Influence of Substrate Temperature and Deposition Rate on Structural and Mechanical Properties of Shape Memory NiTi Films

NiTi thin films deposited by DC magnetron sputtering of an alloy (Ni/Ti:45/55) target at different deposition rates and substrate temperatures were analyzed for their structure and mechanical properties. The crystalline structure, phase-transformation and mechanical response were characterized by X-ray diffraction (XRD), Differential Scanning Calorimetry (DSC) and Nano-indentation techniques, respectively. The films were deposited on silicon substrates maintained at temperatures in the range 300 to 500 degrees C and post-annealed at 600 degrees C for four hours to ensure film crystallinity. Films deposited at 300 degrees C and annealed for 600 degrees C have exhibited crystalline behavior with Austenite phase as the prominent phase. Deposition onto substrates held at higher deposition temperatures (400 and 500 degrees C) resulted in the co-existence of Austenite phase along with Martensite phase. The increase in deposition rates corresponding to increase in cathode current from 250 to 350 mA has also resulted in the appearance of Martensite phase as well as improvement in crystallinity. XRD analysis revealed that the crystalline film structure is strongly influenced by process parameters such as substrate temperature and deposition rate. DSC results indicate that the film deposited at 300 degrees C had its crystallization temperature at 445 degrees C in the first thermal cycle, which is further confirmed by stress temperature response. In the second thermal cycle the Austenite and Martensite transitions were observed at 75 and 60 degrees C respectively. However, the films deposited at 500 degrees C had the Austenite and Martensite transitions at 73 and 58 degrees C, respectively. Elastic modulus and hardness values increased from 93 to 145 GPa and 7.2 to 12.6 GPa, respectively, with increase in deposition rates. These results are explained on the basis of change in film composition and crystallization. (C) 2010 Published by Elsevier Ltd

Optimization of cold and warm workability in 304 stainless steel using instability maps

The deformation characteristics of stainless steel type AISI 3O4 under compression in the temperature range 20 degrees C to 600 degrees C and strain-rate range 0.001 to 100 s(-1) have been studied with a view to characterizing the flow instabilities occurring in the microstructure. At strain rates less than 5 s(-1), 304 stainless steel exhibits flow localization, whereas dynamic strain aging occurs at intermediate temperatures and below 0.5 s(-1). At room temperatures and strain rates less than 10 s(-1), martensite formation is observed. To avoid the preceding microstructural instabilities, cold and warm working should be carried out at strain rates greater than 5 s(-1). The continuum criterion, developed on the basis of the principles of maximum rate of entropy production and separability of the dissipation function, predicts accurately all the preceding instability features.

Effect of laser processing parameters on the structure of ductile iron

Laser processing of structure sensitive hypereutectic ductile iron, a cast alloy employed for dynamically loaded automative components, was experimentally investigated over a wide range of process parameters: from power (0.5-2.5 kW) and scan rate (7.5-25 mm s(-1)) leading to solid state transformation, all the way through to melting followed by rapid quenching. Superfine dendritic (at 10(5) degrees C s(-1)) or feathery (at 10(4) degrees C s(-1)) ledeburite of 0.2-0.25 mu m lamellar space, gamma-austenite and carbide in the laser melted and martensite in the transformed zone or heat-affected zone were observed, depending on the process parameters. Depth of geometric profiles of laser transformed or melt zone structures, parameters such as dendrile arm spacing, volume fraction of carbide and surface hardness bear a direct relationship with the energy intensity P/UDb2, (10-100 J mm(-3)). There is a minimum energy intensity threshold for solid state transformation hardening (0.2 J mm(-3)) and similarly for the initiation of superficial melting (9 J mm(-3)) and full melting (15 J mm(-3)) in the case of ductile iron. Simulation, modeling and thermal analysis of laser processing as a three-dimensional quasi-steady moving heat source problem by a finite difference method, considering temperature dependent energy absorptivity of the material to laser radiation, thermal and physical properties (kappa, rho, c(p)) and freezing under non-equilibrium conditions employing Scheil's equation to compute the proportion of the solid enabled determination of the thermal history of the laser treated zone. This includes assessment of the peak temperature attained at the surface, temperature gradients, the freezing time and rates as well as the geometric profile of the melted, transformed or heat-affected zone. Computed geometric profiles or depth are in close agreement with the experimental data, validating the numerical scheme.

Instability map for cold and warm working of as-cast 304 stainless steel

The deformation characteristics of as-cast 304 stainless steel under compression in the temperature range 20-600 degrees C and strain rate range 0.001-100 s(-1) have been studied with a view to characterizing the flow instabilities occurring in the microstructure. Ar strain rates of less than 0.05 s(-1), as-cast 304 stainless steel exhibits flow localization in the temperature range 20-600 degrees C, whereas dynamic strain ageing occurs at intermediate temperatures and below 5 s(-1). At room temperatures and strain rates of less than 0.05 s(-1), martensite formation is observed. To avoid the above microstructural instabilities warm working should be carried out at strain rates greater than 10 s(-1) in the temperature range 400-600 degrees C and cold working could be done in the range of about 0.05-0.8 s(-1). The continuum criterion developed on the basis of the principles of maximum rate of entropy production and separability of the dissipation function, predicts accurately all of the above instability features. (C) 1997 Elsevier Science S.A.

Plate-shaped transformation products in zirconium-base alloys

Plate-shaped products resulting from martensitic, diffusional, and mixed mode transformations in zirconium-base alloys are compared. in the present study. These alloys are particularly suitable for the comparison in view of the fact that the lattice correspondence between the parent beta (bcc) and the product alpha (hcp) or gamma-hydride (fct) phases are remarkably similar for different types of transformations. Crystallographic features such as orientation relations, habit planes, and interface structures associated with these transformations have been compared:, with a view toward examining whether the transformation mechanisms have characteristic imprints on these experimental observables. Martensites exhibiting dislocated lath, internally twinned plate, and self-accommodating three-plate cluster morphologies have been encountered in Zr-2.5Nb alloy. Habit planes corresponding to all these morphologies have been found to be consistent with the predictions based on the invariant plane strain (IFS) criterion. Different morphologies have been found to reflect the manner in which the neighboring martensite variants are assembled. Lattice-invariant shears (LISs) for all these cases have been identified to be either {10 (1) over bar 1}(alpha) ((1) over bar 123)(alpha) slip or twinning on (10 (1) over bar 1)(alpha) planes. Widmanstatten alpha precipitates, forming in a step-quenching treatment, have been shown to have a lath morphology, the alpha/beta interface being decorated with a periodic array of (c + a) dislocations at a spacing of 8 to 10 nm. The line vectors of these dislocations are nearly parallel to the invariant lines. The alpha precipitates, forming in the retained beta phase on aging, exhibit an internally twinned structure with a zigzag habit plane. Average habit planes for the morphologies have been found to lie near the {103}(beta) - {113}(beta) poles, which are close to the specific variant of the {112}(beta) plane, which transforms into a prismatic plane of the type {1 (1) over bar 00}(alpha). The crystallography of the formation of the gamma-hydride phase (fct) from both the alpha and beta phases is seen to match the IFS predictions. While the beta-gamma transformation can be treated approximately as a simple shear on the basal plane involving a change in the stacking sequence, the alpha-gamma transformation call be conceptually broken into a alpha --> beta transformation following the Burgers correspondence and the simple beta-gamma shear process. The active eutectoid decomposition in the Zr-Cu system, beta --> alpha + beta', has been described in terms of cooperative growth of the alpha phase from the beta phase through the Burgers correspondence and of the partially ordered beta' (structurally similar to the equilibrium Zr2Cu phase) through an ordering process. Similarities and differences in crystallographic features of these transformations have been discussed. and the importance of the invariant line vector in deciding the geometry of the corresponding habit planes has been pointed out.

Nanoindentation studies in NiTi films deposited on Si wafer

Nanoindentation tests were carried out at different locations in a Ti rich NiTi film deposited on a 3 `' silicon wafer by dc magnetron sputtering. The purpose of doing nanoindentation at different locations was to check the uniformity of the sample with respect to its mechanical behaviour and shape memory effect. The results showed that elastic modulus and hardness measured by nanoindentation was similar at different locations in the 3 `' wafer. Nanoindcntation coupled with depth profiling of residual indents using AFM also showed that the extent of shape memory recovery obtained by heating the film above its martensite to austcnite phase transformation temperature was also similar at different locations in the 3 `' wafer. However, the measured recovery ratio was lower than that predicted from theoretical calculations for indents made using Berkovich indenter. The results showed that the deposition process resulted in a NiTi film with uniform composition, mechanical properties and shape memory behaviour.

Influence of Tempered Microstructures on the Transformation Behaviour of Cold Deformed and Intercritically Annealed Medium Carbon Low Alloy Steel

This research is focused on understanding the role of microstructural variables and processing parameters in obtaining optimised dual phase structures in medium carbon low alloy steels. Tempered Martensite structures produced at 300, 500, and 650 degrees C, were cold rolled to varied degrees ranging from 20 to 80% deformation. Intercritical annealing was then performed at 740, 760, and 780 degrees C for various time duration ranging from 60 seconds to 60 minutes before quenching in water. The transformation behaviour was studied with the aid of optical microscopy and hardness curves. From the results, it is observed that microstructural condition, deformation, and intercritical temperatures influenced the chronological order of the competing stress relaxation and decomposition phase reactions which interfered with the rate of the expected alpha -> gamma transformation. The three unique transformation trends observed are systematically analyzed. It was also observed that the 300 and 500 degrees C tempered initial microstructures were unsuitable for the production of dual structures with optimized strength characteristics.

Possibility of chaos in interval friction experiments of martensites

Wuttig and Suzuki's model on anelastic nonlinearities in solids in the vicinity of martensite transformations is analysed numerically. This model shows chaos even in the absence of applied forcing field as a function of a temperature dependent parameter. Even though the model exhibits sustained oscillations as a function of the amplitude of the forcing term, it does not exactly capture the features of the experimental time series. We have improved the model by adding a symmetry breaking term. The improved model shows period doubling bifurcation as a function of the amplitude of the forcing term. The solutions of our improved model shows good resemblance with the nonsymmetric period four oscillation seen in the experiment. (C) 1999 Elsevier Science B.V. All rights reserved.

Effect of thermal and thermo-mechanical cycling on the microstructure of Ni-rich NiTi shape memory alloys

Microstructural changes of Ni-rich NiTi shape memory alloy during thermal and thermo-mechanical cycling have been investigated using Electron Back Scattered Diffraction. A strong dependence of the orientation of the prior austenite grain on the misorientation development has been observed during thermal cycling and thermo-mechanical cycling. This effect is more pronounced at the grain boundaries compared to grain interior. At a larger applied strain, the volume fraction of stabilized martensite phase increases with increase in the number of cycling. Deformation within the martensite leads to stabilization of martensitic phase even at temperatures slightly above the austenite finish temperature. Modulus variation with respect to temperature has been explained on the basis of martensitic transformation.

Temperature dependence of indentation recovery ratios in austenitic and martensitic shape memory alloys

Instrumented microindentation (IM) on two Ni-Ti shape memory alloys (SMAs), where one is austenitic and the other is martensitic at room temperature, were conducted from 40 to 150 degrees C. Results show that the depth and work recovery ratios, eta(d) and eta(w) respectively, are complementary to each other. While eta(d) decreases gradually with temperature for austenite, it drops markedly for the martensite in the martensite-to-austenite transformation regime. These results affirm the utility of IM for characterizing SMAs.

Simultaneous measurement of mechanical and electrical contact resistances during nanoindentation of NiTi shape memory alloys

The nanoindentation technique can be employed in shape memory alloys (SMAs) to discern the transformation temperatures as well as to characterize their mechanical behavior. In this paper, we use it with simultaneous measurements of the mechanical and the electrical contact resistances (ECR) at room temperature to probe two SMAs: austenite (RTA) and martensite (RTM). Two different types of indenter tips - Berkovich and spherical - are employed to examine the SMAs' indentation responses as a function of the representative strain, epsilon(R). In Berkovich indentation, because of the sharp nature of the tip, and in consequence the high levels of strain imposed, discerning the two SMAs on the basis of the indentation response alone is difficult. In the case of the spherical tip, epsilon(R) is systematically varied and its effect on the depth recovery ratio, eta(d), is examined. Results indicate that RTA has higher eta(d) than RTM, but the difference decreases with increasing epsilon(R) such that eta(d) values for both the alloys would be similar in the fully plastic regime. The experimental trends in eta(d) vs. epsilon(R) for both the alloys could be described well with a eta(d) proportional to (epsilon(R))(-1) type equation, which is developed on the basis of a phenomenological model. This fit, in turn, directs us to the maximum epsilon(R), below which plasticity underneath the indenter would not mask the differences in the two SMAs. It was demonstrated that the ECR measurements complement the mechanical measurements in demarcating the reverse transformation from martensite to austenite during unloading of RTA, wherein a marked increase in the voltage was noted. A correlation between recovery due to reverse transformation during unloading and increase in voltage (and hence the electrical resistance) was found. (C) 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Evolution and stability of phases in a high temperature shape memory alloy Ni49.4Ti38.6Hf12

Ni49.4Ti38.6Hf12 shape memory alloy has been characterized for structure, microstructure and transformation temperatures. The microstructure of the as-cast sample consists of B19' and R-phases, and (Ti,Hf)(2)Ni precipitate phase along the grain boundaries in the form of dendrites. The microstructure of the solution treated sample contains only B19' martensite phase, whereas a second heat treatment after solutionizing results in reappearance of the R-phase and the (Ti,Hf)(2)Ni grain boundary precipitate phase in the microstructure. A detailed microstructural examination shows the presence of precipitates having both coherent and incoherent interface with the matrix, the type of interface being dictated by the crystallographic orientation of the matrix phase. The present study shows that the (Ti,Hf)(2)Ni precipitates having coherent interface with the matrix, drive the formation of the R-phase in the microstructure. (C) 2013 Elsevier Ltd. All rights reserved.

Effect of chemical treatment on surface characteristics of sputter deposited Ti-rich NiTi shape memory alloy thin-films

NiTi thin-films were deposited by DC magnetron sputtering from single alloy target (Ni/Ti: 45/55 aL.%). The rate of deposition and thickness of sputter deposited films were maintained to similar to 35 nm min(-1) and 4 mu m respectively. A set of sputter deposited NiTi films were selected for specific chemical treatment with the solution comprising of de-ionized water, HF and HNO3 respectively. The influence of chemical treatment on surface characteristics of NiTi films before and after chemical treatment was investigated for their structure, micro-structure and composition using different analytical techniques. Prior to chemical treatment, the composition of NiTi films using energy dispersive X-ray dispersive spectroscopy (EDS), were found to be 51.8 atomic percent of Ti and 48.2 atomic percent of Ni. The structure and morphology of these films were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD investigations, demonstrated the presence of dominant Austenite (110) phase along with Martensite phase, for untreated NiTi films whereas some additional diffraction peaks viz. (100), (101), and (200) corresponding to Rutile and Anatase phase of Titanium dioxide (TiO2) along with parent Austenite (110) phase were observed for chemically treated NiTi films. FTIR studies, it can be concluded that chemically treated films have higher tendency to form metal oxide/hydroxide than the untreated NiTi films. XPS investigations, demonstrated the presence of Ni-free surface and formation of a protective metal oxide (TiO2) layer on the surface of the films, in both the cases. The extent of the formation of surface oxide layer onto the surface of NiTi films has enhanced after chemical treatment. (C) 2014 Elsevier B.V. All rights reserved.

Dynamics of a driven magneto-martensitic ribbon

We investigate the dynamics of a sinusoidally driven ferromagnetic martensitic ribbon by adopting a recently introduced model that involves strain and magnetization as order parameters. Retaining only the dominant mode of excitation we reduce the coupled set of partial differential equations for strain and magnetization to a set of coupled ordinary nonlinear equations for the strain and magnetization amplitudes. The equation for the strain amplitude takes the form of parametrically driven oscillator. Finite strain amplitude can only be induced beyond a critical value of the strength of the magnetic field. Chaotic response is seen for a range of values of all the physically interesting parameters. The nature of the bifurcations depends on the choice of temperature relative to the ordering of the Curie and the martensite transformation temperatures. We have studied the nature of response as a function of the strength and frequency of the magnetic field, and magneto-elastic coupling. In general, the bifurcation diagrams with respect to these parameters do not follow any standard route. The rich dynamics exhibited by the model is further illustrated by the presence of mixed mode oscillations seen for low frequencies. The geometric structure of the mixed mode oscillations in the phase space has an unusual deep crater structure with an outer and inner cone on which the orbits circulate. We suggest that these features should be seen in experiments on driven magneto-martensitic ribbons. (C) 2014 Elsevier B. V. All rights reserved.

Microstructure dependent elastic modulus variation in NiTi shape memory alloy

Modulus variation of NiTi shape memory alloy has been investigated at microstructural level through nano dynamical mechanical analysis and compared with bulk experimental measurements. The differences between the modulus values at the macro and micro level as well as within the micro level are discussed and the corresponding variations have been explained based on the crystal structure, orientation and misorientation. The experimental results confirm a higher modulus value for the martensite phase that is in agreement with the theoretical predictions. (C) 2015 Elsevier B. V. All rights reserved.