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XDS Beamline

The XDS beamline is an experimental station dedicated to X-ray Diffraction and Spectroscopy in the hard x-rays (5 to 30 keV) energy range. It focuses on determination of atomic, electronic and magnetic structure of materials with applications to condensed matter physics, chemistry, geosciences, among others. Several sample environments are available at XDS: high pressure cells to subject samples up to 80 GPa, magnetic field of 6 T magnet for diffraction experiments, cryostat for temperatures as low as 1.8 K, furnaces for temperatures up to 1200 K.

The X-ray Diffraction and Spectroscopy (XDS) beamline uses the radiation emitted by the Superconducting Wiggler source and is employed for multipurpose experiments. Some of the diffraction experiments demand control of the horizontal divergence, only achievable with sagittal focusing in a double crystal monochromator. On the other hand, the use of flat crystals and focusing with a toroidal mirror was considered to be the best choice for XAS measurements. These apparently contradictory requirements from the diffraction and absorption community led us to introduce a flexible configuration for this beamline. According to this concept, the beamline operates with a collimating mirror with bender (with Si, Rh and Pt stripes), a double crystal monochromator (DCM) with two interchangeable sets of crystals [plane Si(111), sagittal Si(111) and plane Si(311)], and a focusing mirror with three stripes (toroidal Rh, plane Rh and toroidal Pt) and a bending mechanism to allow for focus adjustments.

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 spectroscopy of elements at 4th row of periodic table;
  • X-ray diffraction under high pressure (HP-XRD);
  • X-ray spectroscopy under high pressure (HP-XAS);
  • Pair distribution function (PDF);
  • Diffraction Anomalous Fine Structure (DAFS);
  • Resonant/magnetic x-ray diffraction (XRMS);
  • Inelastic X-ray Scattering (RIXS / X-ray Raman);
  • Grazing incidence x-ray scattering (GI-XRD).

LAYOUT & OPTICAL ELEMENTS

Element Type Position [m] Description
SOURCE Insertion Device Insertion Device W09A, 4T Superconducting Wiggler, 1.28 x 0.023 m2
M1 Cylindrical Vertical Collimating Mirror 11 Si, Rh and Pt coated stripes, θ=2.75 mrad
Mono Double Crystal Monochromator 13.5 Cryo-cooled flat Si(111) and Si(311) pairs; Si(111) with sagital bending
M2 Cylindrical and Toroidal Focusing Mirror 16 Rh and Pt coated, θ=2.75 mrad, bending mechanism for vertical focusing, toroidal stripes for horizontal focusing, flat Rh stripe for use with sagittal focusing or unfocus mode

PARAMETERS

Parameter Value Condition
Energy range [keV] 5 – 30 Si(111) and Si(311)
Energy resolution [ΔE/E] 10-4 Si(111)
Energy resolution [ΔE/E] 10-5 Si(311)
Beam size at sample [µm2, FWHM] 1400 x 300 at 10 keV
Beam divergence at sample [mrad2, FWHM] 2.5 x 0.4 at 10 keV
Flux density at sample [ph/s/mm2] 5 x 1012 at 10 keV

INSTRUMENTATION

Instrument Type Model Manufacturer Specifications
Detector Area Pilatus 300K Area 83.8 × 106.5 mm2. Pixel size: 172 x 172 µm2, 1kHz frame rate. Dectris
Detector Fluorescence SiLi 12 element PGT
Detector Area MarCCD 225 Rayonix
Furnace Capillary HTK 1200N Max Temp.: 1200ºC, Temp Rate: 50°C/min Anton Paar
Diffractometer 6+2 circle 6 circle diffractometer Huber
Sample Cell High pressure Diamond anvil cell Membrane and screw driven Can reach up to 80 GPa LNLS in-house development, Syntek, Princeton
Cryostats JT Cryostat Minimum temp.:1.2 K Closed loop cryostat A S Scientific
Magnet SC cryo-free 6 T HTS-11 Superconducting magnet HTS 110

CONTROL AND DATA ACQUISITION

All beamline controls are done through SPEC software.

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.

F. A. Lima et al.,  XDS: a flexible beamline for X-ray diffraction and spectroscopy at the Brazilian synchrotron, J. Synchrotron Rad. (2016). 23, 1538–1549

The majority of the beamlines at the Brazilian Synchrotron Light Source Laboratory (LNLS) use radiation produced in the storage-ring bending magnets and are therefore currently limited in the flux that can be used in the harder part of the X-ray spectrum (above ∼10 keV). A 4 T superconducting multipolar wiggler (SCW) was recently installed at LNLS in order to improve the photon flux above 10 keV and fulfill the demands set by the materials science community. A new multi-purpose beamline was then installed at the LNLS using the SCW as a photon source. The XDS is a flexible beamline operating in the energy range between 5 and 30 keV, designed to perform experiments using absorption, diffraction and scattering techniques. Most of the work performed at the XDS beamline concentrates on X-ray absorption spectroscopy at energies above 18 keV and high-resolution diffraction experiments. More recently, new setups and photon-hungry experiments such as total X-ray scattering, X-ray diffraction under high pressures, resonant X-ray emission spectroscopy, among others, have started to become routine at XDS. Here, the XDS beamline characteristics, performance and a few new experimental possibilities are described.

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