The LNLS Users Committee – LNLSUC– is organising a series of live online seminars on the latest LNLS scientists research.

In the frame of LNLS Users Group Seminar series, monthly online lectures will be held, in which examples of recent results of experiments carried out at the LNLS and what science Sirius will enable. Join us and learn about the techniques scientists use to run their experiments, discuss the impact that these developments could have on the scientific community, then there will be the opportunity to ask our scientists any questions you may have via the Zoom ‘Q & A’ option.

LNLS Users Group Seminar series typically will be held on the last Tuesday of the month from 4:00-4:40 pm BRT with a Q&A session from 4:40-5:00 pm BRT. The upcoming Zoom presentations, with abstracts and links are available below.

María Fernanda Mera

On behalf of LNLSUC


Speaker: Hélio C. N. Tolentino – Head of the Heterogeneous and Hierarchical Matter Division of LNLS



Abstract: The X-ray nanoprobe beamline CARNAÚBA [1-4] at Sirius/LNLS has been operating for technical commissioning since November 2020 and for scientific commissioning since October 2021. The beamline design is for high-resolution multi-analytical and coherent X-ray imaging techniques over the energy domain of 2.05 to 15 keV. An all-achromatic mirror-based optics provides the nano-focused beam [5]. The beamline can operate in pink (high flux) or monochromatic (high energy resolution) mode. A 4-bounce Si(111) crystal monochromator (4CM) [6] provides the latter mode, with a resolving power of 10000 over the entire energy range. The first nanoprobe station, named TARUMÃ, provides a diversity of sample environments for in situoperando, cryogenic, and in vivo experiments for research areas in chemistry, physics, geophysics, biology, agriculture, environment, and energy, to name a few. The sample (or sample environment) is raster-scanned through the nanoprobe to generate fast two-dimensional maps of simultaneous contrasts, which can then be combined with a rotation for computed tomography. The second nanoprobe station, which is under UHV and cryogenic, is under construction.

On behalf of the LNLS team, I will present in this lecture a few aspects of technical commissioning and the first relevant scientific cases studied. The current beamline performance is getting to the main specifications, with the predicted photon flux and a focus size close to 160×140 nm2, measured in fluorescence and transmission modes. Using X-ray ptychography, both with pink and monochromatic beam, improves the resolution down to 20 nm, as demonstrated by preliminary analysis. As far as the first experiments are concerned, I will show results in agriculture, geophysics, solar energy, along with innovative instrumentation solutions for sample environments.

[1] Tolentino, H. C. N., et al., “CARNAÚBA: The Coherent X-Ray Nanoprobe Beamline for the Brazilian Synchrotron SIRIUS/LNLS”, Journal of Physics: Conf. Series 849 (2017) 012057.

[2] Tolentino, H. C. N., et al., “TARUMÃ station for the CARNAÚBA beamline at SIRIUS/LNLS.” X-Ray Nanoimaging: Instruments and Methods IV. Vol. 11112. International Society for Optics and Photonics, 2019.

[3] Geraldes, R. R., et al., “Design and Commissioning of the TARUMÃ Station at the CARNAÚBA Beamline at SIRIUS/LNLS”, Proc. MEDSI 2020, 2021.

[4] Tolentino, H. C. N., et al., “X-ray microscopy developments at Sirius-LNLS: first commissioning experiments at the Carnauba beamline.” X-Ray Nanoimaging: Instruments and Methods V. Vol. 11839. International Society for Optics and Photonics, 2021.

[5] Moreno, G. B. Z. L., et al., “Exactly-constrained KB Mirrors for Sirius/LNLS Beamlines: Design and Commissioning of the TARUMÃ Station Nanofocusing Optics at CARNAÚBA Beamline”, Proc. MEDSI 2020, 2021.

[6] Saveri Silva, M., et al., “Four-Bounce Crystal Monochromators for the Sirius/LNLS Beamlines”, in Proc. MEDSI 2020, 2021.

Speaker: Luis Carlos Colocho Hurtarte – Post-doc Beamline ID21 European Synchrotron Radiation Facility (ESRF)


Title: Synchrotron based microspectroscopy for the investigation of Carbon and Nutrient cycling in soils

Abstract: The cycling of nutrients and soil organic matter (SOM) is closely intertwined, and it is expected that changes in SOM turnover in terrestrial ecosystems as consequence of climate warming and global change are also changing the nutrient dynamics. These shifts in biogeochemical C and nutrient cycling have an important societal and economic impact on our day to day lives. An important factor to consider in biogeochemical cycling is that, most of the nutrients present in soils have organic forms associated with different SOM fractions. However, due to the lack of appropriate techniques to resolve their speciation and microspatial distribution, much of the information regarding their cycling is still unknown. Synchrotron-based techniques can aid in the understanding of the cycling of these elements, through both analyses at the macro and the microscale. Thus, my presentation aims to build the knowledge and generate discussion around the novel applications of synchrotron based techniques on soil science, and show case successful scientific cases of my own research where its combination with other techniques have yielded novel insights into SOM and nutrient cycling. Regarding the beamline ID21 is worldwide renown for X-ray micro-spectroscopy in the tender X-ray domain. It offers unique capabilities for 2D micro X-ray fluorescence mapping (µXRF, for element identification and localization) and micro X-ray absorption spectroscopy (µXAS, for speciation analysis), in the 2 – 11 keV range. This energy range allows exciting the K-edge of elements such as P, S, Cl as well as 3d transition metals. In addition, the presence and speciation of heavier metals of interest such as Pd, Ag, Sn, Cd, etc. can be probed via their L-lines. This, together with the cryo-stage option make ID21 a perfect beamline for micron scale studies of the interactions between inorganic materials and organic systems (cells, tissues, organisms, plants). Thanks to the new Extremely Brilliant Source (EBS) source and beamline refurbishment, the instrument’s performance will be further boosted offering the possibility to track changes at even lower concentrations, at higher resolution but preserving the field of view. Furthermore, it will allow us to combine the capabilities of 2D µXRF maps with single point µXAS analyses into hyperspectral imaging. Showcase studies will include, (i) the development of new approaches for bulk soil speciation of phosphorus (P), (ii) the application of correlative (cryo) microspectroscopy and nanoSIMS imaging, (iii) the use of microspectroscopy to investigate soil organic C microenvironments. In the first case, I will develop onto the use of conventional XANES spectroscopy for P research, and how alternative approaches can complement and aid in the identification of different forms of P. The second case study focuses on the combination of nano-scale Secondary Ion Mass Spectrometry (nanoSIMS) with synchrotron based µ-XRF and µ-XANES on german rock-soil interfaces and on Amazonian soils to investigate C and P cycling. The third case study will highlight new possibilities combining synchrotron-based techniques applied to soil organic C cycling. As concluding remarks, I will highlight the shortcomings of each presented technique and future possibilities using the EBS.

Speaker: Harry Westfahl Jr., LNLS’ Director


Title: The Present and Future of the LNLS User Program on Sirius

Abstract: With the beginning of the scientific commissioning in the first Sirius beamlines, the community of users of the new Brazilian synchrotron light source has had access to unprecedented experimental methods in the country, resulting in an already expressive scientific production for the current phase of the project. Furthermore, as we progress with the technical commissioning of new instruments for the beamlines in operation and the installation of the phase 1 beamlines, we will be able to reestablish the LNLS user program to pre-UVX shutdown levels. More recently, the budget required to complete phase 1 of Sirius was approved by FNDCT (National Fund for Scientific and Technological Development), bringing significant perspectives for the near-term future of the project. By receiving the financial transfers on time for the execution of the project according to our schedule, we envision reaching 2024 operating 14 light beamlines, the associated support laboratories and infrastructure for data processing, and a storage ring working within the design parameters with 350 mA. This seminar will present highlights of the new results from Sirius, the current status of the project, and the short and mid-term plans for our new synchrotron light source.

Harry Westfahl Jr. is the LNLS’ Director since 2020. He also served LNLS as Scientific Director from 2013 to 2019, as deputy scientific director from 2011 to 2012 and, as a researcher since 2001, when he joined the Laboratory after three years of postdoctoral research. Since 2013 he coordinates the project and construction of the beamlines for the new Brazilian synchrotron light source, Sirius. Its main research interests are in the physics of condensed matter systems, in the use of synchrotron radiation for the study of materials, mainly polymers and magnetic materials, and in the development of synchrotron radiation instrumentation.

Speaker: Silvia Russi, beamline scientist at the Stanford Synchrotron Radiation Lightsource (SSRL) at SLAC National Accelerator Laboratory


Title: Hybrid Methods and Multi-Techniques at SLAC National Accelerator Laboratory

Abstract: Synchrotrons have evolved from cyclic particle accelerators splitting matter into modern powerhouses to study fundamental natural, physical, technological, and environmental processes. The SLAC National Accelerator Laboratory operated by Stanford University for the US Department of Energy hosting the Stanford Synchrotron Radiation Lightsource (SSRL), the Linac Coherent Light Source (LCLS), and the Stanford-SLAC Cryo-EM Center (S2C2), embodies the entrepreneurial and high technology essence of Silicon Valley. At SSRL, twelve different beamlines are dedicated to macromolecular crystallography, small-angle X-ray scattering, X-ray absorption spectroscopy, and X-ray fluorescence to study protein structure, protein folding, electronic and geometric phenomena, conformational changes and structure/function relationships. The LCLS X-ray free electron laser (XFEL) delivering bursts of photons at the angstrom wavelength for the femtosecond time duration allows to resolve structure and dynamics on the atomic scale. The S2C2 provides access to state-of-the-art instrumentation for specimen vitrification and cryo-EM data collection towards atomic resolution structure determination. Combining expertise across SLAC directorates is custom. The SSRL Structural Macromolecular Biology Group (SMB) and S2C2 scientists implemented combined user administration software and scheduling and developed experimental methods for time-resolved studies and micro-electron diffraction. SSRL’s 12-1 beamline and LCLS’s MFX instrument share equipment and control software (Blu-Ice) and data processing and analysis routines. Further, the new SSRL undulator microfocus 12-1 began operation in May 2020 to develop efficient fixed-target serial femtosecond diffraction experiments at MFX while methods originally developed for MFX endow SSRL new capabilities for ambient temperature and serial data collection. Through fully remote access via SSRL’s Blu-Ice software the researcher runs experiments at cryogenic and elevated temperatures under controlled humidity conditions. SSRL’s SMB team introduced a portable in-situ crystallization plate and a thermal shipping container for at room and elevated temperature experiments at X-ray diffraction and UV-Visible absorption spectroscopy studies. Combining expertise and technologies across-the-boundaries is vital for the challenging and ever more complex needs from academic, non-profit, and industry scientists pushing the frontiers in numerous scientific fields such as physics, chemistry, materials and life sciences.

Dr. Silvia Russi is a beamline scientist at the Stanford Synchrotron Radiation Lightsource (SSRL) at SLAC National Accelerator Laboratory. Earlier in her career, Dr. Russi worked on the X-ray structure determination of bioactive organometallic compounds and inorganic complexes at the Laboratorio de Cristalografia, School of Chemistry, Universidad de la República, in her home country Uruguay. She moved then to the Structural Biology Group at the IBMB in Barcelona, Spain, to work on the structural characterization of bacterial proteins mediating the transfer of genetic material and spread of antibiotic resistance. After earning her PhD, she first joined the Diffraction Instrumentation Team at the EMBL-Grenoble Outstation, France, to conduct research on a new device for controlled crystal dehydration and then she moved to the Structural Biology Group at the ESRF where she studied new phasing strategies that exploited the anisotropy of the anomalous signal. In May 2013, she joined the SSRL, SLAC National Accelerator Laboratory, as Beamline Scientist. She provides scientific and technical support to visiting scholars and users of the macromolecular crystallography beamlines and perform research developing new experimental methods and instrumentation to accelerate protein crystallography experiments such as with the current Stanford Auto-Mounter (SAM) crystal-mounting robot and to implement fully automated, remotely-accessible, room temperature X-ray diffraction experiments.

Speaker: Cristiane B. Rodella (Paineira Group Leader)


Title: PAINEIRA beamline – Powder X-ray Diffraction beamline at Sirius

Abstract: Paineira beamline will be dedicated to X-ray diffraction experiments of polycrystalline materials (PXRD). It has been designed as a state-of-the-art PXRD beamline combining the benefits of brilliance and low emittance of a fourth-generation synchrotron source with sensitive, high-resolution, and fast detectors for high-quality data collection. Moreover, it will improve the trend of working in high-throughput mode at the synchrotron facility enabling efficient use of beamtime as well as reducing operational costs to provide easy access to the user. Measurements can be performed in high-resolution mode (0.008o FWHM at 15 keV) and/or fast detection (≈1s; 0.05o FWHM at 15 keV). The design optimizes the beamtime via high-throughput operation mode, using an automated system with a magazine of samples, a sample management system, and two robotic cells. Additionally, the sample holders developed will enable measurements in powder form using capillaries or self-supported samples (pellets, films) with variable temperatures during data acquisition (80K to 1273K). Furthermore, Paineira will allow PXRD experiments under in-situ and operando conditions at pressures up to 95 bar using a plug-flow capillary reactor and an automated module to control the gas flow and pressure during measurements.

Speaker: Dean Hesterberg, Soil Science Advisor and Researcher (LNLS-CNPEM)


Title: Multimodal Analyses at Sirius to Improve Soil Phosphorus Management

Abstract: Soils are fundamental to life as a natural resource for producing food and fiber, in addition to protecting water quality and mitigating climate change. More precise micro- to molecular-scale knowledge about the hierarchical assemblages of minerals and non-crystalline inorganic solids, biological residues, organic matter, living organisms, and pore networks that soils comprise is essential for more precise management of agricultural and environmental systems. This seminar will present ongoing research at LNLS and CNPEM that aims to increase the efficiency of plant acquisition of phosphorus. Phosphorus binding into slowly reversible forms, often termed “fixation”, is particularly problematic in highly weathered tropical soils of Brazil and renders this life-essential nutrient less available to plants over time. Our research aims to integrate information from multiple Sirius beamlines to discover how physical, chemical, and biological processes collectively contribute to this fixation, and how to diminish or reverse this process to maintain more sustainable and productive agriculture. Sirius is particularly well-suited, by design, for analyzing static and dynamic processes in soils using complementary scattering, imaging, and spectroscopy capabilities that span length scales from angstroms to centimeters. Specific examples of ongoing research will be presented, including complementary analyses of chemical and physical-structure of soil microaggregates and development of a rhizomicrocosm for in-vivo imaging of nutrient movement to a living plant root.

Dean Hesterberg is a Soil Science Advisor and Researcher at the Brazilian Synchrotron Light Laboratory (LNLS) at the Brazilian Center for Research in Energy and Materials (CNPEM) in Campinas, Brazil. He is also a William Neal Reynolds Distinguished Professor Emeritus of Soil Chemistry in the Department of Crop and Soil Sciences at North Carolina State University in the United States, where he taught and conducted research for 28 years. Dr. Hesterberg earned a B.S. degree in Plant and Soil Science from Southern Illinois University – Carbondale in 1981, an M.S. degree in Agronomy from Purdue University in 1984, and a Ph.D. degree in Soil and Environmental Sciences from the University of California – Riverside in 1988.  Before joining NC State University in 1993, he worked for Chevron Oil Field Research Company and for the Institute for Soil Fertility Research in the Netherlands. His research at LNLS focuses on developing and applying synchrotron imaging and spectroscopy techniques for understanding micro- to molecular- level dynamic processes that control behavior of phosphorus and other soil elements of importance in agricultural and environmental systems.

Speaker: Dr. Eleanor Lawrence Bright, post-doctoral researcher at the Materials Science beamline (ID11) at the European Synchrotron Radiation Facility (ESRF) in Grenoble, France.


Title:  Beam heating effects on materials science experiments: investigations at a fourth-generation synchrotron source

Abstract: Fourth-generation synchrotron X-ray sources bring increasing levels of flux and coherence, allowing unprecedented levels of resolution for a wide range of techniques, but with increasing risk of radiation damage. The high flux achievable at synchrotrons has been well known to cause damage in biological samples at around 5–20 keV; however, with increasing flux we have found that radiation effects become significant even for metal samples and high-energy X-rays through beam heating, leading to temperature increases of over 400 K with a monochromatic beam. In this seminar, we will look into an investigation of these effects performed at the ID11 beamline at the recently upgraded European Synchrotron Radiation Facility-Extremely Brilliant Source. By using thermal lattice expansion, we were able to perform in situ measurements of beam heating. Results showed significant increases in temperature for metal and ceria samples, with temperature increases as high as 400 K. By building a lumped thermodynamic model with which to compare our results, we are able to provide tool for estimating beam heating effects. These results demonstrate the importance of beam heating and provide information needed to consider, predict, and mitigate these effects.

Dr. Eleanor Lawrence Bright is a post-doctoral researcher at the Materials Science beamline (ID11) at the European Synchrotron Radiation Facility (ESRF) in Grenoble, France. Eleanor earned a M.Sci. in physics at the University of Bristol, UK, where she continued to study for a Ph.D. in the Interface Analysis Centre with work focusing on uranium compounds. During this time, Eleanor developed novel samples of uranium compounds using thin films (well suited to x-ray investigations), which she used to perform synchrotron experiments with a wide range of techniques, from imaging to resonant scattering. This sparked her interest in synchrotron research and led her to moving to ID11 at the ESRF. At such a versatile beamline, Eleanor has been involved in projects on x-ray diffraction computed tomography and beamline optimisation, as well as leading her own research on topotactic oxidation and beam heating effects. With the recent upgrade of the ESRF to a fourth-generation source, Eleanor has been investigating the effects of the increased flux on materials science experiments.

Speaker:  Dr. rer. nat. Bernd R. Müller is deputy of division Micro NDE at BAM, Berlim – Germany.


Title: Microstructure characterization of materials using synchrotron X-ray refraction techniques

Abstract: X-ray refraction is an excellent tool for the characterization of the microstructure of materials. However, there are only a few (synchrotron) laboratories in the world that use this technique for material characterisation. Therefore, the seminar will first explain the basic principles of X-ray refraction and the measurement techniques installed at the hard X-ray beamline BAMline at BESSY II (Berlin, Germany). This is followed by examples of investigations on fibre-reinforced plastic composites (CFRP) as well as ceramic (Cordierite, ZrO2-SiO2) and metallic materials (Ti-6Al-4V, Inconel). Some of the investigations were carried out both ex-situ and in-situ under mechanical and thermal load. The results are correlated with the mechanical properties of the materials.

Dr. rer. nat. Bernd R. Müller studied Physics at Technische Universität Berlin where he presented his thesis in atomic physics in 1990. After several years in basic research at several European synchrotron facilities he joined the X-ray Topography Group at BAM in 1995. At BESSY II (Berlin, Germany), he has constructed the hard X-ray beamline BAMline. His activities focus on the development and application of new techniques in high-energy synchrotron topography and computed tomography. Dr. Müller is deputy of division Micro NDE at BAM. He is lecturer at Technical University Berlin. In 2015, he received the Science Award of the German Society for Non-destructive Testing (DGZfP).

Speaker: Marina Raboni Ferreira – LNLS/CNPEM (LNLS Users Group Master’s Thesis Award 2022 winner)


Title: Spin Orientation Manipulation of Antiferromagnetic CoO Thin Films Through Structural Deformations 


Spintronics is the research branch that uses the electron spin as the degree of freedom for transporting, processing, and storing information. Recently, many studies have been focusing on applying antiferromagnetic (AFM) thin films as active layers for spintronic devices. Although AFM materials present many exciting properties, such as robustness against magnetic field perturbations and ultrafast spin dynamics, the magnetic moment manipulation in such materials is very challenging. In this seminar, I will present the main results of my Master`s Thesis, which focused on achieving the manipulation of the spin orientation on AFM CoO thin films through the controlled application of strain. For that purpose, we deposited polycrystalline CoO thin films over cross-shaped flexible Kapton substrates. Together with UVX’s XRD2 group, we developed the Bi-axial Multi Analysis Strain Instrument (2D-MASI) for performing in-plane extensive and compressive bi-axial deformations on these films. This device was designed for being compatible with multiple synchrotron radiation techniques (e.g., X-ray Diffraction and X-ray Absorption Spectroscopy) and sample environments such as low temperatures and high vacuum.  As a result, we were able to cause many different strain states to our samples and apply in-situ X-ray Stress Analysis (XSA) measurements for characterizing the deformation of the films’ crystalline structure. Finally, to connect the results obtained by XSA with the sample magnetic behavior, we performed in-situ X-ray Magnetic Linear Dichroism (XMLD) experiments for multiple strain states. Through this technique, we were able to probe changes in the CoO magnetic structure as a function of the sample’s deformation and temperature. The data allowed us to conclude that our method of applying strain was indeed able to cause the sample’s spin axis to change its orientation. 


Marina has a bachelor’s degree in physics (2017) from Universidade Federal do Paraná (UFPR), with an exchange period at the Technical University of Munich (TUM). In 2020 she got her Master’s degree in Applied Physics from Universidade Estadual de Campinas (UNICAMP). During her Master, she worked with antiferromagnetic spintronics at the XRD2 group from Laboratório Nacional de Luz Síncrotron (LNLS). Since 2020, Marina is a Ph.D. student at UNICAMP, working at EMA beamline (LNLS), where she is focused on applying synchrotron radiation techniques for the study of superconducting thin films in extreme conditions.


Speaker: Mateus Borba Cardoso (Soft and Biological Matter Division – DMB)

Title: SARS-CoV-2 and nanomedicine: What do they have in common?

Abstract: The severe acute respiratory syndrome coronavirus-2 (SARS-CoV-2) outbreak has taken the world’s attention due to the unprecedented Coronavirus Disease 2019 (COVID-19) pandemic. Therefore, the scientific community must use this moment to reflect and understand what structural characteristics give the virus such a high targeting and infectious efficiency. One of the main challenges in nanomedicine relies on designing successful targeting strategies. Currently-available nanoparticle formulations undergo non-specific interactions that result on random drug-delivery and cellular internalization profiles. These interactions deviate nanoparticles from their intended path, generate a series of off-target effects and leave them more vulnerable, for example, to phagocyte clearance. Viruses, in turn, are considered as successful examples of targeted nanoparticles that were refined through evolution. Along this talk, I will shed light on the SARS-CoV-2 and propose to look at it as a highly-efficient targeted nanoparticle, establishing an analogy with the current challenges regarding synthetic targeted nanomaterials.

Speaker: Ricardo Donizeth Reis (Extreme condition x-ray Methods of Analysis – EMA beamline group)

Title: Understanding quantum materials by X-ray techniques under extreme conditions.

Abstract: Many of today’s most exciting and potentially useful materials display states of matter that seem to be explicable only by applying quantum mechanical models. This is perhaps unsurprising as these materials can be host to a complex medley of ingredients that include many-body interactions between spins, electrons and phonons. The ground states frequently exhibit cooperative properties, such as superconductivity, charge or spin-order, Kondo effect, or exotic excitations such as Weyl or Majorana fermions. Besides the fundamental interest in understanding such materials, there is also the prospect of controlling their properties and putting them to use. Therefore, deciphering what causes quantum states of matter to form remains one of the most pressing challenges facing modern physics. In this talk, I will highlight how we can shed light on the building blocks of these materials by a combination of synchrotron techniques (x-ray absorption, diffraction, and scattering) with external pressure (hydrostatic and uniaxial), low temperature and high magnetic field in order to enable a continuous, clean and reversible tuning of quantum correlations. Our aim with this work is to drive materials through the critical region where the state of matter changes and inherently quantum effects dominate in order to probe the electronic, magnetic and structural properties as a function of lattice contraction. For that I will focus on materials that are on the verge of a phase instability with distinct crystalline structures and with electronic behavior displaying nontrivial topology.


Speaker: Ana Carolina de Mattos Zeri – Manacá (MAcromolecular micro and NAnoCrystAllography) beamline group

Title: Structural Biology at Sirius: MANACA beamline and new developments in macromolecular crystallography

Abstract: MANACÁ (Macromolecular Micro and NAno CrystAllography), first beamline in scientific commissioning at Sirius (LNLS/CNPEM), is dedicated to a range of crystallography techniques, including the most recent, serial crystallography (SX). Originally developed for use in XFELs (Xray Free Electron Lasers), SX takes advantage of micro-sized focal spots and higher flux from new light sources, as Sirius, to acquire data from hundreds of thousands of microcrystals per experiment. Experiments where samples are presented to the beam in microchip-like devices or liquid jets are already being used in other SR sources, and will be implemented at Sirius. The possibility of working with very small crystals, and also studying them at room temperature, opens new avenues for the exploration of biochemical reactions and drug development. Details of the beamline construction and commissioning, as well as first experiments, will be presented.


Speaker: Amelie Claire Rochet – Quati (X-ray Spectroscopy with Temporal Resolution) beamline group

Title: How heterogeneous catalysis will benefit from the new synchrotron source Sirius

Abstract: Synchrotrons have been used to study heterogeneous catalysis for as long as synchrotrons have existed. Due to high penetration of X-rays and non-destructive nature of analysis, X-rays are perfectly suited for studies of catalytic phenomena under in situ/operando conditions. The development of 4th generation synchrotron radiation facilities, such as SIRIUS [1], with improvement of brilliance and coherence properties, opens new ways towards catalysts characterisation, in particular with emerging imaging methodologies [2]. Moreover, the possibility of working with faster acquisition, better spatial resolution, higher sensitivity to various chemical and physical properties opens new avenues for the exploration of catalytic reactions. In this talk, I will present an overview of techniques that will be available at Sirius for getting a deep understanding of catalytic materials. In particular, I will focus on recent studies of chemical, morphological and structural properties of both model and real catalysts under in situ or operando conditions.

[1] Lin, L., Milas, N., Mukai, A. H. C., Resende, X. R., De Sá, F. H. (2014) J. Sync. Rad. 21 904

[2] Passos, A. R., Rochet, A., Manente, L. M., Suzana, A. F., Harder, R., Cha, W., Meneau, F. (2020) Nat. Comm. 11 4733


Speaker: Carlos A. Pérez – Carnaúba (X-Ray Nanoscopy) beamline group

Title: X-ray imaging methods and spatially-resolved X-ray spectroscopy at Sirius: potential applications in agronomy, environmental toxicology, and geochemistry

Abstract: Essential elements or micronutrients in low concentrations (often called trace elements) are required for plant, animal, and human nutrition. Nonessentials metal(loid)s are phytotoxic and/or zootoxic and are widely known as toxic elements. Regarding this, particularly important are those studies related to understanding the relationship between physicochemical properties of these materials and their toxicity that affects the ecosystems due to their extensive transformations. Environmental materials are intrinsically complex consisting of multiple solid phases where pollutants species at low concentration are heterogeneously distributed among different phases. Studies also in-vitro and in-vivo conditions would be preferentially conducted to properly understand their physicochemical properties and thus to assess the impact of these materials in complex systems. Given the complexity and heterogeneity of these microenvironments, analytical techniques capable of having a high spatial resolution, elemental sensitivity while preserving the main features of the volume under investigation, are well-preferred. In my presentation, an overview of synchrotron-based x-ray microscopy and spectromicroscopy techniques such as SR-XRF imaging, XRF tomography, and spatially-resolved XANES analysis, will be illustrated with some examples from the fields of agro-environmental, ecotoxicology, nanotoxicology, and geochemistry. A brief introduction to the Coherence X-Ray Nanofocus (CARNAÚBA) beamline will also be given, highlighting the capability for performing x-ray imaging and spectroscopic measurements on samples coming from those above-mentioned research areas. I will also describe an ongoing challenging project for conducting in-situ as well as in-vivo experiments at the root-soil environment of plants.


Speaker: Tulio Costa. Rizuti Rocha – IPÊ (Inelastic scattering and PhotoElectron spectroscopy) beamline group

Title: Probing elementary excitations in solids and molecules with RIXS

Abstract: Atoms in crystals are not standing still, they vibrate around equilibrium positions forming displacement waves that propagate. It is the dynamics of this collective motion that enable sound to propagate through solids. Excited electrons in crystals also have rich dynamics forming a plethora of collective modes and quasiparticles involving their charge, spin, and orbital, like plasmons, excitons, magnons, polarons. A key factor to model the macroscopic properties of solids, like superconductivity, ferroelectricity, thermoelectricity among others is to determine the type of excitations present, their energy and momentum dispersion. The experimental investigation of elementary excitations is based on the inelastic scattering of probe-particles such as electrons, neutrons and photons. In this talk I will explain how the resonant inelastic X-ray scattering (RIXS) technique can be used to measure the spectrum of excitations in solids and molecules, showing examples of my current research in collaboration with LNLS users. I will also highlight the main features and status of the IPE beamline of Sirius and the RIXS endstation.


Speaker: Nathaly L. Archilha – MOGNO (X-ray Micro and Nanotomography) beamline group

Title: Time-resolved experiments at Mogno beamline – applications in groundwater remediation and oil recovery

Transport in porous media is related to many fields of research and there are still several open questions, mainly related to pore scale events. The oil and gas industry has developed a lot of knowledge related to non-reactive and multiphase flow in porous media, relating pore scale events to field scale observations, which is known as upscaling. However, the same type of knowledge using a reactive fluid, covering areas such as groundwater remediation, is still very limited. In this talk, I will present results of time-resolved X-ray microtomography experiments in two different areas: enhanced oil recovery using Si nanoparticles and groundwater remediation using zero-valent iron nanoparticles. Both nanoparticles, at the time of the experiment, were well known for promoting or oil recovery or remediating groundwater for a specific family of contaminants. The proposal, in both experiments, was to investigate pore scale events, using an in-house developed flow cell, to bring new information to this field from the pore scale perspective. In addition, I will be commenting on current challenges in these areas and how Mogno’s unique design can help resolve open issues.


Speaker: Raul de Oliveira Freitas – IMBUIA (Infrared Multiscale Beamline for Ultra-resolved Imaging Applications) beamline group

Title: Infrared ultramicroscopy as a decisive tool for chemical and optical analysis of multidisciplinar nanomaterials.

Abstract: The use of infrared (IR) radiation from storage rings has brought unprecedented opportunities in label-free chemical analysis of materials. Such breakthrough was intrinsically connected to the higher brightness of the synchrotron IR compared to the classic back body thermal sources. Hence, the era of IR microscopy had started, and synchrotron facilities were meeting points for advanced spatial-spectral chemical imaging. In the last decade, the interest in sub-microscopic properties of the matter became a day-by-day demand and the classical diffraction limit of light prevented IR microscopy to follow those updates. In this presentation, the ultramicroscopy modality named synchrotron IR nanospectroscopy (SINS) is presented as an established analytical technique able to access complex optical and vibrational `properties of multidisciplinary materials at the nanoscale. In special, it will be presented the advances brought by this modality to the IR users’ program at the LNLS. Drug delivery, new energy materials, in-liquid nano-chemistry of biosystems and nano-optics of quantum materials are some of cases to be approached in this talk.


Speaker: Lucia Maria Toscani – Centro Atomico Bariloche (LNLS Users Group PhD thesis award 2021 winner)

Title: Catalytic and electrocatalytic study of ceria-based nanomaterials as anodes of intermediate-temperature solid oxide fuel cells

Abstract:The development of an economically feasible Solid Oxide Fuel Cell (SOFC) technology has driven the research activity in this area toward the reduction of their operating temperature. The focus has been set in the design of new anode materials, with high catalytic and electrocatalytic activity and resistance to coke deposition when hydrocarbons are used as fuels. In particular, efforts have been set in the development of new nanostructured materials with high ionic-electronic conductivity to enhance electrode reactions kinetics when operating temperature is reduced to the intermediate temperature regime (IT-SOFC, 500-700°C). In this talk I will present the main results of my thesis work in which I followed different materials’ design strategies to improve the performance of CeO2-based materials for catalytic and electrocatalytic applications. In particular, I addressed the optimization of catalytic materials to be used as anodes of SOFCs operated with different fuels. In this field, generally a ceramic material is used as a support for a metallic active phase. Thus, I applied two design strategies focused in the improvement of both ceramic and metallic active phases to enhance the ionic conductivity and resistance to coke deposition of the electrode material. In this context, the use of synchrotron techniques at the UVX ring in the LNLS was crucial to characterize in depth the performance of the electrodes by carrying out in-situ experiments in oxidizing and reducing conditions to be able to study the fuel interaction with the materials in close-to operating conditions.