Authors: Yong Hua Li, F.L. Meng, Chang Sheng Liu, Y.M. Wang
Abstract: Ti-51.45at.%Ni thin films were deposited onto copper substrates by magnetron sputtering.
The copper substrates were pre-punched into dog-bone specimens with 4.5mm×30mm(gauge portion)
×35µm( thickness). The substrate temperature was about 673K. The thin films were about 20µm thick.
The as-deposited films were first solution treated at 1073K for 1h, and then aged at 773K for 30min.
The grain size was estimated to be 1.5µm from scanning electron microscopy micrographs. Tensile
tests were carried out on CSS-44100 electron universal test-machine. The strain rate was 1.1×10-4 s-1.
The stress-strain curves of the free-standing film were obtained from the experimental stress-strain
curves of copper substrate together with the thin film adherent to the substrate compared with the
curves of copper substrate without film. The Hall-Patch coefficient was calculated, k=205Mpa.µm1/2.
It seems that the Hall-Patch coefficient decreases with increasing film thickness. The experimental
results showed that a series of parallel cracks grew in a concerted fashion across the thin film and the
cracks were equally spaced. The cracks were more closely spaced if the film stress was increased. The
fracture toughness of the film was estimated, c KΙ =0.96MPa·m1/2. Therefore, the minimum crack
spacing is predicted by the film stress given.
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Authors: Rui M.S. Martins, Manfred Beckers, A. Mücklich, Norbert Schell, Rui Jorge C. Silva, Karimbi Koosappa Mahesh, Francisco Manuel Braz Fernandes
Abstract: 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.
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Authors: Rui M.S. Martins, Norbert Schell, H. Reuther, Luís Pereira, Rui Jorge C. Silva, Karimbi Koosappa Mahesh, Francisco Manuel Braz Fernandes
Abstract: 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.
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Authors: Rui Miguel S. Martins, Francisco Manuel Braz Fernandes, Rui Jorge C. Silva, Manfred Beckers, Norbert Schell
Abstract: A sputter deposition chamber inserted into the six-circle Huber diffractometer of the
materials research station of the ROssendorf BeamLine (ROBL-CRG) at ESRF allowed to perform
in-situ experiments during film growth of Ni-Ti. It is equipped with Kapton windows for X-Ray
Diffraction (XRD) and specular Reflectivity (XRR) measurements. By following in situ the
evolution of the structure of the growing film, we reveal intermediate “states” which cannot be
seen/revealed ex situ, because those states occurred only during the growth but were no longer
visible after deposition. Vertical Bragg-Brentano large-angle scattering geometry was employed to
study the different trends of structural transformations taking place during deposition. Ni-Ti films
exhibiting a non-uniform phase content across the film thickness could be produced by varying the
power of co-sputtering Ni-Ti plus Ti. A significant decrease of IB2{110}/IB2{200} was observed when a
bias of -45 V was applied.
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