Compositional analysis of atom beam co-sputtered metal-silica nanocomposites by Rutherford backscattering spectrometry

Metal:SiO₂ (metal: Ni, Ag, Au) nanocomposite films of different compositions have been prepared by atom beam co-sputtering. The estimation of composition of films is done theoretically using sputtering yield and relative area of metal and SiO₂. The sputtering yields used for estimation of composition are calculated by three theoretical methods: Monte Carlo simulations (SRIM code), Sigmund’s theory and Sigmund’s theory modified by Anderson and Bay. Rutherford backscattering spectrometry (RBS) is also used to analyze the composition of the nanocomposite films. RUMP simulations of RBS data are performed. The errors in theoretical calculations and RBS results are estimated. It is found that SRIM is more appropriate for Ni:SiO₂ nanocomposite films, while modified Sigmund’s theory based method is better for Ag:SiO₂ and Au:SiO₂ nanocomposite films. The possible sources of errors in theoretical methods with respect to experimental (RBS) results are also discussed.     

Pulsed extraction of ionization from helium buffer gas

The migration of intense ionization created in helium buffer gas under the influence of applied electric fields is considered. First the chemical evolution of the ionization created by fast heavy-ion beams is described. Straight forward estimates of the lifetimes for charge exchange indicate a clear suppression of charge exchange during ion migration in low pressure helium. Then self-consistent calculations of the migration of the ions in the electric field of a gas-filled cell at the National Superconducting Cyclotron Laboratory (NSCL) using a particle-in-cell computer code are presented. The results of the calculations are compared to measurements of the extracted ion current caused by beam pulses injected into the NSCL gas cell.     

Charge exchange of medium energy H and He ions emerging from solid surfaces

Charge exchange of medium energy H and He ions emerging from clean solid surfaces is studied extensively using a toroidal electrostatic analyzer with an excellent energy resolution. The charge distributions of He ions scattered from sub-monolayers near a surface are non-equilibrated, resulting in a surface peak even for poly-crystal solids. By solving simultaneous rate equations numerically, we derive electron capture and loss cross sections for Ni and Au surfaces. Based on a free electron gas model, non-equilibrated He⁺ fractions dependent on emerging angle reveals uniform electronic surfaces for metals and corrugated surfaces for Si and graphite with covalent bonds. It is also found that equilibrium charge fractions of H⁺ are independent of surface materials (Z₂) and in contrast equilibrium He⁺ fractions depend pronouncedly on Z₂. The data obtained are compared with semi-empirical formulas.     

Production and characterization of thin Li targets fabricated by ion implantation

Very high fluence implantation of ⁷Li⁺ ions was used to promote the formation of a thin and high density ⁷Li target in the surface region of Al samples. The implanted volume was characterized by particle induced gamma-ray emission, Rutherford backscattering spectrometry, X-ray photoelectron spectroscopy and nuclear reaction analysis, revealing that the implanted surface is a combination of Li₂CO₃, metallic lithium, LiOH and C, with almost no Al present. Radiation damage effects by proton beams were studied by observing the evolution of the ⁷Li(p, α)⁴He nuclear reaction yield with the accumulated charge, at different proton energies, revealing high stability of the produced Li target.     

Applications of a compact ionization chamber in AMS at energies below 1 MeV/amu

The increasing demand for measuring long-lived radionuclides with small AMS machines at energies below 1 MeV per nucleon raises the need for compact detectors which still have a decent energy resolution and allow for a clear identification of the incident particles. Based on a design by the AMS group at the ETH Zurich a compact gas ionization chamber was built and installed at the 3 MV tandem AMS facility VERA (Vienna Environmental Research Accelerator). The main challenge in AMS is the detection of rare isotope species in the presence of strong isotopic and isobaric interferences. The task of the ionization chamber is the suppression of the unwanted isobar by separating the ions via their different stopping powers. Measurements of ³⁶Cl at VERA showed an achieved suppression of the unwanted stable isobar ³⁶S of 3 × 10⁻⁴ and measurements of ¹⁰Be showed an achieved suppression of ¹⁰B of at least 3 × 10⁻⁶. Additional suppression of the isobaric ions can be achieved by a degrader foil technique applied to ¹⁰Be measurements by G.M. Raisbeck. In combination with the new ionization chamber the achieved suppression of ¹⁰B is at least 10⁻¹⁰. Measurements of blank samples at VERA show that the background for AMS with ¹⁰Be is below 2 × 10⁻¹⁵.     

The new Cyclone 18/9 beam transport line at the CNA (Sevilla) for high energy PIXE applications

The Cyclone 18/9 cyclotron system at the Centro Nacional de Aceleradores (Sevilla, Spain) is commonly used to create short life radioisotopes for PET applications. Besides, an external beam transport line has been recently installed in one of the target ports with two major purposes: to study the effects of 18 MeV protons irradiation on the behaviour of electronic devices for space applications and to complement the analysis of materials using our 3 MV tandem accelerator with the PIXE measurements at high energy.In this work, the main elements of our beamline will be briefly described and the first PIXE application will be presented. The usual PIXE, in the analysis of archaeological metallic objects, using around 3 MeV protons requires having a shiny area. Our purpose is to obtain a deeper determination of the bulk composition bombarding with 18 MeV protons through the corroded samples surfaces, without polishing the ancient object. To check this methodology high energy PIXE has been performed on two fibulae of the Later Bronze Age and First Iron Age, coming from the area around Sevilla.     

Modification of the etching properties of x-cut Lithium Niobate by ion implantation

In this work x-cut Lithium Niobate crystals were implanted with 0.5 MeV O ions (nuclear stopping regime), 5 MeV O ions (sub-threshold electronic stopping regime) and 12.5 MeV Ti ions (ion track regime) at the fluences required for the formation of a surface fully disordered layer. The damage depth profiles were determined by RBS-channeling. Wet etching was performed at room temperature in 50% HF:H₂O solution. The data indicated an exponential dependence of the etching rate on the damage concentration. Independently of the damage regime, once random level in the RBS-channeling spectra was attained we measured the same etching rate (50-100 nm/s) and the same volume expansion (∼10%) in all samples. These results indicate that the fully disordered layers obtained by electronic damage accumulation have the same chemical properties of those obtained by conventional nuclear damage accumulation and therefore they can be defined “amorphous”. The impressive etching selectivity of ion implanted regions makes this process suitable for sub-micro machining of Lithium Niobate.     

A Time of Flight-Energy spectrometer for stopping power measurements in Heavy Ion-ERD analysis at iThemba LABS

The quantitative analysis of thin layers using Heavy Ion-Elastic Recoil Detection (HI-ERD) can be reliably performed if the stopping powers of the probing ions and recoils in a given target matrix are known accurately. Unfortunately for many projectile/target combinations experimental data is limited and where available, deviations of up to 50% between experiment and theory have been reported. This presentation describes the assembly of a Time of Flight-Energy (ToF-E) detector system developed for HI-ERD analysis and adapted for stopping power measurements at iThemba LABS. First results from energy loss measurements of 0.1-0.5 MeV/nucleon ²⁸Si and ⁸⁴Kr ions in ZrO₂ are presented and compared with predictions of the widely used SRIM2003 (Stopping Range of Ions in Matter).     

International Atomic Energy Agency intercomparison of ion beam analysis software

Ion beam analysis (IBA) includes a group of techniques for the determination of elemental concentration depth profiles of thin film materials. Often the final results rely on simulations, fits and calculations, made by dedicated codes written for specific techniques. Here we evaluate numerical codes dedicated to the analysis of Rutherford backscattering spectrometry, non-Rutherford elastic backscattering spectrometry, elastic recoil detection analysis and non-resonant nuclear reaction analysis data. Several software packages have been presented and made available to the community. New codes regularly appear, and old codes continue to be used and occasionally updated and expanded. However, those codes have to date not been validated, or even compared to each other. Consequently, IBA practitioners use codes whose validity, correctness and accuracy have never been validated beyond the authors’ efforts. In this work, we present the results of an IBA software intercomparison exercise, where seven different packages participated. These were DEPTH, GISA, DataFurnace (NDF), RBX, RUMP, SIMNRA (all analytical codes) and MCERD (a Monte Carlo code). In a first step, a series of simulations were defined, testing different capabilities of the codes, for fixed conditions. In a second step, a set of real experimental data were analysed. The main conclusion is that the codes perform well within the limits of their design, and that the largest differences in the results obtained are due to differences in the fundamental databases used (stopping power and scattering cross section). In particular, spectra can be calculated including Rutherford cross sections with screening, energy resolution convolutions including energy straggling, and pileup effects, with agreement between the codes available at the 0.1% level. This same agreement is also available for the non-RBS techniques. This agreement is not limited to calculation of spectra from particular structures with predetermined parameters, but also extends to extracting information from real data. In particular, we have shown data from an Sb implanted sample where the Sb fluence was certified with an uncertainty of 0.6%. For this sample, and using SRIM03 stopping powers for 1.5 MeV ⁴He in Si, the codes were able to extract the Sb fluence with an average 0.18% deviation from the certified value and a 0.11% agreement between the codes. Thus IBA is a suitable technique for accurate analysis where traceability is critical. These results confirm that available IBA software packages are, within their design limitations, consistent and reliable. The protocol established may be readily applied to validate future IBA software as well.     

Modification of poly(ether ether ketone) by ion irradiation

Poly(ether ether ketone) was irradiated with 3.0 MeV Si²⁺, 3.25 MeV Cu²⁺ and 4.8 MeV Ag²⁺ ions to the fluences from 10¹² to 10¹⁴ cm⁻² and the effects of irradiation were studied using ERDA, RBS and FTIR methods. The irradiation leads to release of hydrogen from the PEEK surface layer modified by the ion beam. The release is mild for low ion fluences but it becomes more pronounced at the ion fluences above 10¹³ cm⁻². At highest ion fluences the hydrogen concentration falls to 20-35% of its initial value. In contrast to hydrogen no significant oxygen release was observed. The kinetic of the hydrogen release is similar for the three ion species. FTIR measurement shows deep structural changes of the polymer structure resulting from the ion irradiation.     

Calibration factors for the SNOOPY - NP-100 neutron dosimeter

Within CANDU nuclear power facilities, only a small fraction of workers are exposed to neutron radiation. For these individuals, roughly 4.5% of the total radiation equivalent dose is the result of exposure to neutrons. When this figure is considered across all workers receiving external exposure of any kind, only 0.25% of the total radiation equivalent dose is the result of exposure to neutrons. At many facilities, the NP-100 neutron dosimeter, manufactured by Canberra Industries Incorporated, is employed in both direct and indirect dosimetry methods. Also known as “SNOOPY”, these detectors undergo calibration, which results in a calibration factor relating the neutron count rate to the ambient dose equivalent rate, using a standard Am-Be neutron source. Using measurements presented in a technical note, readings from the dosimeter for six different neutron fields in six source-detector orientations were used, to determine a calibration factor for each of these sources. The calibration factor depends on the neutron energy spectrum and the radiation weighting factor to link neutron fluence to equivalent dose. Although the neutron energy spectra measured in the CANDU workplace are quite different than that of the Am-Be calibration source, the calibration factor remains constant - within acceptable limits - regardless of the neutron source used in the calibration; for the specified calibration orientation and current radiation weighting factors. However, changing the value of the radiation weighting factors would result in changes to the calibration factor. In the event of changes to the radiation weighting factors, it will be necessary to assess whether a change to the calibration process or resulting calibration factor is warranted.     

A method for very low fluence implantations using Rutherford scattering

A simple method for extremely low fluence ion implantation is described. It is based on implanting ions which are Rutherford backscattered (RBS) from a thin gold layer into the desired target. This method enables ion implantations to be carried out, as are needed to realize quantum centers on the atomic scale to serve as qubits and other nano sized devices. The required implantation fluences are orders of magnitude below the commonly-used current integration capabilities; hence control on the implanted fluence is usually complicated. The described method enables control on the implanted fluence even when extremely low. The dependence of the energy and fluence of scattered ions on the angle and scattering target thickness is analyzed by using SRIM simulations. These are verified for the case of N scattering implantation by direct counting in a surface barrier detector and for the case of Xe by counting the tracks that scattered and implanted Xe ions leaved in HOPG as viewed by scanning probe microscopy.     

Improved energy resolution of a cyclotron beam for RBS measurements

For RBS (Rutherford Back Scattering) analysis, the quality of the beam is of premium importance because the depth profile resolution of the method is strongly dependent on the energy resolution of the probing beam. A magnetic analyzer, consisting of two 90 left-right bending magnets forming an achromatic doublet has been adapted to the Liege 20 MeV (proton) AVF (Azimuthal Varying Field) cyclotron. The energy resolution of that system has been measured by recording the resonance width of a ³²S(p,p′γ)³²S (3.38 MeV. p⁺ lab. energy). We have obtained a value of ΔE = ± 2 keV, reducing by a factor of 20 the natural dispersion of our cyclotron.We describe our magnetic analyzer system and present the results of our RBS measurements at energies up to 14 MeV α.     

Sol-gel silica coatings for the protection of cultural heritage glass

To slow down the phenomenon of weathering of ancient stained glass, the present work proposes the coating of glass. Several recipes have been tested in the past. The coatings are made of sol-gel silica prepared with different catalysts like H⁺, Pb(II), Sn(IV) and without catalyst. All the investigated samples show a good adhesion of the coating to the glasses used to simulate the behaviour of ancient artefacts and a good resistance to ageing tests.In the present work, some tests on Au and Ti surfaces coated with sol-gel silica were done, in order to investigate the adhesion of a H⁺ sol-gel coating to the surface of metals. In fact, in the case of glassy mosaics called “golden leaf tessera”, the adhesion of the glass to the metal is a critical point, due to the fact that the weathering of such tesserae causes the detaching of the “cartellina” (small glass layer) from the metal leaf. The main techniques adopted to investigate are optical microscopy (OM), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and Rutherford backscattering spectroscopy (RBS).     

Development of a novel reaction chamber for ion beam analysis of large samples

A novel vacuum chamber for ion beam analysis of large-size industrial samples - whose analysis are not feasible in conventional ion beam analysis reaction chambers - has been designed, fabricated and successfully tested. Using the newly developed chamber, both PIXE and RBS analyses could be carried out at the same time and on the same point of the samples. Ion beam analysis using this novel chamber lacks the disadvantages of external beam analysis and benefits the advantages of in-vacuum analysis. This has been achieved by designing a tiny open port in the wall of the reaction chamber to be sealed with a small flat area of sample body where its analysis is of interest. As a case study, two samples of gas turbine blades, a corroded one at highly corrosive environment and a refurbished one after application of certain coatings are analysed using the novel chamber. Experimental results confirm the performance and capability of the reaction chamber.     

Silver surface enrichment controlled by simultaneous RBS for reliable PIXE analysis of ancient coins

Evidence of silver surface enrichment of ancient silver-copper coins has been pointed out in the past years. Surface enrichment can be fortuitous or intentional. In this paper, we have investigated the cleaning procedures usually performed after excavation or in museums. We have shown that chemicals or commercial products routinely used dissolve preferentially the copper phase and consequently contribute to the silver surface enrichment. As a result, surface analyses such as PIXE or XRF can be strongly affected by this effect. By using simultaneously RBS and PIXE, it is possible to check through the silver surface enrichment and then select the reliable measurements, characteristic of the bulk composition. Results on coins recently discovered and mechanically or chemically cleaned are presented.     

Measurement of nitrogen depth profile in steel

The characterization of nitridated steel samples, in special the depth profile of nitrogen, aims to help improving the quality of the surface and to increase the durability of the steel pieces. In this work we used ERDA and NRA to determinate the profile of nitrogen in different sets of stainless steel samples. An incident beam of ³⁵Cl of 56 MeV was used for ERDA analysis of a first set of samples. Results indicated an homogeneous distribution for most of the identified elements, with atomic nitrogen concentrations around 2% in the analyzed depth range (0.2 μm) and the presence of thin films on the surface (about 50 × 10¹⁵ at/cm²), one of C and the other of iron oxide. In a second set of samples, 4.43 MeV gamma rays produced from ¹⁵N(H,αγ)¹²C reaction, using an external proton beam of 1.3 MeV, were used to quantify nitrogen concentration. N concentrations of about 0.47% were obtained comparing the gamma production rate of the samples with a referenced material (Stainless steel CRM298 - 0.236% of N in mass) irradiated in the same conditions. Also PIXE analyses were done on both sets of samples in order to identify main elements in the matrix.     

RBS analysis of InGaN/GaN quantum wells for hybrid structures with efficient Förster coupling

There is strong current interest in Förster resonant energy transfer (FRET) from a semiconductor quantum well (QW) to an overlayer of another luminescent material. The FRET process becomes efficient when the two materials are placed at interaction distance of a few nanometres. The additional requirement of large spectral overlap between the energy donor and acceptor can be satisfied by combinations of InGaN/GaN QWs (as donors) and overlayers of either light-emitting polymers or nanocrystalline semiconductor quantum dots (as acceptors), both of which can be tailored to have high absorption in the QW emission region. Here we study a set of custom grown InGaN/GaN single QW samples, in which the GaN cap layer thickness was varied to modulate the FRET rate in hybrid structures. We used high-resolution grazing angle RBS experiments to determine the GaN cap layer thickness, varied from 2 to 12 nm, which controlled the interaction distance between the QW and the coupled luminescent medium in hybrid structures. The very careful experiments and data analysis are discussed in detail, including a consideration of the errors in the final results obtained. An example of the use of the measured thickness values to confirm the dominance of sheet-to-sheet dipole-dipole interactions in QW-polymer hybrid structures is discussed.