Tiago F. Silva

MultiSIMNRA: A computational tool for self-consistent ion beam analysis using SIMNRA

Abstract SIMNRA is widely adopted by the scientific community of ion beam analysis for the simulation and interpretation of nuclear scattering techniques for material characterization. Taking advantage of its recognized reliability and quality of the simulations, we developed a computer program that uses multiple parallel sessions of SIMNRA to perform self-consistent analysis of data obtained by different ion beam techniques or in different experimental conditions of a given sample. In this paper, we present a result using MultiSIMNRA for a self-consistent multi-elemental analysis of a thin film produced by magnetron sputtering. The results demonstrate the potentialities of the self-consistent analysis and its feasibility using MultiSIMNRA.

First Experiments with the IFUSP Microtron Injector

The first accelerating structures of the Sao Paulo microtron accelerator presently deliver a continuous‐wave 1.9 MeV electron beam, which can be used in atomic physics studies. An energy‐analyzed beam line with focalization magnets, irradiation chamber, movable target system and Faraday cup was built. Here, we will describe the preliminary results of two experiments. In the first one, upper limits on K‐shell ionization cross sections of Pd and Au atoms by electron impact were obtained. To this end, thin targets of these elements were irradiated with the beam impinging at 45° while the emitted Kα x‐rays were recorded with an HPGe x‐ray detector positioned at 90° with respect to the beam direction. The other experiment was the measurement of the bremsstrahlung energy spectra produced by the aforementioned targets in the same geometrical configuration but using an HPGe γ‐ray detector instead. The latter experiment enabled the determination of the electron‐beam energy as 1.909(5) MeV.

In-air RBS measurements at the LAMFI external beam setup

This work describes new developments in the external beam setup of the Laboratory of Material Analysis with Ion Beams of the University of Sao Paulo (LAMFI-USP). This setup was designed to be a versatile analytical station to analyze a broad range of samples. In recent developments, we seek the external beam Rutherford Backscattering Spectroscopy (RBS) analysis to complement the Particle Induced X-ray Emission (PIXE) measurements. This work presents the initial results of the external beam RBS analysis as well as recent developments to improve the energy resolution RBS measurements, in particular tests to seek for sources of resolution degradation. These aspects are discussed and preliminary results of in-air RBS analysis of some test samples are presented.

Deciphering the preservation of fossil insects: a case study from the Crato Member, Early Cretaceous of Brazil

Exceptionally well-preserved three-dimensional insects with fine details and even labile tissues are ubiquitous in the Crato Member Konservat Lagerstätte (northeastern Brazil). Here we investigate the preservational pathways which yielded such specimens. We employed high resolution techniques (EDXRF, SR-SXS, SEM, EDS, micro Raman, and PIXE) to understand their fossilisation on mineralogical and geochemical grounds. Pseudomorphs of framboidal pyrite, the dominant fossil microfabric, display size variation when comparing cuticle with inner areas or soft tissues, which we interpret as the result of the balance between ion diffusion rates and nucleation rates of pyrite through the originally decaying carcasses. Furthermore, the mineral fabrics are associated with structures that can be the remains of extracellular polymeric substances (EPS). Geochemical data also point to a concentration of Fe, Zn, and Cu in the fossils in comparison to the embedding rock. Therefore, we consider that biofilms of sulphate reducing bacteria (SRB) had a central role in insect decay and mineralisation. Therefore, we shed light on exceptional preservation of fossils by pyritisation in a Cretaceous limestone lacustrine palaeoenvironment.

Large areas elemental mapping by ion beam analysis techniques

The external beam line of the Laboratory for Material Analysis with Ion Beams (LAMFI) is a versatile setup for multi-technique analysis. X-ray detectors for Particle Induced X-rays Emission (PIXE) measurements, a Gamma-ray detector for Particle Induced Gamma- ray Emission (PIGE), and a particle detector for scattering analysis, such as Rutherford Backscattering Spectrometry (RBS), were already installed. In this work, we present some results, using a large (60-cm range) XYZ computer controlled sample positioning system, completely developed and build in our laboratory. The XYZ stage was installed at the external beam line and its high spacial resolution (better than 5 μm over the full range) enables positioning the sample with high accuracy and high reproducibility. The combination of a sub-millimeter beam with the large range XYZ robotic stage is being used to produce elemental maps of large areas in samples like paintings, ceramics, stones, fossils, and all sort of samples. Due to its particular characteristics, this is a unique device in the sense of multi-technique analysis of large areas. With the continuous development of the external beam line at LAMFI, coupled to the robotic XYZ stage, it is becoming a robust and reliable option for regular analysis of trace elements (Z > 5) competing with the traditional in-vacuum ion-beam-analysis with the advantage of automatic rastering.

Preliminary measurements of the Bremsstrahlung doubly differential cross section for electrons between 20 and 100 keV in Au

Electron Bremsstrahlung cross sections were experimentally determined, for five kinetic energies, unfolding the measured photon spectra with an analytical detector response function.

Innovative Low Temperature Plasma Approach for Deposition of Alumina Films

Alumina films were deposited from a new plasma method using aluminum acetylacetonate (AAA) powder as precursor. The AAA was sputtered in argon and oxygen plasma mixtures. It was investigated the effect of the oxygen proportion (O2%) on the properties of the coatings. Deposition rate was derived from the layer height measured by profilometry. The elemental composition and molecular structure of the films were determined by Rutherford backscattering and infrared spectroscopies, respectively. Grazing incidence X-ray diffraction was used to investigate the microstructure of the films while hardness was determined by nanoindentation technique. Inspections on the surface morphology and on the film composition were conducted associating scanning electron microscopy and energy dispersive spectroscopy. Incorporation of oxygen affects the plasma kinetics and consequently the properties of the coatings. As moderated concentrations of oxygen ( 25%) are incorporated, the structure become rich in metallic aluminum with carbon rising at low proportions. The deposited layer is not homogeneous in thickness once the chemical composition of the precursor is changed by the action of the reactive oxygen plasma. Oxygen ablation on the film surface also contributes to the lack of homogeneity of the structure, especially as high oxygen proportions are imposed. Hardness data (0.5-2.0 GPa) corroborated the idea of an amorphous structure. Based on the results presented here it was possible to identify the oxygen concentration in the plasma atmosphere which mostly removed organics while preserving the stoichiometric alumina precipitation, subject of great relevance as one considers the reduction in the energy necessary for the creation of fully oxide coatings.

Calcination does not remove all carbon from colloidal nanocrystal assemblies

Removing organics from hybrid nanostructures is a crucial step in many bottom-up materials fabrication approaches. It is usually assumed that calcination is an effective solution to this problem, especially for thin films. This assumption has led to its application in thousands of papers. We here show that this general assumption is incorrect by using a relevant and highly controlled model system consisting of thin films of ligand-capped ZrO2 nanocrystals. After calcination at 800 °C for 12 h, while Raman spectroscopy fails to detect the ligands after calcination, elastic backscattering spectrometry characterization demonstrates that ~18% of the original carbon atoms are still present in the film. By comparison plasma processing successfully removes the ligands. Our growth kinetic analysis shows that the calcined materials have significantly different interfacial properties than the plasma-processed counterparts. Calcination is not a reliable strategy for the production of single-phase all-inorganic materials from colloidal nanoparticles.Synthesis of all-inorganic nanomaterials often relies on organic templates, which are assumed to then be fully removed by calcination. Here, the authors use elastic backscattering spectroscopy to challenge this assumption, finding that calcination leaves behind considerable carbon content that can severely affect material function.

Study of boron detection limit using the in-air PIGE set-up at LAMFI-USP

The quantification of small amounts of boron in materials is of extreme importance in different areas of materials science. Boron is an important contaminant and also a silicon dopant in the semiconductor industry. Boron is also extensively used in nuclear power plants, either for neutron shielding or for safety control and boron is an essential nutrient for life, either vegetable or animal. The production of silicon solar cells, by refining metallurgical-grade silicon (MG-Si) requires the control and reduction of several silicon contaminants to very low concentration levels. Boron is one of the contaminants of solar-grade silicon (SG-Si) that must be controlled and quantified at sub-ppm levels. In the metallurgical purification, boron quantification is usually made by Inductive Coupled Plasma Mass Spectrometry, (ICP-MS) but the results need to be verified by an independent analytical method. In this work we present the results of the analysis of silicon samples by Particle Induced Gamma-Ray Emission (PIG...

Automatic energy calibration algorithm for an RBS setup

This work describes a computer algorithm for automatic extraction of the energy calibration parameters from a Rutherford Back-Scattering Spectroscopy (RBS) spectrum. Parameters like the electronic gain, electronic offset and detection resolution (FWHM) of a RBS setup are usually determined using a standard sample. In our case, the standard sample comprises of a multi-elemental thin film made of a mixture of Ti-Al-Ta that is analyzed at the beginning of each run at defined beam energy. A computer program has been developed to extract automatically the calibration parameters from the spectrum of the standard sample. The code evaluates the first derivative of the energy spectrum, locates the trailing edges of the Al, Ti and Ta peaks and fits a first order polynomial for the energy-channel relation. The detection resolution is determined fitting the convolution of a pre-calculated theoretical spectrum. To test the code, data of two years have been analyzed and the results compared with the manual calculations done previously, obtaining good agreement.