CN105296836B - A kind of N with SMExMyHigh-entropy alloy and preparation method thereof - Google Patents
A kind of N with SMExMyHigh-entropy alloy and preparation method thereof Download PDFInfo
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- CN105296836B CN105296836B CN201510788841.8A CN201510788841A CN105296836B CN 105296836 B CN105296836 B CN 105296836B CN 201510788841 A CN201510788841 A CN 201510788841A CN 105296836 B CN105296836 B CN 105296836B
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Abstract
The present invention relates to a kind of N with SMExMyHigh-entropy alloy and preparation method thereof, the chemical composition of alloy are as follows：45≤x≤55,45≤y≤55, N are any two or more than two kinds in Ti, Zr, Hf, V, Nb, Ta, Mo and W, and the content of every kind of element is more than or equal to 5%, less than or equal to 35%；M be in V, Mn, Fe, Co, Ni, Cu, Cr and Zn any two or it is a variety of, and the content of every kind of element be more than or equal to 5%, less than or equal to 35%.Phase structure of alloy involved in the present invention is：Body-centered cubic single phase solid solution and intermetallic compound of the volume fraction not less than 95%.The alloy is prepared using the method for electric arc melting.Alloy involved in the present invention has SME in wide temperature range, while has the characteristic of high-entropy alloy.Had broad application prospects in aerospace field, mechano-electronic product, low-temperature industrial field.
Description
Technical field
The invention belongs to high-entropy alloy and shape memory alloy material field, and in particular to one kind has SME
NxMyHigh-entropy alloy and preparation method thereof.
Background technology
The Shape memory mechanism of metal and high-entropy alloy is that crystal structure has the rule that can be changed with temperature, and
Influenceed by the composition of material, structure and phase transformation etc..Shape memory characteristic is represented with deformation-recovery coefficient.1963, the U.S.
The ratio of naval ordnance research institute is strangled and found in research work, in certain temperature range more higher than room temperature, a kind of Ni-Ti
B alloy wire burns till spring, and then it is stretched or casts the shapes such as square, triangle in cold water, then is placed on more than 40 DEG C
In hot water, the B alloy wire just reverts to original spring shape.Find successively later, other some alloys also have similar work(
Energy.This kind of alloy is referred to as marmem.Marmem extensively should due to many excellent performances
For multiple fields such as Aero-Space, mechano-electronic, biologic medical, bridge construction, auto industry and daily lifes.Aviation industry
Fast development and mechano-electronic and biologic medical industry outburst, cause market to different-alloy system, and different performance
It is required that sharp rise, promoted the development in pluralism of marmem, marmem has developed to tens kinds at present,
Also it is widely used in Aero-Space, mechano-electronic, biologic medical, bridge construction, auto industry because of its many excellent performance
And the multiple fields such as daily life.Marmem has application to aviation and space device.Such as it is used in the hydraulic pressure of military aircraft
Low temperature fit connection in system, Europe and the U.S. are developing the shape note in the level of intelligence rotor for helicopter
Recall alloy material.Because the high vibrations of helicopter and strong noise use are restricted, the source of its noise and vibrations is mainly leaf
Piece vortex interference, and the little deviation of vane type line.This just needs a kind of device of balance blade pitch, enables each blade essence
Really rotated in same plane.A kind of tracking controller of blade is developed at present, it is remembered with a small two-tube shape
Recall the position of the small fin on alloy driver control blade edge track, be preferably minimized its vibrations.Common shape memory
The temperature that metal is undergone phase transition is typically more than room temperature, and shape memory temperature scope is narrower, the high entropy metal material of in general
In the absence of SME.
For the variously-shaped memorial alloy needed for meeting under different temperatures, people have developed large quantities of high temperature or low temperature shapes
Memorial alloy, " shape memory " has been started since the practical stage from USN's mechanical investigations in 1963, develops Ni-Ti in succession
Base, Cu-Al2-Ni bases and Cu-Zn-Al base marmems, Fe-Mn-Si bases, stainless are have developed to the 80's of last century
The iron-base marmems such as base steel.High-temperature shape memory alloy, wide transformation hysteresis marmem turn into research heat after the nineties
Point.But there is the problem of following three aspects in existing market：
1) because high-entropy alloy is new metallic material, not yet the high entropy shape memory of invention closes in high-entropy alloy series
Gold；
2) because marmem single-phase phase transition temperature is relatively stable, regulation phase transition temperature is more difficult；
3) because the phase transformation of general shape memorial alloy is in the more difficult generation of extremely low temperature, so service temperature is higher, low temperature shape
Memorial alloy species is less.
Due to above reason, closed using existing shape memory and be difficult to meet industrial application requirement at low temperature, resistance
The further development of low-temperature industrial is hindered；It is effective the characteristics of using high-entropy alloy in addition, high-entropy alloy invention marmem
Phase transformation temperature pointses are adjusted, also promote being easier for phase transformation generation.Therefore research and development can be kept available for low temperature, in larger temperature range
The novel alloy of SME turns into the recent studies on direction in this field.
The content of the invention
Present invention is limited for temperature in use existing for current marmem, the more difficult regulation of phase transition temperature, and
In high-entropy alloy the characteristics of non-invention marmem, it is proposed that a kind of N with SMExMyHigh-entropy alloy and
Its preparation method.
To reach above-mentioned purpose, the N with SME of the inventionxMyHigh-entropy alloy, including：45%~
55% N and 45%~55% M.
Described N requirements are two or more elements in Ta, Nb, Hf, Zr, Ti, Mo, W, and the content of every kind of element is big
In equal to 5%, less than or equal to 35%；M requirements are two or more elements in V, Mn, Fe, Co, Ni, Cr, Cu, Zn, and every kind of
The content of element is more than or equal to 5%, less than or equal to 35%；.
The effect of essential element in alloy：N is high-melting point alloy element, while is also to promote to form body-centered cubic structure
Element；M is the element for promoting to be formed face-centred cubic structure, increases the randomness of element in structure, promotes body-centered cubic B2 phases
Separate out.
The shape-memory properties of alloy are also influenceed in addition to the composition influence by alloy by the institutional framework of alloy.This
The shape memory high-entropy alloy of invention uses vacuum arc melting furnace melting, and direct pouring is molded, and technique is very simple.
The preparation method of the present invention comprises the following steps：
Step 1：Take 45%~55% M to add vacuum arc furnace ignition, take 45%~55% N to add vacuum arc melting
Stove, M upper stratas are placed in, M is covered.
Step 2：Open electric arc, first with small electric arc by upper strata N element burn it is red, electric current is tuned up afterwards make N melt after with
Layer M is fused together.
Step 3：Alloy pig is placed in crucible several times again, and horizontal by 20 °~40 ° of angle, melt back
4 times and more than.
There is SME N made of the preparation method of the present inventionxMyHigh-entropy alloy exists in wide temperature range
SME, while there is the characteristic of high-entropy alloy.The alloy is the body-centered cubic that structure is mainly more than 95%
Single phase solid solution and a small amount of intermetallic compound.The high-entropy alloy with SME of the present invention is properly applied to low temperature
Under the conditions of the part that works.
Present invention advantage possessed compared with prior art is：
(1) alloy shape memory phase transition temperature of the present invention is wider, can have shape within the temperature range of -196 to 600 degree
Memory effect, the low temperature and high-temperature shape memory alloy of brand-new series are developed in existing marmem.
(2) compared with existing marmem, alloy of the present invention is high entropy marmem, has shape memory effect
There should be the performance of high-entropy alloy simultaneously.
Brief description of the drawings
Fig. 1 schemes for the alloy microstructure pattern SEM of embodiment 1
Fig. 2 is the alloy microstructure XRD of embodiment 1
Fig. 3 is the alloy heat analysis DSC curve of embodiment 1
Fig. 4 is that loading-unloading-be warming up to stress-strain more than austenite transformation temperature is bent under the alloy low temperature of embodiment 1
Line, show that the deformation of alloy has returned to original state in temperature-rise period, there is SME.
Fig. 5 is the diffraction curve during the loading-unloading under the conditions of the alloy high energy synchrotron radiation of embodiment 1, shows to close
There occurs reversible transition during loading-unloading for gold.
Fig. 6 is the 2-in-1 payment organization structure and morphology SEM figures of embodiment
Fig. 7 is the 2-in-1 payment organization structure XRD of embodiment
Fig. 8 is that loading-unloading-be warming up to stress-strain more than austenite transformation temperature is bent under the 2-in-1 golden low temperature of embodiment
Line, show that the deformation of alloy has returned to original state in temperature-rise period, there is SME.
Embodiment
First, embodiment 1
1. alloying component
The alloying component of embodiment 1 is TaNbTiNiCoFe
2. the melting of alloy
The melting of alloy comprises the following steps：
Step 1：Take 16.67%Ni, 16.67%Co, 16.67%Fe to be placed in the crucible in electric arc furnaces, then take
16.67%Ta, 16.66%Nb, 16.66%Ti are placed to be covered on the first vegetarian noodles formerly placed.(the high element of fusing point is put
On upper strata)
Step 2：Electric arc is opened, first with small electric arc that upper strata member biscuiting is red, tune up electric current makes upper strata elements melt afterwards
Afterwards with lower floor elements melt together with.
Step 3：Alloy pig is placed in crucible several times again, and horizontal by 20 °~40 ° of angle, melt back
4 times, obtain alloy pig.
3. tissue signature and the shape-memory properties of alloy
The microstructure of the prepared alloy of embodiment 1 is can be seen that by Fig. 1 and Fig. 2, wherein dendrite is consolidated for body-centered cubic
Solution, intercrystalline are distributed intermetallic compound on a small quantity, and solid solution accounts for more than 95%.DSC thermal analysis curves as shown in Figure 3 can be with
Find out a martensite type phase transformation at -35.8 DEG C be present during cooling, phase transformation peak value appears in -84.3 DEG C, exists in heating
One reverse transformation, reverse transformation initial temperature are -38.1 DEG C, illustrate that the embodiment of the present invention has reversible transition in temperature change.
Alloy is compressed at low temperature, its load-deformation curve (such as Fig. 4) is the deformation curve of typical memorial alloy type, will be closed
When gold is warming up to more than room temperature, that is, Reverse Martensitic Transformation Temperatures, it can be seen that alloy returns fully to initial length, show there occurs
SME.By to invention alloy deformed under high energy synchrotron radiation, its knot in deformation process of home position observation
Structure change, as shown in figure 5, it can be found that in loading procedure there occurs parent phase->The phase transformation of sub- phase, and occur in uninstall process
Sub- phase->The reverse transformation of parent phase, the SME for showing the present invention are made by the alternate SME of parent phase and son
Into.
2nd, embodiment 2
1. alloying component
The alloying component of embodiment 2 is TiZrFeNi.
2. the melting of alloy
The melting of alloy comprises the following steps：
Step 1：Take 25%Ni, 25%Fe to be placed in the crucible in electric arc furnaces, then take 25%Ti, 25%Zr to place formerly
Covered on first vegetarian noodles of placement.(the high element of fusing point is placed on upper strata)
Step 2：Electric arc is opened, first with small electric arc that upper strata member biscuiting is red, tune up electric current makes upper strata elements melt afterwards
Afterwards with lower floor elements melt together with.
Step 3：Alloy pig is placed in crucible several times again, and horizontal by 20 °~40 ° of angle, melt back
4 times, obtain alloy pig.
3. tissue signature and the shape-memory properties of alloy
Fig. 6 and Fig. 7 for institute's invention alloy embodiment XRD and SEM shape appearance figures, it can be seen that prepared embodiment alloy
Microstructure is mainly made up of single phase solid solution, and wherein dendrite is single phase solid solution, and intercrystalline is distributed intermetallic on a small quantity
Thing.Alloy is compressed at low temperature, its load-deformation curve is as shown in figure 8, show as the deformation of typical memorial alloy type
Curve, when alloy is warming up to more than room temperature, that is, Reverse Martensitic Transformation Temperatures, it can be seen that alloy returns fully to initial length,
Show that there occurs SME.
In summary, alloy provided by the present invention has wide applicable temperature range, especially has under cryogenic
There are excellent shape-memory properties, while alloy of the present invention has the composition and characteristics of organizational structure of high-entropy alloy, it may have high
The characteristic of entropy alloy, while the present invention provides the marmem of excellent performance again, there is provided one kind is closed based on high entropy
Marmem design under golden design concept.
Claims (1)
- A kind of 1. N with SMExMyHigh-entropy alloy, it is characterised in that N and M atom percentage content is 45% ~55%,N requirements are two or more in Ti, Zr, Hf, Ta, Nb, Mo, W, and the content of every kind of element is more than or equal to 5%, Less than or equal to 35%；M requirements are two or more in V, Mn, Fe, Co, Ni, Cr, Cu, Zn element, and every kind of element Content is more than or equal to 5%, less than or equal to 35%；The preparation method of the high-entropy alloy, including following steps：Step 1：Take 45%~55% M to add vacuum arc furnace ignition, take 45%~55% N to add vacuum arc melting furnace, put In M upper stratas, M is covered, requires during smelting the high element of fusing point being placed on upper strata；Step 2：Open electric arc, first with small electric arc by upper strata N element burn it is red, electric current is tuned up afterwards make N melt after with lower floor M It is fused together；Step 3：Alloy pig is placed in crucible several times again, and horizontal by 20 °~40 ° of angle, melt back 4 times More than and；NxMyThere is SME in high-entropy alloy, while have high-entropy alloy within the temperature range of -196 to 600 degrees Celsius Characteristic；Body-centered cubic single phase solid solution and a small amount of intermetallic compound of the alloy for structure more than 95%.
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