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Neutron investigation of Nitinol stents and massive samples before and after PIRAC coating
Rogante, M. ; Buhagiar, J. ; Cassar, G. ; Debono, M. ; Lebedev, V. ; Mikula, Pavol ; Ryukhtin, Vasil
Nitinol, a thermoelastic Ni-Ti Shape Memory Alloy (SMA) with approximately 50 at. % Ti, is adopted in a wide range of medical equipment and devices used in interventional radiology, orthopaedics, neurology and cardiology, in particular as a smart material for stents. In this work, NiTi real stents and massive samples before and after different Powder Immersion Reaction Assisted Coating (PIRAC) treatments have been investigated by using two neutron techniques: (1) Small and Ultra-Small Angle Neutron Scattering (SANS, USANS) for nano- and micro-scale characterization, obtaining information on structure and the effects due to the coating treatment, and (2) High-Resolution Neutron Diffraction (HRND), evaluating the macrostrain components resulting from angular shifts of diffraction peaks and the micro-strains in the plastically deformation region by means of profile-broadening analysis. The obtained results contribute: improving knowledge of defects and other key features of the materials complementary to those achieved by using traditional examination techniques. helping to better understand the functional characteristics of Nitinol parts and predict the material's mechanical behaviour.
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Residual stresses of laser-welded pressure vessel steel determined by X-ray and neutron diffraction
Trojan, K. ; Vlk, A. ; Čapek, J. ; Hervoches, Charles ; Ganev, N.
To gain insight into the quality of the laser weld, information about the residual stress state across the weld is very useful. In this contribution, the residual stress profiles for lowalloy carbon steel plates of P355NL1 grade, which were laser welded from both sides, are presented. To separate the effects of the production of plates from the welding process, the samples were annealed for stress relieving. Using X-ray and neutron diffraction, the surface and bulk RS profiles were obtained. From the obtained data, first, the difference in the character of the longitudinal (parallel to the weld axis) and the transversal component of the RS tensor can be seen. The longitudinal component has a tensile character with a maximum value approximately 500 MPa. Values and character of the transversal component vary strongly with depth and distance from the weld axis.
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On a possible use of neutron three axis diffractometer for studies of elastic and plastic deformation of polycrystalline materials
Mikula, Pavol ; Ryukhtin, Vasil ; Rogante, M.
Feasibility of using a high-resolution three axis neutron diffractometer performance for elastic and plastic deformation studies of metallic polycrystalline samples is presented. The method consists of unconventional set up employing bent perfect crystal (BPC) monochromator and analyzer with a polycrystalline sample in between. After the realization of focusing conditions in real and momentum space at the neutron wavelength of 0.162 nm, a high angular resolution up to FWHM(d/d)=2x10-3 was achieved on the standard Fe(110) sample (2 mm diameter) which then opened the possibility for the measurements of small lattice parameter changes of samples. The feasibility of the instrument for macro-and microstrain as well as grain size studies is demonstrated on the polycrystalline samples of low carbon shear deformed steel wires and the NiTi plates subjected to heat treatment.
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Instrumentation for study of nanomaterials in NPI REZ (New laboratory for material study in Nuclear Physics Institute in REZ)
Bejšovec, Václav ; Cannavó, Antonino ; Ceccio, Giovanni ; Hnatowicz, Vladimír ; Horák, Pavel ; Lavrentiev, Vasyl ; Macková, Anna ; Tomandl, Ivo ; Torrisi, Alfio ; Vacík, Jiří
Nano-sized materials become irreplaceable component of a number of devices for every aspect of human life. The development of new materials and deepening of the current knowledge require a set of specialized techniques-deposition methods for preparation/modification of the materials and analytical tools for proper understanding of their properties. A thoroughly equipped research centers become the requirement for the advance and development not only in nano-sized field. The Center of Accelerators and Nuclear Analytical Methods (CANAM) in the Nuclear Physics Institute (NPI) comprises a unique set of techniques for the synthesis or modification of nanostructured materials and systems, and their characterization using ion beam, neutron beam and microscopy imaging techniques. The methods are used for investigation of a broad range of nano-sized materials and structures based on metal oxides, nitrides, carbides, carbon-based materials (polymers, fullerenes, graphenes, etc.) and nano-laminate composites (MAX phases). These materials can be prepared at NPI using ion beam sputtering, physical vapor deposition and molecular beam epitaxy. Based on the deposition method and parameters, the samples can be tuned to possess specific properties, e.g., composition, thickness (nm-μm), surface roughness, optical and electrical properties, etc. Various nuclear analytical methods are applied for the sample characterization. RBS, RBS-channeling, PIXE, PIGE, micro-beam analyses and Transmission Spectroscopy are accomplished at the Tandetron 4130MC accelerator, and additionally the Neutron Depth Profiling (NDP) and Prompt Gamma Neutron Activation (PGNA) analyses are performed at an external neutron beam from the LVR-15 research reactor. The multimode AFM facility provides further surface related information, magnetic/electrical properties with nano-metric precision, nano-indentation, etc.
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Study of lithium encapsulation in porous membrane using ion and neutron beams
Ceccio, Giovanni ; Cannavó, Antonino ; Horák, Pavel ; Torrisi, Alfio ; Tomandl, Ivo ; Hnatowicz, Vladimír ; Vacík, Jiří
Ion track-etched membranes are porous systems obtained by etching of the latent ion tracks using a suitable etchant solution. In this work, control of the pores' spatial profiles and dimensions in PET polymers was achieved by varying etching temperature and etching time. For determination of the pores' shape, Ion Transmission Spectroscopy technique was employed. In this method, alterations of the energy loss spectra of the transmitted ions reflect alterations in the material density of the porous foils, as well as alterations of their thickness. Simulation code, developed by the team, allowed the tomographic study of the ion track 3D geometry and its evolution during chemical etching. From the doping of porous membranes with lithium-based solution and its analysis by Thermal Neutron Depth Profiling method, the ability of porous PET membranes to encapsulate nano-sized material was also inspected. The study is important for various applications, e.g., for catalysis, active agents, biosensors, etc.
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Production and characterization of micro-size pores for ion track etching applications
Cannavó, Antonino ; Havránek, Vladimír ; Lavrentiev, Vasyl ; Torrisi, L. ; Cutroneo, Mariapompea ; Ceccio, Giovanni ; Torrisi, Alfio ; Horák, Pavel ; Vacík, Jiří
For many years the applications of ion track etch materials have increased considerably, like charged particles detection, molecular identification with nanopores, ion track filters, magnetic studies with nanowires and so on. Over the materials generally used as track detector, the Poly-Allyl-Diglycol Carbonate (PADC), offers many advantages, like its nearly 100 % detection efficiency for charged particle, a high resistance to harsh environment, the lowest detection threshold, a high abrasion resistance and a low production costs. All of these properties have made it particularly attractive material, even if due to its brittleness, obtaining a thin film (less than 500 μm) is still a challenge. In this work, PADC foils have been exposed to a-particles emitted by a thin radioactive source of 241Am and to C ions from the Tandetron 4130 MC accelerator. The latent tracks generated in the polymer have been developed using a standard etching procedure in 6.25 NaOH solution. The dependence of the ion tracks' geometry on the ion beam energy and fluence has been evaluated combining the information obtained through a semiautomatic computer script that selects the etched ion tracks according to their diameter and mean grey value and nanometric resolution images by atomic force microscopy.
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Laser-generated nanoparticles to change physical properties of solids, liquids and gases
Torrisi, Alfio ; Cutroneo, Mariapompea ; Ceccio, Giovanni ; Cannavó, Antonino ; Horák, Pavel ; Torrisi, L. ; Vacík, Jiří
Synthesis of nanoparticles was possible employing a Nd: YAG pulsed laser at fundamental harmonic. The production of nanoparticles in water depends mainly on the laser parameters (pulse duration, energy, wavelength), the irradiation conditions (focal spot, repetition rate, irradiation time) and the medium where the ablation occurs (solid target, water, solution concentration). The nanoparticles can be introduced in solids, liquids or gases to change many physical characteristics. The optical properties of polymers and solutions, the wetting ability of liquids, the electron density of laser-generated plasma, represent some examples that can be controlled by the concentration of metallic nanoparticles (Au, Ag, Ti, Cu). Some bio-medical applications will be presented and discussed.
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Stability of the sodium content in selected botanical reference materials
Kameník, Jan ; Kučera, Jan ; Borovička, Jan ; Havránek, Vladimír
Sodium mass fractions in NIST standard reference materials (SRM) SRM 1547 Peach Leaves and SRM 1515 Apple leaves determined by INAA in our laboratory in recent years has been higher than the certified values. Similarly, increased values were published for SRM 1547 by several other laboratories. The increased Na mass fractions was found also for freshly opened SRM 1547 bottle and for material originating from a different lab. Increased Na mass fractions were confirmed by ICP-MS analysis of both materials. Analysis of archived samples revealed that sodium mass fraction in materials stored in polyethylene capsules is in agreement with the certified values. The sodium content in the glass of SRM 1547 bottle was roughly 10 %. Direct measurement of the Na depth profile by micro-PIXE was not indicative whether Na is released, i.g., by a glass corrosion due to residual humidity in the botanical material. However, a model experiment with freshly prepared and pulverized peach leaves demonstrated that such a scenario is possible for leaf-based materials. Although the study was focused on two NIST materials, the process is possible for any material with rather low Na content.
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Role of activation analysis in the preparation of reference materials
Kučera, Jan
The fundamentals of neutron activation analysis (NAA) and prompt gamma activation analysis (PGAA) and practices of both methods are briefly review, together with enlightening their specific role in the preparation of reference materials. The importance of homogeneity testing for the certification and use of reference materials (RMs) using NAA is appraised. Examples of the use of NAA and PGAA for the certification of element contents in environmental, biological, and material science RMs produced by world-leading institutions, such as U.S. NIST, IRMM, IAEA and by national institutions, as well, at the Nuclear Physics Institute within last almost 30 years are presented.
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