CN105296836A - NxMy high-entropy alloy with shape memory effect and preparing method thereof - Google Patents
NxMy high-entropy alloy with shape memory effect and preparing method thereof Download PDFInfo
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Abstract
The invention relates to NxMy high-entropy alloy with a shape memory effect and a preparing method thereof. The alloy comprises NxMy, wherein x is larger than or equal to 45 and smaller than or equal to 55, y is larger than or equal to 45 and smaller than or equal to 55, the N is any two or more of Ti, Zr, Hf, V, Nb, Ta, Mo and W and the M is any two or more of V, Mn, Fe, Co, Ni, Cu, Cr and Zn; and the content of the Ti, the content of the Zr, the content of the Hf, the content of the V, the content of the Nb, the content of the Ta and the content of the Mo in the N are each larger than or equal to 5% and smaller than or equal to 35%, and the content of the V, the content of the Mn, the content of the Fe, the content of the Co, the content of the Ni, the content of the Cu, the content of the Cr and the content of the Zn are each larger than or equal to 5% and smaller than or equal to 35%. A body-centered cubic single-phase solid solution with the volume fraction not lower than 95% and an intermetallic compound form the alloy phase structure. The alloy is prepared through an electric arc melting method. The alloy has the shape memory effect within a wider temperature range and meanwhile has the high-entropy alloy feature. The NxMy high-entropy alloy and the preparing method have wide application prospects in the fields of aerospace, mechanical electronic products and low-temperature industries.
Description
Technical field
The invention belongs to high-entropy alloy and shape memory alloy material field, be specifically related to one and there is shape memory effect N
xm
yhigh-entropy alloy and preparation method thereof.
Background technology
The Shape memory mechanism of metal and high-entropy alloy is that crystalline structure has the rule that can change with temperature, and is subject to the impact of the composition, structure and phase transition etc. of material.Shape memory characteristic deformation-recovery coefficient represents.1963, the ratio of United States Navy's Armament Research Establishment is strangled and is found in research work, in certain temperature range more higher than room temperature, a kind of Ni-Ti alloy silk is burnt till spring, then in cold water, it is stretching or cast the shape such as square, trilateral, be placed in the hot water of more than 40 DEG C again, this B alloy wire just reverts to original spring shape.Found successively afterwards, some other alloy also has similar function.This class alloy is called as shape memory alloy.Shape memory alloy, owing to having the performance of many excellences, is thus widely used in multiple fields such as aerospace, mechano-electronic, biologic medical, bridge construction, automotive industry and daily life.The outburst of the fast development of aviation industry and mechano-electronic and biologic medical industry, cause market to different-alloy system, and different performance require sharp rise, impel the development in pluralism of shape memory alloy, shape memory alloy has developed into tens kinds at present, is also widely used in multiple fields such as aerospace, mechano-electronic, biologic medical, bridge construction, automotive industry and daily life because of the performance of its many excellence.Shape memory alloy has been applied to aviation and space device.As being used in the low temperature fit connection in the hydraulic efficiency system of military aircraft, Europe and the U.S. are developing for the shape memory alloy material in the level of intelligence rotor of vertisplane.Be restricted because the vibrations of vertisplane height and strong noise use, the source mainly blade vortex interference of its noise and vibrations, and the little deviation of vane type line.This just needs a kind of device of balance blade pitch, and each blade can accurately be rotated at same plane.Developed at present a kind of tracking controller of blade, it is the position with the little fin on a little shaped double tube shape memory alloys driver control blade edge track, makes it shake to drop to minimum.The temperature that common shape memory metal undergoes phase transition is generally more than room temperature, and shape memory temperature scope is narrower, and general high entropy metallic substance does not exist shape memory effect.
For meeting different shape memorial alloy required under differing temps, people have developed large quantities of high temperature or low temperature shape memory alloy, " shape memory " has been started since the practical stage from United States Navy's mechanical investigations in 1963, in succession develop Ni-Ti base, Cu-Al2-Ni base and Cu-Zn-Al base marmem, have developed Fe-Mn-Si base, the iron-base marmem such as stainless steel-based to the eighties in last century.After the nineties, high-temperature shape memory alloy, wide transformation hysteresis shape memory alloy become study hotspot.But there is the problem of following three aspects in existing market:
1) because high-entropy alloy is new metallic material, not yet in high-entropy alloy series, high entropy shape memory alloy is invented;
2) because shape memory alloy single-phase transformation temperature is more stable, regulate transformation temperature more difficult;
3) because general shape memory alloy phase transformation is in the more difficult generation of pole low temperature, so service temperature is higher, low temperature shape memory alloy kind is less.
Due to above reason, use existing shape memory to close and be difficult to meet industrial application requiring at low temperatures, hinder further developing of low-temperature industrial; In addition, high-entropy alloy invention shape memory alloy, utilize the feature of high-entropy alloy effectively to regulate phase transformation temperature points, that also impels phase transformation to occur is easier.Therefore research and development can be used for low temperature, the novel alloy of shape memory effect can be kept to become the recent studies on direction in field for this reason in larger temperature range.
Summary of the invention
The use temperature that content of the present invention exists for current shape memory alloy is limited, the more difficult adjustment of transformation temperature, and the feature of non-invention shape memory alloy in high-entropy alloy, propose a kind of N with shape memory effect
xm
yhigh-entropy alloy and preparation method thereof.
For achieving the above object, the N with shape memory effect of the present invention
xm
yhigh-entropy alloy, comprising: the N of 45% ~ the 55% and M of 45% ~ 55%.
Described N requires as two or more element in Ta, Nb, Hf, Zr, Ti, Mo, W, and the content of often kind of element is more than or equal to 5%, is less than or equal to 35%; M requires as two or more element in V, Mn, Fe, Co, Ni, Cr, Cu, Zn, and the content of often kind of element is more than or equal to 5%, is less than or equal to 35%; .
In alloy, the effect of principal element: N is high-melting point alloy element, is also the element promoting to be formed body-centered cubic structure simultaneously; M is the element promoting to be formed face-centred cubic structure, increases the randomness of element in structure, impels the precipitation of body-centered cubic B2 phase.
The shape-memory properties of alloy, except by except the composition influence of alloy, is also subject to the impact of the weave construction of alloy.Shape memory high-entropy alloy of the present invention adopts vacuum arc melting furnace melting, and direct pouring is shaping, and technique is very simple.
Preparation method of the present invention comprises the following steps:
Step one: the M getting 45% ~ 55% adds vacuum arc fumace, the N getting 45% ~ 55% adds vacuum arc melting furnace, is placed in M upper strata, is covered by M.
Step 2: open electric arc, first with little electric arc by upper strata N element burn red, afterwards electric current is tuned up make N melt after and lower floor M be fused together.
Step 3: several times alloy pig is placed in crucible again, and horizontal by the angle of 20 ° ~ 40 °, melt back 4 times and more than.
What preparation method of the present invention made has shape memory effect N
xm
ythere is shape memory effect in high-entropy alloy, have the characteristic of high-entropy alloy in wide temperature range simultaneously.This alloy is that structure is mainly the body-centered cubic single phase solid solution of more than 95% and a small amount of intermetallic compound.The parts that the high-entropy alloy with shape memory effect of the present invention works under being suitable for being applied to cold condition.
The advantage that the present invention is compared with prior art had is:
(1) alloy shape memory transformation temperature of the present invention is wider, can have shape memory effect in the temperature range of-196 to 600 degree, develops low temperature and the high-temperature shape memory alloy of brand-new series in existing shape memory alloy.
(2) compared with existing shape memory alloy, alloy of the present invention is high entropy shape memory alloy, has the performance that shape memory effect has high-entropy alloy simultaneously.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 alloy microstructure pattern SEM schemes
Fig. 2 is embodiment 1 alloy microstructure XRD figure
Fig. 3 is embodiment 1 alloy thermal analyses DSC curve
Fig. 4 is the stress-strain curve of loading-unloading under embodiment 1 alloy low temperature-be warmed up to more than austenite transformation temperature, shows that the distortion of alloy has returned to original state in temperature-rise period, has shape memory effect.
Fig. 5 is the diffraction curve in the loading-unloading process under embodiment 1 alloy high energy synchrotron radiation condition, shows that alloy there occurs reversible transformation in loading-unloading process.
Fig. 6 is that embodiment 2-in-1 payment organization structure and morphology SEM schemes
Fig. 7 is embodiment 2-in-1 payment organization structure XRD figure
Fig. 8 is the stress-strain curve of loading-unloading under the 2-in-1 golden low temperature of embodiment-be warmed up to more than austenite transformation temperature, shows that the distortion of alloy has returned to original state in temperature-rise period, has shape memory effect.
Embodiment
One, embodiment 1
1. alloying constituent
The alloying constituent of embodiment 1 is TaNbTiNiCoFe
2. the melting of alloy
The melting of alloy comprises the following steps:
Step one: get the crucible that 16.67%Ni, 16.67%Co, 16.67%Fe are placed in electric arc furnace, then get 16.67%Ta, 16.66%Nb, 16.66%Ti and place on first vegetarian noodles of formerly placing and covered.(element high for fusing point is placed on upper strata)
Step 2: open electric arc, first with little electric arc by red for the biscuiting of upper strata unit, afterwards electric current is tuned up and to make after the elements melt of upper strata together with lower floor elements melt.
Step 3: several times alloy pig is placed in crucible again, and horizontal by the angle of 20 ° ~ 40 °, melt back 4 times, obtains alloy pig.
3. the tissue signature of alloy and shape-memory properties
Can be found out the microtexture of prepared embodiment 1 alloy by Fig. 1 and Fig. 2, wherein dentrite is body center cubic solid solution, and intercrystalline distributes intermetallic compound on a small quantity, and sosoloid accounts for more than 95%.DSC thermal analysis curve as shown in Figure 3 can be found out,-35.8 DEG C time, a martensite type phase transformation is there is during cooling, phase transformation peak value appears at-84.3 DEG C, a reverse transformation is there is when heating up, reverse transformation starting temperature is-38.1 DEG C, illustrates that the embodiment of the present invention exists reversible transformation when temperature variation.Alloy is compressed at low temperatures, its stress-strain curve (as Fig. 4) is the deformation curve of typical memorial alloy type, alloy is warmed up to room temperature, time namely more than Reverse Martensitic Transformation Temperatures, can see that alloy is returned to initial length completely, show to there occurs shape memory effect.By to invention alloy be out of shape under high energy synchrotron radiation, its structural changes in deformation process of home position observation, as shown in Figure 5, the phase transformation that there occurs the sub-phase of parent phase-> in loading procedure can be found, and in uninstall process, there occurs the reverse transformation of sub-phase-> parent phase, show that shape memory effect of the present invention is caused by the shape memory effect that parent phase is alternate with son.
Two, embodiment 2
1. alloying constituent
The alloying constituent of embodiment 2 is TiZrFeNi.
2. the melting of alloy
The melting of alloy comprises the following steps:
Step one: get the crucible that 25%Ni, 25%Fe are placed in electric arc furnace, then get 25%Ti, 25%Zr and place on first vegetarian noodles of formerly placing and covered.(element high for fusing point is placed on upper strata)
Step 2: open electric arc, first with little electric arc by red for the biscuiting of upper strata unit, afterwards electric current is tuned up and to make after the elements melt of upper strata together with lower floor elements melt.
Step 3: several times alloy pig is placed in crucible again, and horizontal by the angle of 20 ° ~ 40 °, melt back 4 times, obtains alloy pig.
3. the tissue signature of alloy and shape-memory properties
Fig. 6 and Fig. 7 by XRD and the SEM shape appearance figure of invention alloy embodiment, can find out that the microtexture of prepared embodiment alloy is formed primarily of single phase solid solution, wherein dentrite is single phase solid solution, and intercrystalline distributes intermetallic compound on a small quantity.Compressed at low temperatures by alloy, its stress-strain curve as shown in Figure 8, shows as the deformation curve of typical memorial alloy type, alloy is warmed up to room temperature, time namely more than Reverse Martensitic Transformation Temperatures, can see that alloy is returned to initial length completely, show to there occurs shape memory effect.
In sum, alloy provided by the present invention has the wide temperature range be suitable for, especially there is excellent shape-memory properties under cryogenic, alloy of the present invention has composition and the characteristics of organizational structure of high-entropy alloy simultaneously, also there is the characteristic of high-entropy alloy, while the present invention has reoffered the shape memory alloy of excellent performance, provide a kind of based on the shape memory alloy design under high-entropy alloy design concept.
Claims (3)
1. one kind has the N of shape memory effect
xm
yhigh-entropy alloy, is characterized in that, the atom percentage content of N and M is 45% ~ 55%,
N requires as two or more in Ti, Zr, Hf, Ta, Nb, Mo, W, and the content of often kind of element is more than or equal to 5%, is less than or equal to 35%; M requires as two or more in V, Mn, Fe, Co, Ni, Cr, Cu, Zn element, and the content of often kind of element is more than or equal to 5%, is less than or equal to 35%.
2. one has shape memory effect N as claimed in claim 1
xm
ythe preparation method of high-entropy alloy, is characterized in that comprising following step:
Step one: the M getting 45% ~ 55% adds vacuum arc fumace, the N getting 45% ~ 55% adds vacuum arc melting furnace, is placed in M upper strata, is covered by M, requires element high for fusing point to be placed on upper strata during smelting;
Step 2: open electric arc, first with little electric arc by upper strata N element burn red, afterwards electric current is tuned up make N melt after and lower floor M be fused together;
Step 3: several times alloy pig is placed in crucible again, and horizontal by the angle of 20 ° ~ 40 °, melt back 4 times and more than.
3. as claimed in claim 2 there is shape memory effect N
xm
ythe preparation method of high-entropy alloy, is characterized in that: N
xm
ythere is shape memory effect in high-entropy alloy, have the characteristic of high-entropy alloy in the temperature range of-196 to 600 degrees Celsius simultaneously; This alloy is that structure is mainly the body-centered cubic single phase solid solution of more than 95% and a small amount of intermetallic compound.
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