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The study of Ni-Ti shape memory alloy films is of great technological interest for applications in the field of microengineering. They can work as sensors and actuators at the same time. However, there are still important issues unresolved like formation of film crystallographic orientation and its control. Films exhibiting the two-way shape memory effect are also required. A two-magnetron sputter deposition chamber mounted into the six-circle diffractometer of the Rossendorf Beamline at the European Synchrotron Radiation Facility was used for the processing of Ni-Ti films. The in-situ x-ray diffraction studies enabled to identify the different steps of the structural evolution during film growth. Deposition conditions leading to Ni-Ti films mainly containing grains with (100) or (110) planes of the B2 phase parallel to the film surface were successfully defined. This is an important achievement since texture has a strong influence on the extent of the strain recovery. The deposition of films with a “two-way” actuation (films with a combination of superelasticity and shape memory characteristics) was also achieved. It will allow the development of smaller devices since no consideration has to be paid to a resetting spring.

The study of Ni-Ti shape memory alloy films is of great technological interest for applications in the field of microengineering. They can work as sensors and actuators at the same time. However, there are still important issues unresolved like formation of film texture and its control. Films exhibiting the two-way shape memory effect are also required. A better understanding of the underlying growth mechanisms and their microstructural development requires sophisticated in-situ techniques. A two-magnetron sputter deposition chamber mounted into the six-circle diffractometer of the Rossendorf Beamline at the European Synchrotron Radiation Facility has been used for the processing of the Ni-Ti films. The in-situ x-ray diffraction studies enabled us to identify the different steps of the structural evolution during deposition with a set of parameters as well as to evaluate the effect of changing parameters (Ti target power) during film growth. It has been found that the type of substrate plays an important role for the preferential orientation of sputtered Ni-Ti films. In some cases they exhibit a pronounced depth dependence of their preferential orientations. Amorphous SiO2 and TiN buffer layers have been used to successfully control their crystallographic orientations. This is an important achievement since the texture has a strong influence on the extent of the strain recovery of the Ni-Ti films. The deposition conditions leading to films mainly containing grains with (100) or (110) planes of the B2 phase parallel to the film surface are presented. The deposition of graded Ni-Ti films by changing deliberately the Ti:Ni ratio, thereby altering microstructure and transformation temperatures across the film thickness, has also been performed. The aim has been the optimization of the deposition parameters in order to fabricate films with a “two-way” actuation (films with a combination of superelasticity and shape memory characteristics). It will lead to the development

Ni-Ti films were deposited by magnetron cosputtering using a chamber installed into the six-circle goniometer of the Rossendorf BeamLine at ESRF. The in-situ XRD studies enable us to identify different steps of the structural evolution during growth and annealing. The use of diverse type of substrates and the effect of the application of a bias voltage to the substrate during film deposition were major tools in this study. When a negative bias voltage is applied, it causes a higher energetic ion bombardment of the growing film, resulting in an enhanced surface-atom mobility, but at sufficiently high voltage, leads to defect formation. Cross-sectional TEM and SEM micrographs have shown a change in the morphology of the films linked with different levels of bias voltages (0, -45 and -90V in this study). The transformation behaviour of the sputtered Ni-Ti films (as shown by electrical resistivity measurements) is influenced by the energy of the bombarding ions. The microstructure details resulting from the deposition using different bias values are discussed. Additionally, it has been commissioned an ion gun allowing post-deposition ion irradiation or ion bombardment during sputter deposition. In this first series of experiments, a Ni-Ti film was irradiated with He ions after deposition (without exposing the film to the atmosphere, i.e. reduced surface oxide formation) thus modifying deliberately the microstructure of the film locally. A layer of approximately 50% of the thickness of the film was selectively removed at the irradiated region (6 x 6 mm²). This type of studies will be very useful for the easier design and miniaturization of Ni-Ti films based devices in the field of micro-electro-mechanical systems (MEMS).

Ni-Ti thin films have been recognized as promising and high performance materials in the field of microelectromechanical system applications. However, important issues like formation of film texture and its control are still unresolved. Widening the scope of previous experiments concerning the influence of the deposition parameters on the Ni-Ti films structure, here we show how different crystallographic orientations can be obtained by changing the substrate type. The growth of near-equiatomic Ni-Ti films, deposited by magnetron co-sputtering from Ni-Ti and Ti targets on heated substrates ( 470C), has been studied in situ by x-ray diffraction at a synchrotron radiation beamline. As mentioned in other studies for depositions on Si(100), a (110) fiber texture is observed for the B2 phase. However, a preferential stacking of (100) planes of the B2 phase parallel to the film surface was observed when using a MgO(100) substrate. The preferential orientation of B2(100) // MgO(100) was very strong and was kept as such until the end of the deposition, which lasted for 2 hours (~ 900 nm). Ni-Ti films were also deposited on a TiN layer (~ 15 nm) previously deposited on top of a SiO2/Si(100) substrate. In this case, a crossover from (110) oriented grains dominating at small thicknesses, to (211) oriented grains taking over at larger thicknesses was observed. These are promising results concerning the manipulation of the crystallographic orientations of Ni-Ti thin films, since the texture has a strong influence on the extent of the strain recovery.

Ni-Ti SMA are smart materials undergoing first order martensitic transformations driven by temperature and/or stress. In the form of film they are very attractive candidates for microelectro-mechanical system (MEMS) applications. Future directions include the production of functionally graded films by changing deliberately the ratio Ti/Ni across their thickness. However, for the successful development of this type of films, it is important to characterize, model and control the variations in composition, crystalline structure and transformation temperatures. Our approach is in-situ XRD study of the actual growth of the films of varying composition along the thickness carried out using a deposition chamber installed at a synchrotron radiation beamline. These studies were complemented with ex-situ analysis techniques. The results achieved on a Ni-Ti film co-sputtered from Ni-Ti and Ti targets on a TiN buffer layer are presented in this paper. The deposition started by using optimised parameters for a near equiatomic composition. After 1 h (≈330 nm thick film), the Ti power was increased from 20 to 25 W, leading to the precipitation of Ti2Ni. The evolution of the lattice parameter values of the B2 phase, calculated from the corresponding XRD data, is clearly linked with the increase of the Ti power. The depth profile of the atomic concentrations determined by Auger Electron Spectroscopy (AES) is in agreement with the in situ XRD results. The temperature dependence of the electrical resistivity was used to monitor phase transformations, Scanning Electron Microscopy (SEM) has shown the presence of twinned martensite on the film’s surface at room temperature.

Ni-Ti Shape Memory Alloy thin films are suitable materials for microelectromechanical devices. During the deposition of Ni-Ti thin films on Si substrates, there exist interfacial diffusion and chemical interactions at the interface due to the high temperature processing necessary to crystallize the film. For the present study, Ni-Ti thin films were prepared by magnetron cosputtering from Ni-Ti and Ti targets in a specially designed chamber mounted on the 6-circle goniometer of the ROssendorf BeamLine (ROBL-CRG) at ESRF, Grenoble (France). The objective of this study has been to investigate the interfacial structure resulting from depositions (at a temperature of ≈ 470°C) on different substrates: naturally oxidized Si(100), Si(111) and poly-Si substrates. A detailed High-Resolution TEM analysis of the interfacial structure has been performed. When Ni-Ti is deposited on Si(100) substrate, a considerable diffusion of Ni into the substrate takes place, resulting in the growth of semi-octaeder A-NiSi2 silicide. In the case of Ni-Ti deposited on Si(111), there appears an uniform thickness plate, due to the alignment between substrate orientation and the [111]-growth front. For Ni-Ti deposited on poly-Si, the diffusion is inhomogeneous. Preferential diffusion is found along the columnar grains of poly-Si, which are favourably aligned for Ni diffusion. These results show that for the Ni-Ti/Si system, the morphology of the diffusion interface is strongly dependent on the type of substrates.

In-situ x-ray diffraction (XRD) was employed to study the effect of the deliberate change of the ratio Ti/Ni during the deposition of Ni-Ti films. Thus, graded films were deposited exhibiting distinctive composition and crystalline structure along the growth direction. The as-sputtered films were ex-situ characterized by Auger Electron Spectroscopy (AES), Cross-sectional Transmission Electron Microscopy (XTEM), and Electrical Resistivity (ER) measurements (during thermal cycling). In this paper results are presented concerning a film with a Ti-rich composition in the central part and near-equiatomic composition in the extremities, following 4 distinct deposition periods (different Ti target powers). During the initial deposition step (near-equiatomic composition) the Ni-Ti B2 phase starts by stacking onto (h00) planes on the naturally oxidized Si(100) substrate due to the presence of the native Si oxide (2-3 nm). The increase of the power of the Ti target in the second and third steps induced the precipitation of Ti2Ni. When stopping the Ti co-sputtering, Ti2Ni “dissolves” and, thus, plays the role of a reservoir for the formation of B2 phase now preferentially stacking onto (110) with the system approaching again the equiatomic composition. The ex-situ study of the interface’s morphology has shown the presence of NiSi2 silicides (A-NiSi2 and B-NiSi2), Ti4Ni4Si7, Ti2Ni and a non-identified phase constituted by Ni, Ti and Si, most likely amorphous. During thermal cycling, electrical resistivity measurements revealed phase transitions associated with the B2, R-phase and B19’ phases. This type of studies allow the identification of intermediate states during deposition and annealing, and the correlation with the final structure of the film, being useful for the optimisation of the deposition parameters in order to fabricate films with a two-way reversible actuation.

Characterization of sputtered Shape Memory Alloy Ni-Ti films by cross-sectional TEM and SEM

Ni-Ti SMA are smart materials undergoing first order martensitic transformations driven by temperature and/or stress. In the form of film they are very attractive candidates for microelectro-mechanical system (MEMS) applications. Future directions include the production of functionally graded films by changing deliberately the ratio Ti/Ni across their thickness. However, for the successful development of this type of films, it is important to characterize, model and control the variations in composition, crystalline structure and transformation temperatures. Our approach is in-situ XRD study of the actual growth of the films of varying composition along the thickness carried out using a deposition chamber installed at a synchrotron radiation beamline. These studies were complemented with ex-situ analysis techniques. The results achieved on a Ni-Ti film co-sputtered from Ni-Ti and Ti targets on a TiN buffer layer are presented in this paper. The deposition started by using optimised parameters for a near equiatomic composition. After 1 h (≈330 nm thick film), the Ti power was increased from 20 to 25 W, leading to the precipitation of Ti2Ni. The evolution of the lattice parameter values of the B2 phase, calculated from the corresponding XRD data, is clearly linked with the increase of the Ti power. The depth profile of the atomic concentrations determined by Auger Electron Spectroscopy (AES) is in agreement with the in situ XRD results. The temperature dependence of the electrical resistivity was used to monitor phase transformations, Scanning Electron Microscopy (SEM) has shown the presence of twinned martensite on the film’s surface at room temperature.

Characterization of sputtered Shape Memory Alloy Ni-Ti films by cross-sectional TEM and SEM

Ni-Ti Shape Memory Alloy thin films are suitable materials for microelectromechanical devices. During the deposition of Ni-Ti thin films on Si substrates, there exist interfacial diffusion and chemical interactions at the interface due to the high temperature processing necessary to crystallize the film. For the present study, Ni-Ti thin films were prepared by magnetron cosputtering from Ni-Ti and Ti targets in a specially designed chamber mounted on the 6-circle goniometer of the ROssendorf BeamLine (ROBL-CRG) at ESRF, Grenoble (France). The objective of this study has been to investigate the interfacial structure resulting from depositions (at a temperature of ≈ 470°C) on different substrates: naturally oxidized Si(100), Si(111) and poly-Si substrates. A detailed High-Resolution TEM analysis of the interfacial structure has been performed. When Ni-Ti is deposited on Si(100) substrate, a considerable diffusion of Ni into the substrate takes place, resulting in the growth of semi-octaeder A-NiSi2 silicide. In the case of Ni-Ti deposited on Si(111), there appears an uniform thickness plate, due to the alignment between substrate orientation and the [111]-growth front. For Ni-Ti deposited on poly-Si, the diffusion is inhomogeneous. Preferential diffusion is found along the columnar grains of poly-Si, which are favourably aligned for Ni diffusion. These results show that for the Ni-Ti/Si system, the morphology of the diffusion interface is strongly dependent on the type of substrates.

The preferential orientation of Ni-Ti thin films is a crucial factor in determining the shape memory behavior. The texture has a strong influence on the extent of the strain recovery. The relationship between structure and deposition parameters is of extreme importance for future device applications. Our approach is in-situ x-ray diffraction during deposition carried out in a process chamber installed at a synchrotron radiation beamline. Near-equiatomic films were co-sputtered from Ni-Ti and Ti targets. Substrate type and bias voltage play an important role for the preferred orientation. On naturally oxidized Si(100) substrates the NiTi B2 phase starts by stacking onto (h00) planes and then changes to (110) fiber texture with increasing film thickness. For thermally oxidized Si(100) substrates, this cross-over is only observed when a bias voltage is applied. The experiments were supplemented by ex-situ transmission electron microscopy and Auger Electron Spectroscopy allowing an additional deeper insight into the film/substrate interface.

Ni-Ti thin films present great advantages for the fabrication of micro-actuators. The phase transformation and precipitation, which are responsible for the shape memory effect, have been widely studied in bulk material and thin films. However, in-situ studies have been limited to the ageing/annealing treatments after deposition. In this study we present a series of results that clearly illustrate the interest of in-situ studies, not only during annealing, but also during sputtering. The in-situ annealing experiments, using a Be-dome furnace installed into the six-circle diffractometer of the ROssendorf BeamLine (ROBL-CRG) at the ESRF, Grenoble, allowed us to determine the kinetics of the phenomena, to identify the sequence of precipitation and to correlate the build-up of the final structure with the processing conditions. The in-situ sputtering experiments were performed using a magnetron sputter deposition chamber also installed into the six-circle diffractometer of the ROBL-CRG beamline. This facility allowed us to follow the structural evolution of the films also during the deposition process.

Anisotropy of the shape recovery associated with shape memory effect strongly depends on the type of preferential orientation, that is present, as well as the ‘strength’ of the texture. In the present paper, we report the results obtained by the in-situ study of texture evolution during the annealing process in Ti-rich Ni-Ti Shape Memory Alloys (SMAs) with different thermal and mechanical histories. For this purpose, a Be-dome furnace installed into a 6-circle goniometer at the BM20 beamline (ROBL-CRG) at the ESRF (Grenoble) has been used. It is shown that there is a significant change in the preferential orientation of B2 phase, with the change in microstrain/coherence domain size, as a function of annealing temperature. This effect is also observed in the B19’ phase after cooling. The alpha-fiber II (austenite texture - <110>||RD ({111}<110>-{110}<110>) was present in the as-received alloy, but only up to 400ºC. The evolution of {111}<110> austenite texture component is quite clear for annealing temperatures above 400ºC.

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The aim of the present experiment was to analyse the structural evolution during annealing of Nickel-Titanium (Ni-Ti) SMA subjected to different thermomechanical treatments. As structural evolutions are accompanied by the changes in preferential orientations, pole figures were employed to study the in-situ conditions.

Ni-Ti thin films present great advantages for the fabrication of micro-actuators. The phase transformation and precipitation, which are responsible for the shape memory effect, have been widely studied in bulk material and thin films. However, in-situ studies have been limited to the ageing/annealing treatments after deposition. In this study we present a series of results that clearly illustrate the interest of in-situ studies, not only during annealing, but also during sputtering. The in-situ annealing experiments, using a Be-dome furnace installed into the six-circle diffractometer of the ROssendorf BeamLine (ROBL-CRG) at the ESRF, Grenoble, allowed us to determine the kinetics of the phenomena, to identify the sequence of precipitation and to correlate the build-up of the final structure with the processing conditions. The in-situ sputtering experiments were performed using a magnetron sputter deposition chamber also installed into the six-circle diffractometer of the ROBL-CRG beamline. This facility allowed us to follow the structural evolution of the films also during the deposition process.

The Ni-Ti system is the most popular of the SMA’s because of its large recovery force, a transformation temperature near room temperature and a good oxidation resistance. Although the transformation frequency is low (mainly limited by thermal inertia), a thin film of Ni-Ti coupled with silicon for heat dissipation can produce cycling frequencies much larger than the typical macrosize structures. The thin films can be electrically driven using joule heating, and they demonstrate fast cooling rates because of their large surface-to-volume ratio. The control of film composition and properties has proven difficult in sputter-deposited films, and a deeper study of deposition techniques is needed. Furthermore, the as-deposited films show an amorphous structure and thus have to be heat treated to induce crystallization in order to have the shape memory effect. In the present study, thin films have been prepared by dc and rf magnetron sputtering. The crystallization of these films has been studied by in-situ grazing incidence X-Ray diffraction (GIXRD), allowing us to establish a correlation between the deposition conditions and the tendency for crystallization.

Kein Abstract vorhanden.