Papers by Author: Norbert Schell

Abstract: Grain tracking is a term used to describe experiments that investigate polycrystalline materials in terms of the crystallites or grains from which they are composed, non-destructively and in three dimensions. The new German high brilliance synchrotron radiation source, Petra III, will become available to users in 2010 [1]. The GKSS research centre will operate two beamlines, including the high energy materials science beamline (HEMS) [2]. HEMS will feature an instrument dedicated to grain tracking, able to support a range of experiments of this kind. This paper describes the design and specification of this instrument, and gives examples of the types of experiments that will be possible.

Abstract: In shape memory alloys (SMA), the texture can be an interesting factor influencing the anisotropic physical and mechanical characteristics during the phase transformations. It is well known that the texture significantly influences the stress-strain curve and shape memory strain of NiTi SMA. The aim of the present experiment was to analyze the textural modifications in the Ti-rich Ni-Ti SMA after annealing at moderate (500°C for 30 min) and subsequent low level of cold work reduction (10% thickness reduction). The textural results were obtained by X-Ray Diffraction (XRD) during thermal cycling in three points: (i) at room temperature (B19’ phase, after cold work), (ii) at 180°C (B2 phase), and (iii) at room temperature (B19’ phase, after cooling from 180°C). The phase transformations were characterized by Differential Scanning Calorimetry (DSC) and XRD.

Abstract: GKSS is currently investing heavily into new beamlines at DESY in Hamburg, Germany. After the completed installation of the wiggler beamline HARWI II at DORIS III GKSS is now building two new undulator beamlines at the new PETRA III storage ring. The High Energy Materials Science Beamline (HEMS) will allow high resolution diffraction experiments using samples and sample environments with masses up to 1 t, 3DXRD measurements, and high-energy micro-tomography experiments. The Imaging Beamline (IBL) will provide a nano-tomography as well as a micro-tomography station for X-ray energies up to 50 keV. Examples of typical experiments in the field of residual stress analysis, micro-tomography, and high-energy small-angle X-ray scattering will be given.

Abstract: The Shape Memory Effect on Ni-Ti thin films is strongly dependent on several factors: (i) chemical composition of the matrix, (ii) presence of precipitates and (iii) preferential orientation. Ni-Ti alloys derive their unique nonlinear and anisotropic mechanical behavior from stress-induced martensitic transformations, where the resulting strains are affected by crystallographic orientation. The influence of the texture on the transformation characteristics of Ni-Ti thin films is discussed on the basis of models and experimental results of the literature. A brief review of the texture build-up on thin films obtained by different fabrication techniques (sputtering, melt spinning, diffusion treatment of ultra-fine laminates, …) is presented. Details about in situ techniques allowing the identification of the preferential orientation during the fabrication process are presented. The processing parameters that more strongly influence the preferential orientation of the Ni-Ti thin films are identified. The mechanisms for the different microstructures are summarized and a special emphasis is put on the type of preferential orientation and its evolution along the processing time.

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.

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.

Abstract: The future High Energy Materials Science Beamline HEMS at the new German high brilliance synchrotron radiation storage ring PETRA III [1] will have a main energy of 120 keV, will be fully tunable in the range of 50 to 300 keV, and will be optimized for sub-micrometer focusing with Compound Refractive Lenses and Kirkpatrick-Baez Multilayer mirrors. Design and construction is the responsibility of the Research Center Geesthacht, GKSS, with approximately 70 % of the beamtime being dedicated to Materials Research, the rest reserved for “general physics” experiments covered by DESY, Hamburg. Fundamental research will encompass metallurgy, physics and chemistry. For first experiments in investigating grain-grain-interactions a dedicated 3D-microstructure-mapper will be designed. Applied research for manufacturing process optimization will benefit from the high flux in combination with ultra-fast detector systems allowing complex and highly dynamic in-situ studies of microstructural transformations. The beamline infrastructure will allow easy accommodation of large user provided equipment. Experiments targeting the industrial user community will be based on well established techniques with standardised evaluation, allowing "full service" measurements. Environments for strain mapping [2] on large structural components up to 1 t will be provided as well as automated investigations of large numbers of samples, e.g. for tomography and texture determination. The current design for the beamline (P07 in sector 5 of the future experimental hall) consists of a nearly five meter in-vacuum undulator source (U19-5) optimized for high energies, a general optics hutch, an in-house test facility and three independent experimental hutches working alternately, plus additional set-up and storage space for long-term experiments. HEMS should be operational in spring 2009 as one of the first beamlines running at PETRA III.