The interdiffusion and solid-state reaction of low-energy copper ions implanted in silicon

At room temperature, single-crystal silicon was implanted with Cu⁺ ions at an energy of 80 keV using two doses of 5 × 10¹⁵ and 1 × 10¹⁷ Cu⁺ cm⁻². The samples were heat treated by conventional thermal annealing at different temperatures: 200 °C, 230 °C, 350 °C, 450 °C and 500 °C. The interdiffusion and solid-state reactions between the as-implanted samples and the as-annealed samples were investigated by means of Rutherford backscattering spectrometry (RBS) and X-ray diffraction (XRD). After annealing at 230 °C, the XRD results of the samples (subject to two different doses) showed formation of Cu₃Si. According to RBS, the interdiffusion between Cu and Si atoms after annealing was very insignificant. The reason may be that the formation of Cu₃Si after annealing at 230 °C suppressed further interdiffusion between Si and Cu atoms.     

Strain enhancement in Si induced by direct bonding of a LaAlO3 film to a Si substrate

The depth profiles of lattice strain near the interface regions of LaAlO₃/Si and the SiO₂ interfacial layer/Si were investigated by the ion channeling technique using high-resolution Rutherford backscattering spectroscopy (HRBS). In the case of the LaAlO₃/Si stack, horizontal tensile strain in the Si near the interface was clearly observed. However, this strain was relaxed by formation of the interfacial layer through annealing in an oxygen ambient. These results suggest that the strain in Si induced by a dielectric strongly depends on the material in contact with Si.     

Investigations on the effect of 100 MeV Ni ions irradiated chloride vapour phase epitaxy (Cl-VPE) grown GaN epilayers

Gallium nitride (GaN) epilayers have been grown by chloride vapour phase epitaxy (Cl-VPE) technique and the grown GaN layers were irradiated with 100 MeV Ni ions at the fluences of 5 × 10¹² and 2 × 10¹³ ions/cm². The pristine and 100 MeV Ni ions irradiated GaN samples were characterized using X-ray diffraction (XRD), UV-visible transmittance spectrum, photoluminescence (PL) and atomic force microscopy (AFM) analysis. XRD results indicate the presence of gallium oxide phases after Ni ion irradiation, increase in the FWHM and decrease in the intensity of the GaN (0 0 0 2) peak with increasing ion fluences. The UV-visible transmittance spectrum and PL measurements show decrease in the band gap value after irradiation. AFM images show the nanocluster formation upon irradiation and the roughness value of GaN increases with increasing ion fluences.     

Characterisation of an enamelled metallic object found in Guerrero Negro (Baja California) by PIXE and RBS techniques

The coast of Guerrero Negro (Baja California) has been known for a long time by archaeologists for its shipwrecks. Archaeologists are recovering objects that come from sunken Spanish galleons in the colonial period, and reach the American coast in the frontier of the USA with Mexico.An enamelled metallic object was found next to the beach in Guerrero Negro. We have analysed the piece with proton induced X-ray emission (PIXE) and Rutherford backscattering (RBS) in an attempt to establish whether the object could come from one of the colonial shipwrecks and to valuate its cleaning process.Scanning electron microscopy (SEM) and energy dispersive X-ray spectrometry (EDS) have been also performed in three samples taken from the object in order to observe the heterogeneity of the material.The materials found revealed the presence of typical lead-glass enamels from with pigments such as cuprite (red), or lead-tin yellow used in colonial times. The metallic part consisted of brass. As for the cleaning process, the average efficiency considered as the weight% of chlorine removed, was of 83.4% for brass and 100% for enamels.     

Optical and structural properties of ZnO thin films; effects of high energy electron irradiation and annealing

High energy electron irradiation (HEEI) effects on the as-grown and annealed ZnO thin films grown by electrochemical deposition were investigated. Both samples were exposed to the sequential electron irradiations of 6, 12 and 15 MeV energies at a fluence of 1 × 10¹² e⁻/cm². The results of X-ray diffraction suggest that a highly strong crystallographic structure can be produced by annealing process. Photoluminescence (PL) studies show that the EI produces violet emission which results from the zinc interstitial. Recombination lifetime (RL) values of the both films reveal that the high quality crystals are obtained. The decreasing trends of RL values with increasing electron energy have been explained by the formation of crystal defects due to the HEEI.     

Ion beam studies on reactive DC sputtered manganese doped indium tin oxide thin films

Indium based transparent conducting oxides doped with magnetic elements have been studied intensively in recent years with a view to develop novel ferromagnetic semiconductors for spin-based electronics. In the present work, we have grown manganese doped indium tin oxide (Mn:ITO) thin films, onto Si and Si/SiO₂ substrates by DC reactive sputtering of a composite target containing indium-tin alloy and manganese, in a gas mixture of oxygen and argon. Glancing angle X-ray diffraction (GXRD) studies reveal the polycrystalline nature of the films. Magnetic measurements carried out using vibrating sample magnetometer (VSM) suggest that the films are ferromagnetic at room temperature, with a saturation magnetization of ∼22.8 emu/cm³. The atomic percentages of In, Sn, Mn and O, as estimated using Rutherford backscattering spectrometry (RBS) are 37.0, 4.0, 1.6 and 57.4, respectively. RBS measurements reveal that the interface of the films with Si substrate has a ∼30 nm thick intermediate layer. This layer consists of oxygen, silicon, indium, tin and manganese, in the ratio 1:0.56:0.21:0.07:0.03, indicative of diffusion of elements across the interface. The films on Si/SiO₂, on the other hand, have a sharp interface.     

Elemental analysis of light constituents in thin plastic films

Experiments with 1-3 MeV ⁴He beams and 2.2-3.2 MeV proton beams have been performed in order to develop a precise and highly sensitive method for the detection and analysis of light elements in threat or drug materials using simultaneously the RBS and ERDA techniques. Commercially available plastic films have been used as samples. The 1 MeV ⁴He beam has been found to be inadequate owing to the rapid destruction of the targets. Best results have been obtained using proton beams with energies higher than 3 MeV. For 3.2 MeV proton beams, ERDA has been used for the analysis of the hydrogen constituent.     

Structural and magnetic properties of Tb implanted ZnO single crystals

ZnO single crystals have been implanted with Tb ions. For an atomic concentration of 1.5%, annealing at 823 K leads to an increase of the saturation magnetization per implanted Tb ion up to 1.8 μ_B at room temperature. Structural investigations revealed no secondary phase formation, but the out-diffusion of Tb. No significant evidence is found for Tb substituting Zn sites either in the as-implanted or annealed samples. However, indications for the existence of a small amount of Tb nanoclusters however have been found using magnetization versus temperature measurements. The ferromagnetic properties disappear completely upon annealing at 1023 K. This behavior is related to the formation of oxide complexes or nanoparticles.     

Development of a time-of-flight spectrometer at the Ruder Boškovi? Institute in Zagreb

A new TOF telescope has been constructed for thin film and surface analysis. The timing system consists of two electrostatic mirror type detectors of Busch design. The detection efficiency of timing stations for very light ions was significantly improved using DLC (diamond like carbon) foils coated with LiF instead of the conventionally used carbon foils. Ion energy is measured by a 300 mm² ULTRA ion-implanted silicon detector. For the ERDA measurements with heavy and energetic ion beams, a time-of-flight (TOF) spectrometer is positioned at 37.5°. Spectrometer can be easily moved to 120° backward angle for time-of-flight RBS analysis with low energy beam of light ions. Positioning and fine adjustments of sample orientation are performed with a motorized sample stage. The same spectrometer can be also installed at the ion microprobe scattering chamber for 3D elemental imaging.     

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.     

Depth profiling of carbon in silicon using the C(p, p′γ) reaction

An analytical method has been developed for the measurement of a carbon depth profile of the region a few tens of μm from the surface, using a ¹²C(p, p′γ) reaction. Measurements for a SiC sample coated with a silicon layer and a carbon-implanted silicon sample were performed using this method. Two charged particle detectors and two γ-ray detectors were utilized for the coincident detection of scattered protons and γ-rays from the first excited state (E_x = 4.4 MeV) of ¹²C. The measured depth profiles agree well with results obtained using a surface profiler and an Auger microprobe. These results demonstrate that this method is useful for the non-destructive analysis of carbon at depths of a few tens of μm from the surface.     

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.     

Structural characterization of Fe/Ag bilayers by RBS and AFM

Fe/Ag thin films are intensively investigated due to their special magnetic properties. Recently a deposition-order dependent asymmetric interface has been found. When iron is grown on silver, the interface is sharp, while the growth of Ag on Fe results in a long, low-energy tail of the Ag peak in the Rutherford backscattering spectrometry (RBS) spectra. The main purpose of this paper is to show that the low-energy Ag tail is caused by grain boundary diffusion, and that, when elevating the growing temperature of the Ag layer this effect becomes more significant. Two sets of polycrystalline and epitaxial Fe/Ag bilayers were prepared simultaneously onto Si(1 1 1) and MgO(1 0 0), respectively. The iron layers were grown at 250 °C and annealed at 450 °C in both sets, while the Ag layer was grown in the first set at room temperature (RT) and in the second set at 250 °C (HT). The sample composition, the interface sharpness and the quality of the epitaxy were studied by Rutherford backscattering spectrometry (RBS) combined with channeling effect. The surface morphology was determined by atomic force microscopy (AFM). RBS spectra show that in the case of RT samples the epitaxial MgO/Fe/Ag bilayer has sharp, well-defined interface, while for the polycrystalline Si/Fe/Ag sample the silver peak has a low-energy tail. Both the Fe and Ag peaks smeared out in the case of HT samples. AFM-images show that the RT samples have a continuous Ag layer, while the HT samples have fragmented surfaces. The RBS spectra taken on the HT samples were successfully simulated by the RBS-MAST code taking into account their fragmented structures.     

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.     

Tuning magnetic properties of Co/Pt thin films using energetic ions

In this paper, we present the changes occurring in Co/Pt bi- and multi-layer thin films modified under wide range of ion energy and species and fluence. We have shown the possibility of achieving controlled tuning of magnetic properties of the Co/Pt thin film system. Monte Carlo simulation results for ion-induced atomic displacements were used to explain the observed effects of ion-irradiation interface mixing across the Co/Pt interfaces. Phase formation has been explained in the light of heat of formation rule. On the other hand, we propose that ion induced point defect clustering governs the changes occurring in the structural and the magnetic properties.     

Production and preliminary characterization of DC plasma polymerized allylamine film (PPAA) by NRA, ERD and XPS

Due to its surface properties, especially the presence of amine groups, plasma polymerized allylamine (PPAA) is involved in a large range of applications. Most of them are related to biology and biochemistry. In this work, we demonstrate a quick and simple way to produce PPAA thin films by conventional DC magnetron sputtering. To the best of our knowledge, this is the first method not involving radiofrequency (RF) or microwave discharges. In this paper, we show preliminary characterizations on the produced films (bulk analysis) carried out by ion beam techniques. The Hydrogen content in the whole layers was measured by ERD. The surface composition was probed by XPS on pentafluorobenzaldehyde (PFBA) derivatized films: the maximum concentration of amine groups is 1.6%.     

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).     

MeV-ion beam analysis of the interface between filtered cathodic arc-deposited a-carbon and single crystalline silicon

Amorphous carbon (a-C) films were deposited on Si(1 0 0) wafers by a filtered cathodic vacuum arc (FCVA) plasma source. A negative electrical bias was applied to the silicon substrate in order to control the incident energy of carbon ions. Effects of the electrical bias on the a-C/Si interface characteristics were investigated by using standard Rutherford backscattering spectrometry (RBS) in the channeling mode with 2.1-MeV He²⁺ ions. The shape of the Si surface peaks of the RBS/channeling spectra reflects the degree of interface disorder due to atomic displacement from the bulk position of the Si crystal. Details of the analysis method developed are described. It was found that the width of the a-C/Si interface increases linearly with the substrate bias voltage but not the thickness of the a-C film.     

Analysis of C, N and O in aerosol collected on an organic backing using internal blank measurements and variable beam size

A method with low MDL (minimum detection limit) was developed for analysis of carbon (C), nitrogen (N) and oxygen (O) in aerosol samples collected on an organic backing. An accelerator-produced beam of protons interacting with the sample and the detection of elastically scattered protons (PESA; particle elastic scattering analysis) and emitted X-rays (PIXE; particle-induced X-ray emission) were the basic components of the setup. The method is based on measurement of internal blank concentrations, i.e. measurement of the blank concentration outside the aerosol deposit in each sample, and the use of two sizes of the beam in order to improve the MDL of the analysis. Large beam size covering the entire aerosol deposit was used to obtain quantitative analysis with PIXE. Small beam was used to obtain relative elemental concentrations with PESA and PIXE, which were transformed to absolute values by the aid of large-beam analysis. The small-size-beam served two purposes: to make internal blank measurements feasible and to improve the signal ratio of aerosol-deposit to backing. Compared with the traditional way of analysis, using a beam that is larger than the deposit and specially prepared blank samples, the new method reduced the MDL of C, N and O by a factor of 130, 70 and 90, respectively. The new method was applied to aerosol samples collected in the upper troposphere and the lowermost stratosphere from the CARIBIC platform. As far as the authors know, these measurements are the first quantitative determinations of C, N and O in the aerosol of this part of the atmosphere. The results show that these elements together with sulfur are major components of the aerosol.