr after cleaning, placing the raw materials in a vacuum arc furnace, vacuumizing to 9.5X 10-3And (3) introducing argon to-0.06 MPa below Pa, then striking an arc, controlling the smelting current at 350A and keeping the smelting current for more than 2 minutes in the molten state of the alloy, and ensuring that all metals are completely melted together. The obtained alloy ingot is turned over by a manipulator and then repeatedly smelted for 6 times, so that the raw material components are uniform, and the as-cast state high entropy (TiHfZr) is obtained60(NiCu)40A shape memory alloy.
The compressive strength of the obtained alloy 11 in an as-cast state is 1210MPa, and the fracture strain is 6.55 percent; the maximum recovery rate of the cast state is 70 percent, and the maximum recoverable strain is only 2.8 percent; alloy 11 is cut into a cylindrical sample with the height of 6mm and the diameter of 3mm by utilizing a wire, and the first circulating alloy is broken by pressing and can not be completely recovered after the circulating compression training with the prepressing of 6 percent.
TABLE 1 Performance parameters of memory alloys of examples 1-6 and comparative examples 1-4
As can be seen from the data in Table 1, the high-entropy shape memory alloy of the present invention has excellent memory performance, high strength (including high compressive strength and high post-training output stress strength), and good stability. The cast-state high-entropy memory alloy can recover the strain to be 4.61-8.81 percent before training, and simultaneously has the compressive strength of 1832-2552MPa, the recovery rate after training reaches 100 percent and the output stress strength reaches 1040-2070 MPa. Wherein, the preferable component has recoverable strain as high as 6.5-8.81%, and has the compressive strength of 2300-2550MPa and the output stress strength of 1500-2000 MPa.
The above embodiments are merely preferred technical solutions of the present invention, and should not be construed as limiting the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (6)
1. High entropy and high strength (TiHfX)50（NiCu）50Shape memory alloy, characterized in that the alloy has the following chemical composition in atomic percent: 35% of Ti, 44% of Ni, 10% of Hf, 6% of Cu and 5% of X, wherein the alloy element X is one of Y, Zr, Nb, Al, Co and Mn;
the alloy manufacturing method does not need to carry out homogenization, aging, quenching, rolling and drawing, and comprises the following steps:
1) material preparation and smelting: mixing the raw materials Ti, Ni, Hf, Cu and X according to atomic percentage, putting the mixture into a vacuum arc melting furnace, vacuumizing the furnace, filling argon to prevent oxidation in the alloy melting process, continuously melting for more than 2 minutes in a molten state for more than 6 times repeatedly to uniformly mix the alloy components to obtain the as-cast high-entropy high-strength (TiHfX)50（NiCu）50A shape memory alloy;
2) memory training: the (TiHfX) obtained in the step 1)50（NiCu）50And cutting the shape memory alloy cast ingot into a required columnar sample, and then performing cyclic compression memory training to obtain the columnar high-entropy high-strength shape memory alloy with the recovery rate of 100%.
2. High entropy high strength (TiHfX) according to claim 150（NiCu）50The shape memory alloy is characterized in that in the step 1), the vacuum degree of a vacuum arc melting furnace is less than 10-3Pa, the melting current is 100-350A.
3. High entropy high strength (TiHfX) according to claim 150（NiCu）50The shape memory alloy is characterized in that in the step 1), after argon is filled, the pressure in a smelting furnace is-0.06 MPa, arc striking is carried out, and the current is increased to 250-350A; and the manipulator is adopted for overturning, and the repeated remelting time is more than 6 times.
4. High entropy high strength (TiHfX) according to claim 150（NiCu）50The shape memory alloy is characterized in that in the step 2), the height of the columnar sample is 6mm, the diameter of the columnar sample is 3mm, the prestrain of the cyclic compression memory training is 4-8%, and the cycle number is 5-20.
5. High entropy high strength (TiHfX) according to claim 150（NiCu）50Shape memory alloy, characterized in that, in the step 1), the as-cast state high-entropy high-strength (TiHfX)50（NiCu）50The compressive strength of the shape memory alloy is 1832-2552MPa, and the recoverable strain is 4.61-8.81%.
6. High entropy high strength (TiHfX) according to claim 150（NiCu）50The shape memory alloy is characterized in that in the step 2), the recovery rate of 6% pre-strain of the columnar high-entropy high-strength shape memory alloy is 100%, and the output stress strength after 6% pre-strain training is 1040-2070 MPa.
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