Non-destructive Ion Research Articles

Application of non-destructive analysis methods in TENMAK-PAF

Development of non-destructive analysis systems at the R&D beamline of the Proton Accelerator Facility of the Turkish Energy, Nuclear and Minerals Research Agency (TENMAK-PAF) is described in this work. The proton beam from the cyclotron with energy between 15–30 MeV and current between 0.1 μA–1.2 mA is modified with several components and subsystems to be suitable for the application of non-destructive analysis methods. Certified reference materials (CRM) and samples with different properties were irradiated under vacuum in the irradiation chamber with the new system. Particle Induced X-ray Emission (PIXE) and Particle Induced Gamma ray Emission (PIGE) spectra of these samples were obtained with appropriate radiation detectors and measurement systems. The results of PIXE analyses and X-ray fluorescence (XRF) spectrometry were compared. PIXE and PIGE results are in good agreement with the certified values for the CRMs. This work constitutes the first reported application of non-destructive ion beam analysis methods in TENMAK-PAF and in Türkiye.

Development of electrostatic-induced charge detector for multiturn time-of-flight mass spectrometer.

We developed an autocorrelation function to resolve the overtaking problem in a multiturn time-of-flight mass spectrometer (TOF-MS). The function analyzes the characteristic period for one lap of each ion packet and derives a mass spectrum from a signal pulse train composed of multiturn ion packets. To detect the ion pulse train, a new nondestructive ion detector was developed and installed in the multiturn orbit of MULTUM-S II. This detector is composed of an electrostatically induced charge detector, a preamplifier, and a digitizer. The electrostatic noises are smaller than the single-ion signals owing to the accumulation of the multiturn TOF spectrum. The conventional ion detector of TOF-MS is operated after collecting the signal pulse train. The multiturn TOF spectrum was convolved with an autocorrelation function to derive the mass spectrum. The convolved mass spectrum performed a mass resolving power (MRP) of 28,200 at m/z 69 and mass accuracy of 28 ppm for the perfluorotributylamine (PFTBA) gas sample.

Non-invasive probing of dynamic ion migration in light-emitting electrochemical cells by an advanced nanoscale confocal microscope

In this study, we firstly propose an optical approach to investigate the ion profile of organic films in light-emitting electrochemical cells (LECs) without any invasive sputtering processes. In contrast to previous literatures, this pure optical strategy allows us to record clear and non-destructive ion profile images in the (Ru(dtb-bpy)3(PF6)2) consisted organic layer without interferences of complex collisions from the bombardment of secondary sputter induced ions in a conventional time-of-flight secondary ion mass spectrometry. By using the advanced position sensitive detector (PSD)-based Nanoscale Confocal Microscope, ion distribution profiles were successfully acquired based on the observation of nanoscale optical path length difference by measuring the refractive-index variation while the thickness of the LEC layer was fixed. Dynamic time-dependent ion profile displayed clear ion migration process under a 100 V applied bias at two ends of the LEC. This technique opens up a new avenue towards the future investigations of ion distributions inside organic/inorganic materials, Li-ion batteries, or micro-fluid channels without damaging the materials or disturbing the device operation.

Synthesis of CoZn nanowire in anodic aluminum templets and their characterization by Rutherford backscattering spectrometry

In this research, the CoZn alloy nanowire arrays were deposited in a porous aluminum oxide template by alternative current pulse electrodeposition. The aluminum oxide template was fabricated through two-step soft anodization of pure aluminum foils and its morphology was determined using a scanning electron microscope.In order to systematically study the constructed sample, non-destructive ion beam analysis techniques were used. Among these methods, Rutherford backscattering spectrum analysis was performed by interaction of proton ions with energy of 2000 keV and 2500 keV and helium ions with energy of 2500 keV with the sample. Analysis of the RBS spectrum of the sample along with simulations performed by SIMNRA code made it possible to determine the concentration, depth profile of the elements in the sample, and determination of stoichiometry of the alumina template at different depths. The best results are related to a proton with energy 2500 keV, which reported the depth of 10 to 14 μm for CoZn alloy nanowire. Also, for validation of the results, FE-SEM images were prepared from the sample, which confirms the agreement with the results obtained from the RBS method.

Photochromism in Isotopically Labeled Oxygen‐Containing Yttrium−Hydride and Deuteride Thin‐Film Systems

Photochromic mono‐ and bilayered thin films of oxygen‐containing isotope‐labeled yttrium−hydride (i.e., protium and deuterium) are synthesized via reactive Ar sputtering. Selected samples are encapsulated with transparent diffusion barriers. Combining depth‐resolved nondestructive ion beam‐based techniques for composition and optical spectrophotometry, material mobility in the samples during illumination and over time is investigated. The results reveal that deuteride thin films exhibit a strong photochromic response equivalent to hydrogenated systems. No evidence of long‐distance light‐induced hydrogen mobility or thermal diffusion is found. The findings thus show that photochromism is not connected to long‐distance material transport. The observations for encapsulated samples also exclude direct material exchange with the environment and any environmental influence on material mobility.

Tantalum coating inhibits Ni-migration from titanium out-diffusion in NiTi shape memory biomedical alloy

Despite the presence of over 56% Ni by weight, equiatomic NiTi is generally considered biocompatible as it naturally oxidises to form a surface oxide mainly composed of biocompatible oxides of titanium (TiOx). This layer is formed by an oxidation mechanism that promotes out-diffusion of Ti leaving a Ti-depleted, Ni rich subsurface. The long-term in vivo stability of the naturally grown TiOx layer has been a concern as Ni can leach out through this thin, defective layer. The leaching of nickel (Ni) is thus a continuing threat to the alloy’s otherwise outstanding biocompatibility. We have found that a layer of reactively sputtered tantalum (Ta) oxide on the bulk NiTi restricts Ti-out-migration through a biocompatible Ti/Ta inter-diffusion layer that provides a larger barrier against Ni leaching. We have investigated this inter-diffusion as a function of sputtering process parameters and post processing treatments. Surface and interface analytical techniques such as X-ray photoelectron spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy, cross sectional transmission electron microscopy and non-destructive ion beam analysis techniques such as Rutherford backscattering spectrometry and particle induced X-ray emission were used to evaluate the nature of this inter-diffusion layer which can improve long-term biocompatibility of NiTi.

Synthesis and in-situ characterization of photochromic yttrium oxyhydride grown by reactive e−-beam evaporation

We report on controlled growth of photochromic yttrium oxyhydride thin films monitored by in-situ composition depth profiling. Films were grown by reactive e−-beam evaporation and subsequently oxidized, while simultaneously tracking the oxygen and hydrogen concentrations. Sample composition and photochromic response were characterized in-situ using non-destructive ion beam analysis and image analysis, respectively – as well as complementary ex-situ ion beam methods, X-ray diffraction and optical spectrophotometry. We show that photochromic yttrium oxyhydride can be grown as yttrium dihydride, which is then oxidized to O/H ratios triggering the photochromic response.

Characterisation of ion bunches by a single-pass non-destructive charge counter

SynopsisWe present non-destructive single-pass ion bunch detection and characterisation by measuring the induced image charge in a detection electrode. The presented technique allows direct determination of ion kinetic energy, absolute ion number and spatial ion bunch length. We will show the results of corresponding measurements with bunches of low-energy highly charged ions and discuss the minimum detectable number of charges.

In-situ composition analysis of photochromic yttrium oxy-hydride thin films under light illumination

In this work, we investigate the chemical composition of a reactively sputtered photochromic YHxOy thin film by non-destructive ion beam-based techniques, i.e., Rutherford Backscattering Spectrometry, Particle-Induced X-Ray Emission, Time-of-Flight/Energy coincidence Elastic Recoil Detection Analysis and Elastic Backscattering Spectrometry. To enhance the accuracy of the analysis, the set of spectra was evaluated in an iterative self-consistent approach. This procedure resulted in high-resolution depth profiles of the chemical composition and revealed a thin oxygen-rich-layer on the surface, which apparently does not act as a self-passivation layer. In the film, the concentration of Y remains practically constant, whereas O replaces H during the oxidation process. In-situ light illumination was performed during the compositional analysis in a high vacuum setup. The results from these measurements demonstrate that, for these samples, the induced reversible photochromism is not linked to any detectable change in the bulk composition of the film and can thus take place even in a vacuum environment.

First experimental measurements of a new fast ion driven micro-burst instability in a field-reversed configuration plasma

In modern field-reversed configuration (FRC) experiments (Binderbauer et al 2015 Phys. Plasmas 22 056110) at TAE Technologies, classical FRC instabilities are suppressed by advanced neutral beam injection and edge biasing methods, leading to high plasma confinement and fast ion pressure built-up which is comparable to the bulk plasma pressure. In some of these high performance FRC plasmas, a new macroscopically non-destructive fast ion driven micro-burst instability is observed as periodic small amplitude bursts with frequency down chirping in the diamagnetic drift frequency range, repeating about every 0.1 to 0.5 ms. The occurrence of these micro-bursts and burst-free operation can be controlled by changing the injected neutral beam energy. Major observed characteristics of this new instability are presented. Possible explanation of the phenomenon is suggested.

Analysis and modification of natural red spinel by ion beam techniques for jewelry applications

Abstract Natural spinel (MgAl2O4) can be found in several colors resembling corundum, i.e. rubies and sapphires. In particular, spinels with saturated red appearance, called spinel-rubies or balas rubies, are the most appreciated. However, the beautiful rich red spinels are very rare, they can be found in a range of pastel shades blended with either brown, orange or purple. Therefore, the objectives of the present studies are to investigate the origins of the color blending and to improve the optical property of this gemstone by ion beam techniques. Two non-destructive ion beam analysis techniques, i.e., particle induced X-ray emission (PIXE) and iono-luminescence (IL), have been employed for geochemical analysis of the gems. As an alternative method, ion beam treatment using N2-ion was applied for improving optical appearance and color enhancement of the red Burmese (Myanmar) spinel. For each run, samples were implanted at ion energy of 70 keV to a fluence of ~ 1 × 1017 ions/cm2 and subsequently surface cleaning. UV-Vis spectroscopy, Raman spectroscopy and photoluminescence spectroscopy were selected for sample characterization. As for comparison, the spinel samples from the same origin were heated in air and undergone the same measurement. We have found that the color appearance of spinel can be engineered by both techniques. However, the heating has transformed the normal or the ordered spinel to the inverse or the disordered one, and thus disorder might be used as criteria to determine if the stone has been heated. On the other hand, the crystalline structure of the spinel remains almost the same or slightly disordered after ion implantation. This finding leads to future applications for jewelry.

Nanostructure imaging mass spectrometry: the role of fluorocarbons in metabolite analysis and yoctomole level sensitivity.

Nanostructure imaging mass spectrometry (NIMS) has become an effective technology for generating ions in the gas phase, providing high sensitivity and imaging capabilities for small molecules, metabolites, drugs, and drug metabolites. Specifically, laser desorption from the nanostructure surfaces results in efficient energy transfer, low background chemical noise, and the nondestructive release of analyte ions into the gas phase. The modification of nanostructured surfaces with fluorous compounds, either covalent or non-covalent, has played an important role in gaining high efficiency/sensitivity by facilitating analyte desorption from the nonadhesive surfaces, and minimizing the amount of laser energy required. In addition, the hydrophobic fluorinated nanostructure surfaces have aided in concentrating deposited samples into fine micrometer-sized spots, a feature that further facilitates efficient desorption/ionization. These fluorous nanostructured surfaces have opened up NIMS to very broad applications including enzyme activity assays and imaging, providing low background, efficient energy transfer, nondestructive analyte ion generation, super-hydrophobic surfaces, and ultra-high detection sensitivity.

Development of a PIXE method at high energy with the ARRONAX cyclotron

The high energy PIXE (HEPIXE) method is a multi-elemental non-destructive ion beam analysis technique. It is based on the detection of the X-ray emitted due to the interaction of high energy particle beam with a sample. This technique is fast and allows the analysis of heavy and medium elements in thin (lm), thick (mm) and multilayer samples. At the ARRONAX facility (Nantes, France), the HEPIXE method has been used to determine the composition of natural and synthetic sodalites. Photochromic properties of these samples are supposed to come from the trace elements (concentration in the ppm range) present in the samples. Taking advantage of the 70 MeV proton beam available at our facility, the HEPIXE method has been also used to study multilayer samples. It has been shown that it is possible to determine the composition of each layer, their thicknesses and their depth position by analyzing the recorded X-ray spectra.

Development of a PIGE-Detection System for in-situ Inspection and Quality Assurance in the Evolution of Fast Rotating Parts in High Temperature Environment Manufactured from TiAl

Intermetallic γ-titanium aluminides are a promising material in high temperature technologies. Their high specific strength at temperatures above 700°C offers the possibility for their use as components of aerospace and automotive industries. With a specific weight of 50% of that of the widely used Ni-based superalloys TiAl is very suitable as material for fast rotating parts like turbine blades in aircraft engines and land based power stations or turbocharger rotors. Thus lower mechanical stresses and a reduced fuel consumption and CO 2 -emission are expected. To overcome the insufficient oxidation protection the halogen effect offers an innovative way. After surface doping using F-implantation or liquid phase-treatment with an F-containing solution and subsequent oxidation at high temperatures the formation of a protective alumina scale can be achieved. By using non-destructive ion beam analyses (PIGE, RBS) F was found at the metal/oxide interface. For analysis of large scale components a new vacuum chamber at the IKF was installed and became operative. With this prototype of in-situ quality assurance system for the F-doping of manufactured parts from TiAl some performance test measurements were done and presented in this paper. Received: 01 March 2013; Revised: 24 April 2013; Accepted: 25 April 2013

Mechanism of oxide layer growth during annealing of NiTi

After annealing at 540°C, NiTi is covered by a characteristic oxide layer with an Ni-containing outer and an Ni-free inner titanium oxide region. To elucidate details of the yet unclear formation process, samples were annealed in an atmosphere containing different oxygen isotopes at a time and analyzed by nondestructive ion beam techniques at different stages of the oxidation. During the heating stage, an oxygen permeable "low Ni" titanium oxide forms, and the oxide layer grows inward. Subsequently, when the annealing temperature of 540°C is reached, Ni-free stoichiometric titanium oxide forms and inhibits the transport of oxygen toward the bulk. Thus, the oxide layer growth changes to outward, and the final location of the reaction front between O and Ti is inside the oxide layer at the transition of "low Ni" oxide to "Ni-free" oxide. Consequently, the annealing conditions during inward oxide layer growth govern the surface properties, whereas the conditions during outward oxide layer growth are uncritical with respect to the surface properties. The findings are directly applicable to set the amount of surface Ni of NiTi devices, provide basis for detailed interpretation of experimental results involving annealing of NiTi, and can further respective modeling.

Lifetime measurements in an electrostatic ion beam trap using image charge monitoring

A technique for mass-selective lifetime measurements of keV ions in a linear electrostatic ion beam trap is presented. The technique is based on bunching the ions using a weak RF potential and non-destructive ion detection by a pick-up electrode. This method has no mass-limitation, possesses the advantage of inherent mass-selectivity, and offers a possibility of measuring simultaneously the lifetimes of different ion species with no need for prior mass-selection.

Integrating Non-Destructive Ion Beam Analysis Methods and AMS Radiocarbon Dating for the Study of Ancient Bronze Statues

Analytical methods based on particle accelerators are widely used in cultural heritage diagnostics and archaeological sciences from the absolute dating of organic materials by means of radiocarbon accelerator mass spectrometry (AMS) to the analysis of the elemental composition of a wide range of materials (metals, obsidians, pottery) via ion beam analysis (IBA) techniques. At CEDAD (Centre for Dating and Diagnostics), the accelerator facility of the University of Salento, AMS 14C dating and PIXE (particle-induced X-ray emission)-PIGE (particle-induced gamma-ray emission) compositional analysis in external beam mode are combined to study certain archaeological materials. We present a review of the combined application of these analytical methods in the study of casting cores of the Riace bronzes, 2 classical Greek statues of extraordinary importance for the history of art.

Nondestructive Ion Trap Mass Analysis at High Pressure

A method for performing nondestructive ion trap mass analysis at high pressures (>1 mTorr) has been developed using image current measurement with constant dipolar excitation. Instead of monitoring the ion secular motion, a harmonic of the ion motion was used for narrow band image current measurement followed by Fourier Transform. The capability of this technique has been demonstrated with mass analysis using a single measurement at pressures of 10 mTorr or higher. Methods for mixture analysis and tandem mass spectrometry have also been developed for nondestructive mass analysis.

THE EVOLUTION OF LUSTRE CERAMICS FROM MANISES (VALENCIA, SPAIN) BETWEEN THE 14TH AND 18TH CENTURIES

A set of 33 fragments of lustre-decorated ceramics uncovered during an archaeological excavation in Manises (Valencia, Spain) have been studied. These ceramics were produced in Manises from the 14th to the 18th century. This well-dated set of ceramic shards represents the diversity of Manises lustre production and is a complete time sequence of reference for the technological analysis. Texture analysis of the glazes has been carried out by SEM–EDAX, the inner and outer surfaces of the lustre decorations being analysed with non-destructive ion beams by PIXE and RBS, and also by high-resolution electron microscopy. The results are compared with other lustre productions and the time trend of the microstructures, glaze and lustre composition is analysed. It is concluded that Sn was used to opacify glazes until the beginning of the 17th century and that changes in the lustre microstructure occurred around ad 1500.

Effect of Heating Rate on the Fluorine Content in TiAl-alloy After Oxidation at 900°C

The high temperature oxidation resistance of TiAl-alloy was significantly enhanced by applying the halogen-effect using fluorine beam line implantation. Short-time oxidation at 900°C was carried out in order to study the effect of heating rate on the F-concentration profiles detected by non-destructive ion beam analyses. The composition of oxide scale depending on heating rate was also investigated.