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SXS Beamline

The SXS beamline is an experimental station dedicated to X-ray Absorption and Photoelectron Spectroscopy in the soft X-rays (1 to 5 keV) energy range. It focuses on to study the electronic, magnetic and geometric structures of materials with applications to atomic and molecular physics, analytical chemistry, environmental and geoscience. Other experimental techniques available include X-ray Magnetic Dichroism and Resonant Auger Spectroscopy.

The SXS beamline is operational for users since 1997 and a broad scientific community including material science, surface science, atomic physics and chemistry among others has used it. Due an increasing demand from the users, in 2009 this beamline had a new X-ray optics in order to provide photons in the energy range from 1000 eV up to 5000 eV.

SXS’ source is a 1.67T bending magnet. There is a nickel-coated and toroidal (1010 x 100 x 100 mm) water cooled mirror that focuses the photon beam at the sample position and it suppresses the harmonic contamination (> 6keV). The incident angle is 0.6 deg and the spot size is 0.6 x 1.2 mm (FWHM) at the sample position.

sxs-fluxThe monochromator is a double-crystal with 4 pairs of crystals: Si(111), InSb(111), YB66(400) and Beryl(1010). It works under high vacuum ($5 \times 10^{-8}$ mbar) and the first crystals are maintained below 30 Celsius by a water cooling system.

CONTACT & STAFF

For more information on this beamline, contact us.

EXPERIMENTAL TECHNIQUES

The following experimental techniques and setups are available to users in this beamline. To learn more about the techniques’ limitations and requirements (sample, environment, etc.) contact the beamline coordinator before submitting your proposal.

X-RAY ABSORPTION SPECTROSCOPY (XAS)

X-ray absorption spectroscopy (XAS) is a widely used technique for determining the local geometric and/or electronic structure of matter.

Setup: Conventional Total electron yield (TEY) and Fluorescence XAS

This setup is optimized for TEY and fluorescence XAS on “standard samples” in standard sample holders. The setup for these experiments, called BioXAS workstation has two electrometers (Io and sample signal), a silicon drift diode (SDD) fluorescence detector, chamber with a differential pumping and a room temperature sample stage (xyzθ). In order to use this setup, samples/environments must fit within our room temperature sample stage.

Recent publications using this setup:

Abdala DB et al., Residence time and pH effects on the bonding configuration of orthophosphate surface complexes at the goethite/water interface as examined by Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy, Journal of Colloid and Interface Science 442 (2015) 15–21;

Andrini L et al., Extended and local structural description of a kaolinitic clay, itsfired ceramics and intermediates: An XRD and XANES analysis, Applied Clay Science 124–125 (2016) 39–45;

Dalfovo MC et al., Real-Time Monitoring Distance Changes in Surfactant-Coated Au Nanoparticle Films upon Volatile Organic Compounds (VOCs), J. Phys. Chem. C (2015), 119, 5098−5106;

Yasser AA et al., Photostability of gold nanoparticles with different shapes: the role of Ag clusters, Nanoscale, 2015, 7, 11273.

X-RAY PHOTOELECTRON SPECTROSCOPY (XPS)

Setup: Conventional XPS

This setup is intended for XPS on “standard samples” in standard sample holders. The setup for these experiments, called XPS workstation has two electrometers (Io and sample signal), a hemispherical electron analyzer (Phoibos 150), ultra-high vacuum chamber with base pressure about 5×10-10 mbar and a room temperature motorized sample stage (xyzθ). In order to use this setup, samples/environments must fit within our room temperature sample holder inside a high vacuum pre-chamber. The pre-chamber environment allow submitting the samples to different gas atmospheres, while heating up to 900 °C and, after the treatment, the sample holder is inserted within the analysis chamber, using a load lock system.

Recent publications using this setup:

Garcia-Basabe Y et al., The effect of thermal annealing on the charge transfer dynamics of a donor–acceptor copolymer and fullerene: F8T2 and F8T2:PCBM, Phys.Chem.Chem.Phys., 2015,17, 11244;

Larrude DG et al., Electronic structure and ultrafast charge transfer dynamics of phosphorous doped graphene layers on a copper substrate: a combined spectroscopic study, RSC Adv.,2015,5, 74189;

Martins HP et al., X-ray absorption study of the Fe and Mo valence states in Sr2FeMoO6, Journal of Alloys and Compounds 640 (2015) 511–516;

Silva DO et al., Straightforward synthesis of bimetallic Co/Pt nanoparticles in ionic liquid: atomic rearrangement driven by reduction–sulfidation processes and Fischer–Tropsch catalysis, Nanoscale, 2014, 6, 9085.

X-RAY MAGNETIC DICHROISM
RESONANT AUGER SPECTROSCOPY

LAYOUT & OPTICAL ELEMENTS

Element Type Position [m] Description
SOURCE Bending Magnet 0.00 Bending Magnet D04 exit A (4°), 1.67 T
Mirror Toroidal Horizontal and Vertical Focusing Mirror 7.00 Ni coated, RT = 668m, RS = 73mm, θ = 10 mrad
Mono Double Crystal Monochromator 11.75 Water-cooled InSb(111), Si(111), YB66 (400) and Beryl(10-10)

PARAMETERS

Parameter Value Condition
Energy range [keV] 1-5 Si(111)
Energy resolution [ΔE/E] 10-4 Si(111)
Beam size at sample [mm2, FWHM] 0.6 x 1.2 at 3 keV
Beam divergence at sample [mrad2, FWHM] 0.2 x 4 at 3 keV
Flux density at sample [ph/s/mm2] 4 x 1011 at 3 keV

INSTRUMENTATION

Instrument Type Model Manufacturer Specifications
Total electron yield detector Electrometer 6514 20 pA – 2 mA range Keithley
Fluorescence Detector Silicon drift diode SuperFast SDD Area: 25 mm2; Energy resolution: 125–155 eV Amptek
Photoelectron analyzer Hemispherical Phoibos 150 MCD with 9 channels; 3500 eV kinetic energy Specs
Furnace Halogen lamps/ high vacuum Max Temp.: 900°C LNLS in-house development
Sputtering Argon IG2 ion source 0.5-2kV; 2.5mm beam diameter at 25 mm RBD
Residual gas analyzer Mass spectrometer RGA200 1-200 amu; quadrupole SRS
Sample charge neutralizer Electron flood gun FG15/40 0-500 eV; 0-5 mA Specs
Sample Cells  Liquid Ultralene window; 4 x 113 µL LNLS in-house development

CONTROL AND DATA ACQUISITION

All beamline controls are done through EPICS (Experimental Physics and Industrial Control System), running on a PXI from National Instruments. The data acquisition is done using a Red Hat workstation with the Py4Syn, developed at LNLS by SOL group. CSS (Control System Studio) is used as a graphical interface to display and control the beamline devices.

HOW TO CITE THIS FACILITY

Users are required to acknowledge the use of LNLS facilities in any paper, conference presentation, thesis and any other published material that uses data obtained in the execution of their proposal.

 

Additionally, in publications related to this facility, please cite the following publication.

ABBATE, F. C. VICENTIN, V. COMPAGNON-CAILHOL, M. C. ROCHA AND H. TOLENTINO, The soft X-ray spectroscopy beamline at the LNLS: technical description and commissioning results, J. Synchrotron Rad., 6, 964 (1999). doi:10.1107/S0909049599008122.

The soft X-ray spectroscopy beamline installed at a bending-magnet source in the LNLS is presented. A technical description of the main elements is given and some selected commissioning results are shown. The beamline optics was designed to cover the soft X-ray energy range from 790 up to 4000 eV. The bending-magnet source has a critical energy of 2.08 keV and delivers ~10^{12} photons.s^{-1}.mradH^{-1} (0.1% bandwidth)^{-1}(100 mA)^{-1}. The focusing element is a gold-coated toroidal mirror operating at an angle of incidence of 1°. The double-crystal monochromator has three pairs of crystals which can be selected by a lateral translation. The UHV experimental station is equipped with an ion gun, an electron gun, a LEED optics and an electron analyzer. The beamline is intended for X-ray absorption, photoemission, reflectivity and dichroism experiments. The beamline has been installed, commissioned, and is now open to the external users community.

TOLENTINO, V. COMPAGNON-CAILHOL, F. C. VICENTIN AND M. ABBATE,The LNLS soft X-ray spectroscopy beamline, J. Synchrotron Rad., 5, 539 (1998). doi:10.1107/S0909049597016087.

The soft X-ray spectroscopy beamline installed at a bending-magnet source at the LNLS is described. The optics are designed to cover energies from 800 to 4000 eV with good efficiency. The focusing element is a gold-coated toroidal mirror with an angle of incidence of 17 mrad. The UHV double-crystal monochromator has three pairs of crystals, Si (111), InSb (111) and beryl (10-10), that can be selected by a sliding movement. The UHV workstation is equipped with an ion gun, an electron gun, an electron analyser, LEED optics, an open channeltron and a photodiode array. This beamline is intended for photoemission, photoabsorption, reflectivity and dichroism experiments.

PUBLICATIONS

Scientific publications produced with data obtained at the facilities of this beamline, and published in journals indexed by the Web of Science, are listed below.

Attention Users: Given the importance of the previous scientific results to the overall proposal evaluation process, users are strongly advised to check and update their publication record both at the SAU Online website and at the CNPEM library database. For the library, updates can be made by sending the full bibliographic data to the CNPEM library (biblioteca@cnpem.br). Publications are included in the database after being checked by the CNPEM librarians and the beamline coordinators.


Medeiros, G. A. ; Corrêa, J.R.; Andrade, L. P.; Lopes, T. O. ; Oliveira, H. C. B. de; Diniz, A. B. ; Menezes, G. B. de; Rodrigues, M. O.; Neto, B.A.D.. A benzothiadiazole-quinoline hybrid sensor for specific bioimaging and surgery procedures in mice, Sensors and Actuators B-Chemical, v.328, p. 128998, 2021. DOI:10.1016/j.snb.2020.128998


García- Basabe, Y.; Gordo, V. O. ; Daminelli, L. M.; Mendoza, C. D.; Vicentin, F. C.; Matusalem, F.; Rocha, A. R.; Matos, C. J. S. de; Larrude, D. G.. Interfacial electronic coupling and band alignment of P3HT and exfoliated black phosphorous van der Waals heterojunctions, Applied Surface Science, v. 541, p.148455, 2021. DOI:10.1016/j.apsusc.2020.148455


Ramoni, M. ; Bassi, M. de J. ; Wouk, L. ; Pacheco, K. R. M. ; Fernández, A. B. ; Renzi, W.; Duarte, J. L. ; Rocco, M. L. M.; Roman, L. S.. Morphology, Photoexcitation Dynamics and Stability of Water-Dispersed Nanoparticle Films based on Semiconducting Copolymer, Thin Solid Films, v.721, p. 138536, 2021. DOI:10.1016/j.tsf.2021.138536


Sammaritano, M. L. A. ; Cometto, P. M. ; Bustos, D. A. ; Wannaz, E. D.. Monitoring of particulate matter (PM2.5 and PM10) in San Juan city, Argentina, using active samplers and the species Tillandsia capillaris, Environmental Science and Pollution Research, v.28, p.32962–32972, 2021. DOI:10.1007/s11356-021-13174-4


Rodrigues, L. do N. ; Scolfaro, D.; Conceição, L. da; Malachias, A.; Couto Jr., O. D. D.; Iikawa, F.; Deneke, C.. Rolled-Up Quantum Wells Composed of Nanolayered InGaAs/GaAs Heterostructures as Optical Materials for Quantum Information Technology, ACS Applied Nano Materials, v.4, n.3, p.3140-3147, 2021. DOI:10.1021/acsanm.1c00354


Soares, B. M.; Sodré, P. T.; Aguilar, A. M. ; Gerbelli, B. B. ; Pelin, J. N. B. D.; Arguello, K. B. ; Silva, E. R. da; Farias, M. A. de; Portugal, R. V.; Schmuck, C. ; Coutinho Neto, M. D.; Alves, W. A.. Structure optimization of lipopeptide assemblies for aldol reactions in an aqueous medium, Physical Chemistry Chemical Physics, v.23, n.18, p. 10953-10963, 2021. DOI:10.1039/d1cp01060c