Influence of a surfactant on single ion track etching: Preparing and manipulating cylindrical micro wires

The influence of the alkali resistant surfactant Dowfax 2A1 on single ion track etching in 30 μm polycarbonate foils is studied at low etch rate (5 M NaOH at 41.5 ± 2 °C) using electro conductivity measurements. At surfactant concentrations above 10⁻⁴ vol.% break-through times are predictable (Δt/t < 0.25). At high surfactant concentrations (?0.1 vol.%) the formation of cylindrical channels is favoured. The shape of these channels (length ? 26 μm, diameter ? 1.8 μm) is verified by electro-replication and SEM observation of the resulting wires. Agreement of radii is better than 0.1 μm. Depending on the current limit set during electro replication compact or hollow cylinders can be obtained. A technique for localizing and manipulating individual micro wires by their head buds is described.     

Optimization of nanopores obtained by chemical etching on swift-ion irradiated lithium niobate

The morphology of the nanopores obtained by chemical etching on ion-beam irradiated LiNbO₃ has been investigated for a variety of ions (F, Br, Kr, Cu, Pb), energies (up to 2300 MeV), and stopping powers (up to 35 keV/nm) in the electronic energy loss regime. The role of etching time and etching agent on the pore morphology, diameter, depth, and shape has also been studied. The transversal and depth profiles of the pore have been found to be quite sensitive to both irradiation and etching parameters. Moreover, two etching regimes with different morphologies and etching rates have been identified.     

Improvement on thermoelectric properties of multilayered Si1−xGex/Si by ion beam bombardment

We made n-type nano-scale thin film thermoelectric (TE) devices that consist of multiple periodic layers of Si_1−xGe_x/Si. The period is about 10 nm. The structure was modified by 5 MeV Si ion bombardment that formed a nano-scale cluster structure. In addition to the effect of confinement of the phonon transmission, formation of nanoclusters by the ionization energy of incident MeV Si ions further increases the scattering of phonons, increasing the chance of inelastic interaction of phonons, resulting in more annihilation of phonons. This limits phonon mean free path. Phonons are absorbed and dissipated along the layers rather than in the direction perpendicular to the layer interfaces, therefore cross plane thermal conductivity is reduced. The increase of the density of electronic states due to the formation of nanocluster minibands increases the cross plane Seebeck coefficient and increases the cross plane electric conductivity of the film. Eventually, the thermoelectric figure of merit of the TE film increases.     

Large-area and high-density silicon nanocone arrays by Ar sputtering at room temperature

The large-area, high-density of ∼1-2 × 10⁹/cm² silicon nanocone arrays by ion-irradiation with incident angle of 75° have been achieved by using carbon-cone-mask. The scanning electron microscopy (SEM) images show that the width of silicon nanocones is ∼150 nm and the height is ∼400 nm. The investigation of SEM shows that the formation of the silicon nanocones proceeds through three periods, carbon nanocones-nanocones with carbon on the top and silicon at the bottom-silicon nanocones.     

High-resolution transmission electron microscopy and electron backscatter diffraction in nanoscaled ferritic and ferritic-martensitic oxide dispersion strengthened-steels

For specific blanket and divertor applications in future fusion power reactors a replacement of presently considered reduced activation ferritic-martensitic (RAFM) steels as a structural material by suitable oxide dispersion strengthened ferritic-martensitic steels would allow a substantial increase of the operating temperature from ∼823 to about 923 K. Due to this reason the RAFM-alloy ODS-Eurofer has already been developed and produced with industrial partners. In the He-cooled modular divertor concept, where temperatures above 923 K will arise, an ODS-steel with a purely ferritic matrix is advantageous, because of missing phase transitions. Due to this reason, a special ferritic ODS-steel is being manufactured as well. In this work the microstructures of these two ODS-alloy types, analysed mainly by high resolution TEM are compared, with respect to different manufacturing processes. In addition first results of high resolution EBSD scans together with determined orientation maps of the RAFM steel ODS-Eurofer will also be presented.     

Thermal stability of nano-structured ferritic alloy

The excellent tensile and creep strength and the potential for managing radiation damage make nano-structured ferritic alloys (NFAs) promising candidates for high-temperature applications in spallation proton, advanced fission and fusion neutron environments. The thermal stability of NFAs is critical for such applications, hence, this has been investigated in a series of aging experiments on MA957 at 900 °C, 950 °C and 1000 °C for times up to 3000 h. Optical and transmission electron microscopy (TEM) studies showed the fine scale grain and dislocation structures are stable up to 1000 °C. TEM and small angle neutron scattering (SANS) showed that the nm-scale solute cluster-oxide features (NFs), that are a primary source of the high strength of NFAs, were stable at 900 °C and coarsened only slightly at 950 °C and 1000 °C. Porosity that developed during high-temperature aging was minimal at 900 °C and modest at 950 °C, but was much larger after 1000 °C. Microhardness was basically unchanged after the 900 °C aging, and decreased only slightly (?3%) after aging at 950 °C and 1000 °C.     

Formation of dislocation loops in silicon by ion irradiation for silicon light emitting diodes

We have studied the influence of the ion species, ion energy, fluence, irradiation temperature and post-implantation annealing on the formation of shallow dislocation loops in silicon, for fabrication of silicon light emitting diodes. The substrates used were (1 0 0) Si, implanted with 20-80 keV boron at room temperature and 75-175 keV silicon at 100 and 200 °C. The implanted fluences were from 5 × 10¹⁴ to 1 × 10¹⁵ ions/cm². After irradiation the samples were processed for 15 s to 20 min at 950 °C by rapid thermal annealing. Structural analysis of the samples was done by transmission electron microscopy and Rutherford backscattering spectrometry. In all irradiations the silicon substrates were not amorphized, and that resulted in the formation of extrinsic perfect and faulted dislocation loops with Burgers vectors a/2〈1 1 0〉 and a/3〈1 1 1〉, respectively, sitting in {1 1 1} habit planes. It was demonstrated that by varying the ion implantation parameters and post-irradiation annealing, it is possible to form various shapes, concentration and distribution of dislocation loops in silicon.     

Plasma assisted synthesis of hollow nanofibers using electrospun sacrificial templates

In this work, we describe the synthesis of nanostructured polymeric materials of controlled tubular geometries using oxygen plasma and polysiloxane-grafting onto electrospun fiber sacrificial templates. The fibers were characterized using Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) to determine the extent of grafting, graft chemistry and the influence of plasma treatment. Scanning electron microscopy (SEM) was used to determine the morphology and size of the electrospun fibers and nanotubes. The average diameter of the electrospun fibers employed ranged between 300 nm and 1500 nm. The micrographs revealed differences that are dependent on the type of grafting chemistry as well as plasma treatment times. The template synthesis of polysiloxane nanotubes using polyester track-etched membranes also shows that the technique is applicable to different substrates.     

High fluence nitrogen implantation in Al/Ti multilayers

We have studied the effects of high fluence nitrogen ion implantation on the structural changes in Al/Ti multilayers, with the aim of achieving multilayered metal-nitrides. The starting structures consisted of 10 alternate sputter-deposited Al and Ti films, with a total thickness of 270 nm, on (1 0 0) Si substrates. They were implanted with 200 keV , to 1 × 10¹⁷ and 2 × 10¹⁷ at/cm², the projected range being around half-depth of the multilayers. Structural characterization was performed by Rutherford backscattering, Auger electron spectroscopy and transmission electron microscopy. It was found that ion implantation to the higher fluence induces a full intermixing of Al/Ti layers, resulting in a multilayered structure with different content of Al, Ti and N. The applied method can be interesting for preparation of graded (Al,Ti)N multilayers, with a controlled content of nitrogen and a controlled level of Al-Ti intermixing within the structures.     

Shortening of multi-walled carbon nanotubes by γ-irradiation in the presence of hydrogen peroxide

Multi-walled carbon nanotubes (MWCNTs) were effectively cut with a facile and mild cutting method by using γ-irradiation in the presence of hydrogen peroxide. The TEM, Raman and XRD results showed that the structural integrity of the cut MWCNTs was preserved with a little surface functionalization.     

Structures of Au nanowires encapsulated in carbon nanotubes

Classical molecular dynamics simulations have been used to investigate the structure of Au nanowires encapsulated in single-walled carbon nanotubes (SWCNT). It was found that Au nanowires with helical multishell structures can be formed within the SWCNTs. Each shell is composed of helical rows of atoms. The distance between the tube wall and the outermost shell of the Au nanowire is about 3 Å, and the spacing between the Au intershells varies from 2.08 to 2.33 Å. The radii of the SWCNTs and the numbers of filled Au atoms play dominant roles in deciding the final structures of the Au nanowires formed within the SWCNTs over the range of diameters considered. In SWCNTs with a given diameter, the Au nanowires with helical multishell structure will be formed when enough Au atoms have filled the nanotube. Otherwise, Au nanowires with a bulky fcc structure will be formed.     

Influence of asymmetric etching on ion track shapes in polycarbonate

By combining low-energy ion irradiation with asymmetric etching, conical nanopores of controlled geometry can be etched in polycarbonate (PC). Cone bases vary from 0.5 to 1 μm. Top diameters down to 17 nm are reached. When etching from one side, the pH on the other side (bathed in neutral or acidic buffer) was monitored. Etching temperature ranged from 65 °C to 80 °C. Pore shape characterization was achieved by electro replication combined with SEM observation. The tip shape depended on whether an acidic buffer was used or not on the stopped side.     

ECR plasma assisted deposition of zinc nanowires

Deposits of one dimensional nanowires of zinc with diameters of 90-120 nm have been obtained by means of dc sputtering within an electron cyclotron resonance plasma reactor. The sputtering has been made effective by using a negatively biased cylindrical target. The structure of the nanocrystalline wires deposited on glass substrates were investigated with scanning electron microscopy, transmission electron microscopy and scanning tunneling microscopy. STM revealed that the structure of the one dimensional nanowires are ensemble of nanoclusters and nanowires with diameter of 4-5 nm. The crystalline nature of the metallic nanowires was studied with X-ray and electron diffraction analysis. The native oxide present on the metallic wires was revealed by photoluminescent spectroscopy. Theoretical modeling has been used to explain the possible mechanisms operative inside the plasma which lead into deposition of zinc on the substrate starting from the precursor species.     

Electroluminescence from metal-oxide-silicon tunneling diode with ion-beam-synthesized β-FeSi2 precipitates embedded in the active region

A metal-oxide-silicon (MOS) tunneling light-emitting diode is fabricated with ion-beam-synthesized β-FeSi₂ precipitates embedded in the active region. Fe ions were implanted into p⁻-100 silicon substrate at cryogenic temperature (∼−120 °C), followed by rapid thermal oxidation (RTO). Under constant voltage biased in accumulation and at temperatures down to 80 K, electroluminescence (EL) with wavelength peaking at ∼1.5 μm is observed at a current density of about 2.0 A/cm². Light output increases linearly with current density. Temperature dependence of the EL shows that the luminescence is due to interband recombination in the crystalline precipitates. The strain in these isolated precipitates may contribute to the luminescence properties of β-FeSi₂ in silicon.     

Nanoporous β-PVDF membranes with selectively functionalized pores

Poly(vinylidene fluoride) (β-PVDF) nanoporous membranes are obtained by heavy ion irradiation and track etching leading to cylindrical pores. Pores diameter measured by scanning electron microscopy and small angle neutron scattering lies in the 20-50 nm range. Electron paramagnetic resonance study gives evidence that radicals still remains in PVDF membrane after track-etching. These radicals allows acrylic acid polymerization to be initiated onto membrane. Radiografted and functionalized membranes are characterized using infrared spectroscopy and weighing. Finally, radiografted poly(acrylic acid) (PAA) has been selectively labeled by fluorophores and imaged by confocal laser scanning microscopy. Images show the localisation of PAA specifically inside nanopores.     

Formation of InAs nanocrystals in Si by high-fluence ion implantation

We have studied the formation of InAs precipitates with dimensions of several nanometers in silicon by means of As (245 keV, 5 × 10¹⁶ cm⁻²) and In (350 keV, 4.5 × 10¹⁶ cm⁻²) implantation at 500 °C and subsequent annealing at 900 °C for 45 min. RBS, SIMS, TEM/TED, RS and PL techniques were used to characterize the implanted layers. The surface density of the precipitates has been found to be about 1.2 × 10¹¹ cm⁻². Most of the crystallites are from 3 nm to 6 nm large. A band at 1.3 μm has been registered in the low-temperature PL spectra of (As + In) implanted and annealed silicon crystals. The PL band position follows the quantum confinement model for InAs.     

Ion beam induced defects in solids studied by optical techniques

Optical methods can provide important insights into the mechanisms and consequences of ion beam interactions with solids. This is illustrated by four distinctly different systems.X- and Y-cut LiNbO₃ crystals implanted with 8 MeV Au³⁺ ions with a fluence of 1 × 10¹⁷ ions/cm² result in gold nanoparticle formation during high temperature annealing. Optical extinction curves simulated by the Mie theory provide the average nanoparticle sizes. TEM studies are in reasonable agreement and confirm a near-spherical nanoparticle shape but with surface facets. Large temperature differences in the nanoparticle creation in the X- and Y-cut crystals are explained by recrystallisation of the initially amorphised regions so as to recreate the prior crystal structure and to result in anisotropic diffusion of the implanted gold.Defect formation in alkali halides using ion beam irradiation has provided new information. Radiation-hard CsI crystals bombarded with 1 MeV protons at 300 K successfully produce F-type centres and V-centres having the structure as identified by optical absorption and Raman studies. The results are discussed in relation to the formation of interstitial iodine aggregates of various types in alkali iodides. Depth profiling of and aggregates created in RbI bombarded with 13.6 MeV/A argon ions at 300 K is discussed.The recrystallisation of an amorphous silicon layer created in crystalline silicon bombarded with 100 keV carbon ions with a fluence of 5 × 10¹⁷ ions/cm² during subsequent high temperature annealing is studied by Raman and Brillouin light scattering.Irradiation of tin-doped indium oxide (ITO) films with 1 MeV protons with fluences from 1 × 10¹⁵ to 250 × 10¹⁵ ions/cm⁻² induces visible darkening over a broad spectral region that shows three stages of development. This is attributed to the formation of defect clusters by a model of defect growth and also high fluence optical absorption studies. X-ray diffraction studies show evidence of a strained lattice after the proton bombardment and recovery after long period storage. The effects are attributed to the annealing of the defects produced.     

Accelerator-based research activities at “Centro Nacional de Aceleradores”, Seville (Spain)

In February 1998, almost 10 years ago, the set-up of the first IBA (ion beam analysis) facility in Spain took place with the arrival of a 3 MV tandem accelerator [J. García-López, F.J. Ager, M. Barbadillo-Rank, F.J. Madrigal, M.A. Ontalba, M.A. Respaldiza, M.D. Ynsa, Nucl. Instr. and Meth. B 161-163 (2000) 1137]. Since then, an intensive research program using IBA techniques has been carried out. Subsequently, a cyclotron for 18 MeV protons has been also installed at the “Centro Nacional de Aceleradores” (CNA), devoted mainly to isotope production for PET (positron emission tomography) techniques, but possibly applied to material analysis and damage studies on a dedicated beam line. Moreover, a 1 MV tandem has been recently installed for AMS (accelerator mass spectrometry) ¹⁴C dating and environmental research with other isotopes.In the present paper we describe the new facilities and the developments of the 3 MV tandem beam lines occurred during the past years, as well as some examples of the most recent research activities in our Center in the fields of Material Science, Archaeometry, Biomedicine and Environment.     

Status of the compact 1 MV AMS facility at the Centro Nacional de Aceleradores (Spain)

Since February 2006, the new 1 MV multielement compact AMS facility SARA (Spanish Accelerator for Radionuclides Analyses) at the Centro Nacional de Aceleradores (CNA) in Sevilla (Spain) is fully operative. During the first one and a half year of operation, the viability of the system for the measurement of ¹⁰Be, ¹⁴C, ¹²⁹I and plutonium isotopes, ²³⁹Pu and ²⁴⁰Pu, has been evaluated. First results have demonstrated that, in terms of precision and detection limits, the performance of the device compares to other compact AMS facilities, although some progress can still be done in order to optimize its capacities. At this moment, background levels are in the order of 10⁻¹⁴ for ¹⁰Be/⁹Be, 10⁻¹³ for ¹²⁹I/¹²⁷I, 10⁻¹⁵ for ¹⁴C/¹²C (processed and unprocessed blank) and about 10⁶ atoms for plutonium isotopes: ²³⁹Pu, ²⁴⁰Pu and ²⁴²Pu. In this work, the current status of the AMS measurements at CNA for the above mentioned radionuclides is described.     

Effect of swift heavy ion irradiation on nanocrystalline CaS:Bi phosphors: Structural, optical and luminescence studies

Luminescence studies of CaS:Bi nanocrystalline phosphors synthesized by wet chemical co-precipitation method and irradiated with swift heavy ions (i.e. O⁷⁺-ion with 100 MeV and Ag¹⁵⁺-ion with 200 MeV) have been carried out. The samples have been irradiated at different ion fluences in the range 1 × 10¹²-1 × 10¹³ ions/cm². The average grain size of the samples before irradiation was estimated as 35 nm using line broadening of XRD (X-ray diffraction) peaks and TEM (transmission electron microscope) studies. Our results suggest a good structural stability of CaS:Bi against swift heavy ion irradiation. The blue emission band of CaS:Bi³⁺ nanophosphor at 401 nm is from the transition ³P₁ → ¹S₀ of the Bi³⁺. We have observed a decrease in lattice constant (a) and increase of optical energy band gap after ion irradiation. We presume this change due to grain fragmentation by dense electronic excitation induced by swift heavy ion. We have studied the optical and luminescent behavior of the samples by changing the ion energy and also by changing dopant concentration from 0.01 mol% to 0.10 mol%. It has been examined that ion irradiation enhanced the luminescence of the samples.