Irradiation Step Research Articles

Mechanical and microstructural changes in tungsten due to irradiation damage

Stress-relieved pure tungsten received three damage levels (0.10, 0.25 and 0.50 dpa) by self-tungsten ion beam irradiation at room temperature. Positron annihilation spectroscopy showed the formation of mono-vacancies and vacancy clusters after ion beam exposure. In the first irradiation step (0–0.10 dpa) some splitting up of large vacancy clusters occurred which became more numerous. For increasing dose to 0.25 dpa, growth of the vacancy clusters was seen. At 0.50 dpa a change in the defect formation seems to occur leading to a saturation in the lifetime signal obtained from the positrons. Nano-indentation on the cross-sections showed a flat damage depth distribution profile. The nano-indentation hardness increased for increasing damage dose without any saturation up to 0.50 dpa. This means that other defects such as dislocation loops and large sized voids seem to contribute.

Synthesis and Spectral Characterization of Novel nano-Hydroxyapatite from Moringaoleifera Leaves

The conversion of green food materials into biocompatible materials (biomaterials) used in medical surgery and therapeutics is a strategy. Nano- hydroxyapatite (n-HAP, Ca10 (PO4) 6 (OH) 2) was produced from Moringaoleifera leaves using a rapid microwave irradiation method. Moringaoleifera leaves was converted to flakes like n-HAP particles using EDTA as a chelating agent after an appropriate pre-treatment and an irradiation step in a microwave. The as-synthesized n-HAP was characterized using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) coupled with energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR). The process of transforming Moringaoleifera leaves into nano-hydroxyapatite is an environmentally friendly process. Moringaoleifera leaves based nano-hydroxyapatite stand as good chance of reducing the cost of treatment in bone repair.

The influence of high-energy electrons irradiation on the electrical properties of Schottky barrier detectors based on semi-insulating GaAs

In this work we fabricated detectors based on semi-insulating GaAs and studied their electrical properties (current-voltage characteristics, galvanomagnetic measurements) after irradiation with 5 MeV electrons from a linear accelerator up to a dose of 104 kGy. A series of detectors were prepared using Ti/Pt/Au Schottky contact with 1 mm diameter. The thickness of the base material was about 230 μm. A whole area Ni/AuGe/Au ohmic contact was evaporated on the back side. For galvanomagnetic measurements we used three samples from the same wafer. All samples were irradiated by a pulse beam of 5 MeV electrons using the linear accelerator in 11 steps, where the accumulative dose increased from 1 kGy up to 104 kGy. Also different dose rates (20, 40 and 80 kGy/h) were applied to the samples. After each irradiation step we performed electrical measurement of each sample. We analyze the electron Hall mobility, resistivity, electron Hall concentration, breakdown voltage and reverse current of samples before and after irradiation using different dose rates.

Accelerated weathering performance of polylactide and its montmorillonite nanocomposite

The goal of this study was to compare accelerated weathering performance of neat polylactide (PLA) and its 1 mass% organically modified montmorillonite (Mt) nanocomposite; compounded and shaped by twin-screw extrusion melt mixing and injection molding, respectively. Accelerated weathering test system applied consecutive steps of UV irradiation and humidity in accordance with ISO 4892-3 standards for 200h. Chain scission reactions such as photolysis, photooxidation and hydrolysis resulted in significant decrease in the molecular weight of PLA; consequently reductions in the mechanical properties of modulus, strength, ductility and toughness of the specimens occurred. However, after comparing mechanical properties of PLA and Mt–PLA before and after 200h accelerated weathering, use of PLA with only 1 mass% Mt was extremely beneficial not only for “indoor applications” but also for “outdoor applications”. This was due to the effective nanoscale reinforcing and barrier actions of intercalated/exfoliated Mt layers. For example, flexural strength was 6% beneficial before weathering, but after weathering the benefit was 88%.

Electron Processing at 50 eV of Terphenylthiol Self-Assembled Monolayers: Contributions of Primary and Secondary Electrons.

Aromatic self-assembled monolayers (SAMs) can serve as platforms for development of supramolecular assemblies driven by surface templates. For many applications, electron processing is used to locally reinforce the layer. To achieve better control of the irradiation step, chemical transformations induced by electron impact at 50 eV of terphenylthiol SAMs are studied, with these SAMs serving as model aromatic SAMs. High-resolution electron energy loss spectroscopy (HREELS) and electron-stimulated desorption (ESD) of neutral fragment measurements are combined to investigate electron-induced chemical transformation of the layer. The decrease of the CH stretching HREELS signature is mainly attributed to dehydrogenation, without a noticeable hybridization change of the hydrogenated carbon centers. Its evolution as a function of the irradiation dose gives an estimate of the effective hydrogen content loss cross-section, σ = 2.7-4.7 × 10(-17) cm(2). Electron impact ionization is the major primary mechanism involved, with the impact electronic excitation contributing only marginally. Therefore, special attention is given to the contribution of the low-energy secondary electrons to the induced chemistry. The effective cross-section related to dissociative secondary electron attachment at 6 eV is estimated to be 1 order of magnitude smaller. The 1 eV electrons do not induce significant chemical modification for a 2.5 mC cm(-2) dose, excluding their contribution.

Mechanical and thermal properties of polylactide/talc microcomposites: before and after accelerated weathering

The purpose of the first part of this study was to investigate effects of micron-sized talc content on the properties of polylactide (PLA). PLA/talc microcomposites were compounded by melt-mixing method via twin-screw extruder, while specimens for testing and analyses were shaped by injection molding. It was observed that, because of the effective stiffening, strengthening, toughening mechanisms of talc, and also their nucleation agent effects for higher crystallinity, many mechanical and thermal properties were improved. In the second part of the study, effects of accelerated weathering on the behavior of PLA microcomposites with 5 wt% talc were investigated by applying ultra violet irradiation and humidity steps according to Cycle-C of International Organization for Standardization 4892-3 standards for durations of 100, 200, and 300 hr. Various analyses revealed that, because of the degradation mechanisms of photolysis and hydrolysis during each weathering periods, molecular weight of PLA reduced drastically, that is, mechanical properties almost vanished. Copyright © 2015 John Wiley & Sons, Ltd.

Effect of the positional isomerism on the photoreactivity of styryloxazoles

Abstract This paper describes the results obtained in the study of the photobehaviour of heteroanalogs of stilbene bearing an oxazole ring. The competitive relaxation processes (fluorescence, isomerization and cyclization) of the excited states of n-styryloxazoles (n = 2 and 4) were investigated and compared with the behaviour previously reported for n = 5. After preparation of the unknown compound with n = 4 and of its positional isomer with n = 2 (the latter with a new method of synthesis), their photobehaviour was firstly investigated in preparative conditions by NMR analysis to measure the chemical yields of their photoproducts. The study was then continued in mild irradiation conditions to measure the quantum yields of the competitive photoreactions in the primary irradiation steps. The effects of the position of the styryl group at the oxazole ring, the relative abundance of the various conformers and the possible formation of intramolecular H bonds on the deactivation pathways are described. Quantum-mechanical Hyperchem calculations proved to be very useful to describe the conformational equilibria and the role of conformers on photoreactivity while more refined DFT calculations on the Z isomers allowed to explain the structure dependent competition between their isomerization/cyclization processes. The effect of the replacement of the phenyl ring with a second heteroaromatic group of electron donor character was investigated for the 5-(2-(furan-2-yl) ethenyl) oxazole.

Potential routes to stronger carbon nanotube fibres via carbon ion irradiation and deposition

Fibres made from carbon nanotubes (CNTs) have not yet achieved strengths approaching that of individual CNTs. The problem is that load is not effectively transferred between the constituent, discontinuous CNTs. High energy irradiation has shown promise on small CNT bundles, in creating covalent cross-links to enhance load transfer, but cannot sufficiently penetrate real CNT fibres, which typically contain 106 or more CNTs. Here, we suggest that the “draw-twist” process for producing CNT fibres from forests offers an opportunity for CNT bundles to be individually treated with irradiation before being twisted to form a fibre. We use molecular dynamics to examine the effectiveness of low energy (1 eV) carbon ion irradiation (or deposition) in this context. We find that very small amounts of deposition can significantly enhance both intra-bundle and inter-bundle load transfer. Within bundles, deposition atoms mediate covalent links between both the sides and ends of neighbouring CNTs. Inter-bundle load transfer is improved as under-coordinated carbon adatom branches formed during deposition, spontaneously form inter-bundle cross-links as the bundles are forced together by the twisting action. The effects of varying fluence and twisting angles are examined, and the potential to add a prior higher energy irradiation step to penetrate larger bundles is explored. The possibility to produce an amorphous carbon/CNT composite fibre is also discussed.

Photoinduced hydrophilic conversion of hydrated ZnO surfaces

Here we focused on the study of the effect of the zinc oxide nano-coatings surface acidity on the surface hydrophilicity and photoinduced hydrophilic conversion. A three-step procedure was used to have the initial state of the ZnO surface free of organics and to control the conditions during the water wetting and the irradiation steps. The kinetics of photoinduced hydrophilic conversions for ZnO films were obtained and demonstrated a dependence on the initial hydrophilic state. No conversion into the superhydrophilic state was observed for ZnO nano-films independently of the surface acidity. Irradiation in the ultraviolet and visible spectral regions showed the existence of “slow” and “fast” processes in the photoinduced hydrophilic conversion of the ZnO surface. A multi-layered model of hydroxyl-hydrated coverage of the surface is proposed to explain the experimental results.

Comparison of the neutron and ion irradiation response of nano-oxides in oxide dispersion strengthened materials

Abstract

Consequences of accelerated weathering in polylactide nanocomposites reinforced with halloysite nanotubes

The purpose of this study was to explore consequences of accelerated weathering on the behavior of polylactide/halloysite nanotube composites. Nanocomposites were compounded by melt mixing method via a twin-screw extruder while specimens for testing and analyses were shaped by injection molding. Behaviors of the specimens were compared before weathering and after exposure to UV irradiation and humidity steps according to Cycle-C of ISO 4892-3 standards for a total duration of 300 h. IR studies revealed that photolysis and partly hydrolysis were the main degradation mechanisms leading to random main chain scission of the PLA macromolecular structure, which was reflected with drastic reductions both in the molecular weight of PLA and the mechanical properties of flexural strength and fracture toughness. On the other hand, no significant reductions were observed in the values of thermal degradation temperatures, storage modulus and flexural modulus of the specimens, which was due to the compensating effect of higher amounts of crystallinity formed during UV irradiation cycles at 70℃.

Newly Elaborated Multipurpose Polymer Electrolyte Encompassing RTILs for Smart Energy-Efficient Devices.

Profoundly ion-conducting, self-standing, and tack-free ethylene oxide-based polymer electrolytes encompassing a room-temperature ionic liquid (RTIL) with specific amounts of lithium salt are successfully prepared via a rapid and easily upscalable process including a UV irradiation step. All prepared materials are thoroughly characterized in terms of their physical, chemical, and morphological properties and eventually galvanostatically cycled in lab-scale lithium batteries (LIBs) exploiting a novel direct polymerization procedure to get intimate electrode/electrolyte interfacial characteristics. The promising multipurpose characteristics of the newly elaborated materials are demonstrated by testing them in dye-sensitized solar cells (DSSCs), where the introduction of the iodine/iodide-based redox mediator in the polymer matrix assured the functioning of a lab-scale test cell with conversion efficiency exceeding 6% at 1 sun. The reported results enlighten the promising prospects of the material to be successfully implemented as stable, durable, and efficient electrolyte in next-generation energy conversion and storage devices.

Deep ultraviolet laser direct write for patterning sol-gel InGaZnO semiconducting micro/nanowires and improving field-effect mobility.

Deep-UV (DUV) laser was used to directly write indium-gallium-zinc-oxide (IGZO) precursor solution and form micro and nanoscale patterns. The directional DUV laser beam avoids the substrate heating and suppresses the diffraction effect. A IGZO precursor solution was also developed to fulfill the requirements for direct photopatterning and for achieving semi-conducting properties with thermal annealing at moderate temperature. The DUV-induced crosslinking of the starting material allows direct write of semi-conducting channels in thin-film transistors but also it improves the field-effect mobility and surface roughness. Material analysis has been carried out by XPS, FTIR, spectroscopic ellipsometry and AFM and the effect of DUV on the final material structure is discussed. The DUV irradiation step results in photolysis and a partial condensation of the inorganic network that freezes the sol-gel layer in a homogeneous distribution, lowering possibilities of thermally induced reorganization at the atomic scale. Laser irradiation allows high-resolution photopatterning and high-enough field-effect mobility, which enables the easy fabrication of oxide nanowires for applications in solar cell, display, flexible electronics, and biomedical sensors.

Trehalose glycopolymer resists allow direct writing of protein patterns by electron-beam lithography.

Direct-write patterning of multiple proteins on surfaces is of tremendous interest for a myriad of applications. Precise arrangement of different proteins at increasingly smaller dimensions is a fundamental challenge to apply the materials in tissue engineering, diagnostics, proteomics and biosensors. Herein we present a new resist that protects proteins during electron beam exposure and its application in direct-write patterning of multiple proteins. Polymers with pendant trehalose units are shown to effectively cross-link to surfaces as negative resists, while at the same time providing stabilization to proteins during the vacuum and electron beam irradiation steps. In this manner, arbitrary patterns of several different classes of proteins such as enzymes, growth factors and immunoglobulins are realized. Utilizing the high precision alignment capability of electron-beam lithography, surfaces with complex patterns of multiple proteins are successfully generated at the micrometer and nanometer scale without requiring cleanroom conditions.

High-energy photon activation tandem mass spectrometry provides unprecedented insights into the structure of highly sulfated oligosaccharides extracted from macroalgal cell walls.

Extreme ultraviolet photon activation tandem mass spectrometry (MS) at 69 nm (18 eV) was used to characterize mixtures of oligo-porphyrans, a class of highly sulfated oligosaccharides. Porphyrans, hybrid polymers whose structures are far from known, continue to provide a challenge for analytical method development. Activation by 18 eV photons led to a rich fragmentation of the oligo-porphyrans, with many cross-ring and glycosidic cleavages. In contrast to multistage MSn strategies such as activated electron photodetachment dissociation, a single step of irradiation by energetic UV of multiply charged anions led to a complete fragmentation of the oligo-porphyrans. In both ionization modes, the sulfate groups were retained on the backbone, which allowed the pattern of these modifications along the porphyran backbone to be described in unprecedented detail. Many structures released by the enzymatic degradation of the porphyran were completely resolved, including isomers. This work extends the existing knowledge of the structure of porphyrans. In addition, it provides a new demonstration of the potential of activation by high-energy photons for the structural analysis of oligosaccharides, even in unseparated mixtures, with a particular focus on sulfated compounds.

Fabrication of 3D photonic components on bulk crystalline silicon.

We have fabricated three dimensional photonic components such as waveguides and beam splitters from crystalline silicon using a process based on one or more ion irradiation steps with different energies and fluences, followed by electrochemical anodization and thermal annealing. We first demonstrate the fabrication of multilevel silicon waveguides and then extend this process to make multilevel beam splitters, in which three output waveguides are distributed over two depths. The dimensions of the waveguides can be defined within a range from 0.5 μm to several micrometers simply by varying the ion beam fluence.

Irradiation of the CLARO-CMOS chip, a fast ASIC for single-photon counting

The CLARO-CMOS is a prototype ASIC that allows fast photon counting with low power consumption, built in AMS 0.35μm CMOS technology. It is intended to be used as a front-end readout for the upgraded LHCb RICH detectors. In this environment, assuming 10 years of operation at the nominal luminosity expected after the upgrade, the ASIC must withstand a total fluence of about 6×1012 1MeVneq/cm2 and a total ionising dose of 400krad. Long term stability of the electronics front-end is essential and the effects of radiation damage on the CLARO-CMOS performance must be carefully studied. This paper describes results of multi-step irradiation tests with protons up to the dose of ~8Mrad, including measurement of single event effects during irradiation and chip performance evaluation before and after each irradiation step.

Micromechanical properties of one-step and sequentially crosslinked UHMWPEs for total joint replacements

Microindentation hardness testing was applied to five types of highly-crosslinked ultrahigh molecular weight polyethylenes (UHMWPEs) for total joint replacements. UHMWPE's were crosslinked using the same total radiation dose (75 kGy; γ-radiation) either by the standard, single-step irradiation (one-step crosslinking) or by the newer, several-step irradiation (sequential crosslinking). Each irradiation step was followed by thermal treatment (annealing at 110 °C or remelting at 150 °C) in an inert atmosphere. We showed that: (i) the micromechanical properties were determined by the last thermal treatment step, while the number of irradiation cycles was insignificant and (ii) the values of microhardness, microcreep and microplasticity from the microindentation experiments were in excellent agreement with the changes of UHMWPE structure, characterized by IR and DSC. Statistical evaluation of the results, the agreement with theoretical predictions and the comparison with previous studies on similar systems demonstrated that microindentation was a reliable and sensitive method of UHMWPE characterization.

Synthesis of nano-hydroxyapatite (nHA) from waste mussel shells using a rapid microwave method

Nano-crystalline hydroxyapatite (HA, Ca10(PO4)6(OH)2) was produced from waste mussel shells using a rapid microwave irradiation method. Mussel shells were converted to rod like nano-crystalline HA particles of 30–70 nm long using 0.1 M EDTA as a chelating agent for 30 min after an appropriate pre-treatment and an irradiation step in a microwave with a power of 1.1 kW. The produced HA was characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), thermo gravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR) and inductively coupled plasma mass spectrometry (ICP-MS) to determine the morphology, particle size, crystal phases, elemental composition and thermal behaviour. Furthermore, to benchmark the synthesized HA obtained from mussel shells, it was compared with a commercially pure HA (Sigma–Aldrich). The thermal analysis showed that the synthesized HA has remarkable heat stability at 1000 °C, and the XRD and FTIR results showed a high purity of the synthesized HA powders. Compared to the conventional hydrothermal treatment, microwave-assisted method has the advantages of an increased rate of HA formation. The obtained HA have potential engineering applications as materials for bone-tissues.

Fabrication and characterization of glassy carbon membranes

In this work, the authors focus on a method to fabricate arbitrary shaped free standing membranes with a thickness less than 20 nm, produced from different polymers with the help of low-energy ion irradiation. The authors analyze the thickness of the membranes and its dependence on the details of the irradiation process. In order to tune the properties of the suspended membranes, an additional ion irradiation step has been used. This step is applied to already suspended membranes and leads to several effects, such as heating, shape transformation, etc. These effects were analyzed for irradiation with Ar+ and He+ ions. The authors have found that He+ irradiation has a significant advantage over Ar+ irradiation providing strained, smooth, and homogeneous membranes. In order to measure the electrical properties of the suspended membranes, the authors invented a new method to contact the membranes. These low resistance contacts can be achieved as the authors describe in detail. The membranes electrical properties after He+ ion irradiation at different temperatures are presented. Finally, the authors analyze Raman spectra, and thermal and electrical conductivity of the highly conducting membranes. The authors conclude that after high temperature He+ ion irradiation the membranes consist of material similar in properties to the glassy carbon obtained by pyrolysis. However, this method does not require high temperature pyrolysis step, which makes integration with on-chip electronics more feasible.