Effect of solution treatment and aging on microstructural evolution and mechanical behavior of NiTi shape memory alloy

As-received nickel-titanium （NiTi） shape memory alloy with a nominal composition of Ni50.9Ti49.1 （mole fraction,%） was subjected to solution treatment at 1123 K for 2 h and subsequent aging for 2 h at 573 K, 723 K and 873 K, respectively. The influence of solution treatment and aging on microstructural evolution and mechanical behavior of NiTi alloy was systematically investigated by transmission electron microscopy （TEM）, high resolution transmission electron microscopy （HRTEM）, scanning electron microscopy （SEM） and compression test. Solution treatment contributes to eliminating the Ti2Ni phase in the as-received NiTi sample, in which the TiC phase is unable to be removed. Solution treatment leads to ordered domain of atomic arrangement in NiTi alloy. In all the aged NiTi samples, the Ni4Ti3 precipitates, the R phase and the B2 austenite coexist in the NiTi matrix at room temperature, while the martensitic twins can be observed in the NiTi samples aged at 873 K. In the NiTi samples aged at 573 and 723 K, the fine and dense Ni4Ti3 precipitates distribute uniformly in the NiTi matrix, and thus they are coherent with the B2 matrix. However, in the NiTi sample aged at 873 K, the Ni4Ti3 precipitates exhibit the very inhomogeneous size, and they are coherent, semi-coherent and incoherent with the B2 matrix. In the case of aging at 723 K, the NiTi sample exhibits the maximum yield strength, where the fine and homogeneous Ni4Ti3 precipitates act as the effective obstacles against the dislocation motion, which results in the maximum critical resolved shear stress for dislocation slip.

Transformation behavior and shape memory effect of Ti_(50-x)Ni_(48)Fe_2Nb_x alloys by aging treatment

The influence of aging treatment on transformation behavior and shape memory of the Ti 50_x Ni_(48) Fe_2 Nb_x(x=0,0.6,0.8,1.0,and 1.2) alloys was investigated using differential scanning calorimeter(DSC),mechanical drawing machine,and microhardness tester in this paper.It is indicated that the aging treatment has a significant effect on the phase transformation temperatures(M_s,M_f,M_p,A_s,A_f,and A_p) and microhardness of the samples.The phase transformation temperatures are found to decrease initially with the increasing aging temperature from 300 to 500 ℃ and increase with further increase of the aging temperature.The aging treatment at intermediate temperature between 400 and 500 ℃ results in an improved shape memory effect.In addition,the highest microhardness value is also obtained.

Aging-induced two-stage reverse martensitic transformation behavior in Co_(46)Ni_(27)Ga_(27) high-temperature shape memory alloy

The effect of austenite aging at 823 K on the microstructures and martensitic transformation behavior of Co 46 Ni 27 Ga 27 alloy has been investigated using optical microscopy （OM）, transmission electron microscopy （TEM）, X-ray diffraction analysis （XRD）, and differential scanning calorimeter （DSC）. The microstructure observation results show that the unaged Co 46 Ni 27 Ga 27 alloy is composed of the tetragonal nonmodulated martensite phase and face-centered cubic γ phase. It is found that a new nanosized fcc phase precipitates in the process of austenite aging, leading to the formation of metastable age-affected martensite around the precipitates with composition inhomogeneity. Two-stage reverse martensitic transformation occurs in the samples aged for 2 and 24 h due to the composition difference between the age-affected martensite and the original martensite. For the Co 46 Ni 27 Ga 27 alloy aged for 120 h, no reverse transformation can be detected due to the disappearance of the metastable age-affected martensite and the small latent heat of the original martensite. The martensitic transformation temperatures of the Co 46 Ni 27 Ga 27 alloy decrease with an increase in aging time.

Isothermal Aging Kinetics in CuZnAl Shape Memory Alloy

Isothermal aging behaviours of a CuZnAl shape memory alloy have been investigated by means of dilatometry.The length of the specimens during isothermal aging from 190 to 280℃ increases with the aging time at each temperature.The isothermal aging kinetics fits in Avrami equation and the time exponent n decreases with the increase in aging temperature.The apparent activation energy for the isothermal aging process was measured to be 109.0kJ/mol,which is about equal to that of a relaxation internal friction peak at about 200℃ (f≈1 Hz) in the alloy.

Effects of aging on the microstructure of a Cu-Al-Ni-Mn shape memory alloy

The influence of aging on the microstructure and mechanical properties of Cu-11.6wt%Al-3.9wt%Ni-2.5wt%Mn shape memory alloy（SMA） was studied by means of scanning electron microscopy（SEM）,transmission electron microscopy（TEM）,X-ray diffractometer,and differential scanning calorimeter（DSC）.Experimental results show that bainite,γ2,and α phase precipitates occur with the aging effect in the alloy.After aging at 300°C,the bainitic precipitates appear at the early stages of aging,while the precipitates of γ2 phase are observed for a longer aging time.When the aging temperature increases,the bainite gradually evolves into γ2 phase and equilibrium α phase（bcc） precipitates from the remaining parent phase.Thus,the bainite,γ2,and α phases appear,while the martensite phase disappears progressively in the alloy.The bainitic precipitates decrease the reverse transformation temperature while the γ2 phase precipitates increase these temperatures with a decrease of solute content in the retained parent phase.On the other hand,these precipitations cause an increasing in hardness of the alloy.

Martensitic stabilization and defects induced by deformation in TiNi shape memory alloys

Martensitic stabilization caused by deformation in a TiNi shape memory alloy was studied.Special attention was paid to the deformed microstructures to identify the cause of martensitic stabilization.Martensitic stabilization was demonstrated by differential scanning calorimetry for the tensioned TiNi shape memory alloy.Transmission electron microscopy revealed that antiphase boundaries were formed because of the fourfold dissociation of [110]B19＇ super lattice dislocations and were preserved after reverse transformation due to the lattice correspondence.Martensitic stabilization was attributed to dislocations induced by deformation,which reduced the ordering degree of the microstructure,spoiled the reverse path from martensite to parent phase compared with thermoelastic transformation,and imposed resistance on phase transformation through the stress field.

Martensite Aging Effect and Thermal Cyclic Characteristics in Ti-Pd and Ti-Pd-Ni High Temperature Shape Memory Alloys

The effect of thermal cycling and aging in martensitic state in Ti-Pd-Ni alloys were investigated by DSC and TEM observations. It is shown that the thermal cycling causes the decreases in M, and Af temperatures in Ti50Pd50-xNix (x=10, 20, 30) alloys, but no obvious thermal cycling effect was observed in Ti50Pd50Pd40Ni10 alloys and the aging effect shows a curious feature, i.e., the Af temperature does not saturate even after relatively long time aging, which is considered to be due to the occurrence of recovery recrystallization during aging.

Formation Mechanism of Curved Martensite Structures in Cu-based Shape Memory Alloys

The curved martensite structures have been observed in CuZnAI-based shape memory alloys by both transmission electron microscope and optical microscope. It was found that the curved martensite structures observed in as-solution treated, as-aged and as-trained alloys usually occurred around dislocation tangles or precipitate, at the plate boundary or grain boundary, and when the growing plates collided with each other or alternate mutually.

Effects of aging treatment on the microstructure and superelasticity of columnar-grained Cu71Al18Mn11 shape memory alloy

The effect of aging treatment on the superelasticity and martensitic transformation critical stress in columnar-grained Cu_（71）Al_（18）Mn_（11） shape memory alloy（SMA） at the temperature ranging from 250°C to 400°C was investigated. The microstructure evolution during the aging treatment was characterized by optical microscopy, scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. The results show that the plate-like bainite precipitates distribute homogeneously within austenitic grains and at grain boundaries. The volume fraction of bainite increases with the increase in aging temperature and aging time, which substantially improves the martensitic transformation critical stress of the alloy, whereas the bainite only slightly affects the superelasticity. This behavior is attributed to a coherent relationship between the bainite and the austenite, as well as to the bainite and the martensite exhibiting the same crystal structure. The variations of the martensitic transformation critical stress and the superelasticity of columnar-grained Cu_（71）Al_（18）Mn_（11） SMA with aging-temperature and aging time are described by the Austin-Rickett equation, where the activation energy of bainite precipitation is 77.2 kJ ·mol1. Finally, a columnar-grained Cu_（71）Al_（18）Mn_（11） SMA with both excellent superelasticity（5%-9%） and high martensitic transformation critical stress（443-677 MPa） is obtained through the application of the appropriate aging treatments.

Microstructure and diffraction pattern changes resulted from long-term aging of martensite CuZnAlMnNi shape memory alloy

Microstructures of a CuZnAlMnNi shape memory alloy in the as-quenched andlong-term aged conditions were investigated by transmission electron microscopy. Aged for one yearin martensite phase, an equilibrium α-phase with fcc structure was observed in the M18R martensitematrix, accompanied by the appearance of a novel diffraction pattern. By analysis, it was suggestedthat the novel pattern results from the α-phase and the martensite matrix remaining in seven fineplates which produce intense secondary diffraction effect when the diffraction beams enter from onephase into another.

ON THE STABILIZATION OF THERMOELASTIC MARTENSITE IN A Cu-Zn-Al ALLOY

The stabilization of thermoelastic martensite in a rapidly solidified Cu-Zn-A1 alloy is be- lieved to be the process of disordering in atomic configuration during which the structure of martensite gradually transforms into N9R(b/a=1/3^(1/2))from M18R.This is dependent upon the intrinsic decomposition tendency of the martensite.

QUENCH IN STABILIZATION OF Cu-Zn-Al ALLOY

ＱＵＥＮＣＨＩＮＳＴＡＢＩＬＩＺＡＴＩＯＮＯＦＣｕＺｎＡｌＡＬＬＯＹ①ＰｅｎｇＫｕｎ，ＴａｎＳｈｕｓｏｎｇ，ＬｉＳｈｕｔａｎｇＤｅｐａｒｔｍｅｎｔｏｆＭａｔｅｒｉａｌｓＳｃｉｅｎｃｅａｎｄＥｎｇｉｎｅｒｉｎｇ，ＣｅｎｔｒａｌＳｏｕｔｈＵｎｉｖｅｒ...

Improvement of tensile superelasticity by aging treatment of NiTi shape memory alloys fabricated by electron beam wire-feed additive manufacturing

For the first time,this work comprehensively studied the effectiveness of precipitation hardening achieved by aging treatment in improving the tensile superelasticity of NiTi alloys fabricated by elec-tron beam wire-feed additive manufacturing(EBAM),which possesses inherent advantages in producing dense and oxidation-free structures.Aging treatments under three temperatures(450,350,and 250℃)and different durations were conducted,and the resultant performance of tensile superelasticity,together with the corresponding evolution of precipitation and phase transformation behavior were investigated for the EBAM-fabricated NiTi alloys.Results showed that by appropriate aging treatment,EBAM fabricated NiTi alloys could achieve excellent recovery rates of approximately 95%and 90%after the 1st and 10th load/unload cycle for a maximum tensile strain of 6%,which were almost the highest achieved so far by AM processed NiTi alloys and close to those of some conventional NiTi alloys.The improvement of tensile superelasticity benefited from the fine and dispersive Ni4Ti3 precipitates,which could be introduced by aging at 350℃ for 4 h or at 250℃ for 200 h.Moreover,the large amount of Ni4Ti3 precipitates would promote the intermediate R-phase transformation and bring a two-stage or three-stage transformation sequence,which depended on whether the distribution of the precipitation was homogeneous or not.This work could provide guidance for the production of NiTi alloys with good tensile superelasticity by EBAM or other additive manufacturing processes.

Influence of aging on damping behavior of TiNi/TiNi alloys synthesized by explosive welding

The influence of aging time,measuring frequency and strain amplitude on the internal friction of TiNi51/TiNi50.2 sandwich composite was investigated.The DSC and internal friction measurements were employed to characterize the sample.The two internal friction peaks of the specimen were confirmed corresponding to the reverse transformation of TiNi51 and TiNi50.2 component, respectively.The internal friction as a function of the temperature at different measuring frequencies was presented and it was found that the height of both internal friction peaks increased with decreasing frequency;however,the increase corresponding to TiNi50.2 component was larger than that of TiNi51 component.Furthermore,the internal friction of the TiNi/TiNi composite alloy decreased with increasing the measuring strain amplitude.The height of internal friction peak of TiNi51 component increased with increasing the aging time,whereas that of the TiNi50.2 component did not change significantly.The increase in internal friction of TiNi51 appeared to be associated with the formation and growth of precipitate during the aging process.

Structure design of high-performance Cu-based shape memory alloys

The effects of various structure factors on the properties(superelasticity mainly) of Cu-based shape memory alloys(SMAs) were systematically evaluated in this review article through literatures combining with our work. It is concluded that besides the decisive role of grain orientation, the grain boundary(GB) characteristics also play important roles in the superelasticity, which include GB area, GB type, GB morphology and GB direction in descending order of the effect significance. According to the above results, the prior principles of structure design are proposed for high-performance Cu-based SMAs from most to least important:(1) obtaining grain orientation with high phase transformation strain;(2) increasing grain size or reducing GB area;(3) obtaining straight low-energy GBs, especially low-angle GBs;(4) trying to make GB direction parallel to external stress. Consistent with the main or all principles, the bamboo-like-grained and columnar-grained(CG) Cu-based SMAs show excellent comprehensive properties.

Phase Transformation and Thermal Stability of Aged Ti-Ni-Hf High Temperature Shape Memory Alloys

The use of Ni-rich TiNiHf alloys as high temperature shape memory alloys （SMAs） through aging has been presented. For Ni-rich Ti80-xNixHf20 alloys, their phase transformation temperatures are averagely increased more than 100 K by aging at 823 K for 2 h. Especially for the alloys with Ni-content of 50.4 at. pct and 50.6 at. pct, their martensitic transformation start temperatures （Ms） are more than 473 K after aging. TEM observation confirmed that some fine particles precipitate from the matrix during aging. The aged Ni-rich TiNiHf SMAs show the better thermal stability of phase transformation temperatures than the solutiontreated TiNiHf alloys. The fine particles precipitated during aging should be responsible for the increase of phase transformation temperatures and its high stability.

Shape Memory Behavior of [111]-Oriented NiTi Single Crystals After Stress-Assisted Aging

The shape memory behavior of [111]-oriented Ni_（51）Ti_（49） （at.%） single crystals was investigated after stressassisted aging at 500 °C for 1.5 h under a compressive stress of-150 MPa.It was found that a single family of Ni_4Ti_3 precipitates with two crystallographically equivalent variants was formed after aging under compressive stress.Stressassisted aging resulted in tensile two-way shape memory effect strain of 1.56% under-5 MPa.Thermal cycling under-600 MPa resulted in a transformation strain of-2.15%,while the subsequent thermal cycling under-5 MPa resulted in a tensile two-way shape memory effect strain of 2.2%.

STABILITIY OF MARTENSITE IN Cu-Zn-Al SHAPE MEMORY ALLOY AFTER DIRECT OR STEPPED QUENCHING

The stability of thermoelastic martensite in a Cu-14.84 wt-％Zn-7.75 wt-％Al shape mem- ory alloy with M_s=106°C after direct quenching or stepped quenching has been investigated by using TEM,X-ray diffroctometer and double electric bridge instrument.The martensite aged for about 3 h at room temperature after either direct quenching or stepped quenching (150°C,2 rain)is the M18R structure.The martensite just directly quenched is not so stable, both its certain diffraction peaks and specific electric resistivity,change with aging at room temperature;whereas it is stable after stepped quenching(150°C.2 min),and its diffraction peaks and specific electric resistivity change no more with aging at room temperature.The above mentioned results seem to be explained by the martensite reordering.

Effect of Ageing on Martensitic Transformation and Shape Memory Effect of Fe-Mn-Si-Co-Mo Alloy

This paper discusses the effect of ageing on the thermally induced martensitic transformation and its reverse transformation and shape memory effect of Fe-24Mn-5Si-8Co-4Mo shape memory alloy:the precipitation of Fe 2Mo particles increases the hardness and strength of the alloy as ageing goes on;ageing increases the transformation temperatures;ageing improves,the SME of the alloy so remarkably that a maximum shape recovery ratio is obtained while ageing at 600℃.

THE FAILURE MECHANISM OF REVERSE SHAPE MEMORYEFFECT IN A Cu-BASE ALLOY

The interior structural evolution accompanying reverse shape memory effect (RSMEin a Cu-Zn-Al alloy was studied by means of transmission electron microscopy. It was found that RSME is closely related to bainitic transformation in this alloy during the isothermal reaction at moderate temperatures. At a given temperature and a certain external constraint stress, the shape memory effect depends mainly on the aging time.During the early stage, the shape memory effect enhances with the increase of reactiotn time. Then it will decrease gradually apon further aging. If the alloy is overaged, the stacking faults of bainite will disappear gradually by the motion of partial dislocations through which long range diffusion of solute atoms takes place, giving rise to the deterioration of RSME. When all the bainite transforms to α phase, RSME will lose completely.