# OVERVIEW

BACK

Overview of the XDS experimental hutch showing some of the experimental setups.

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

Coordination: Narcizo Marques de Souza Neto
Number: +55 19 3512 1051
E-mail: narcizo.souza@lnls.br

# 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

ElementTypePosition [m]Description
SOURCEInsertion DeviceInsertion Device W09A, 4T Superconducting Wiggler, 1.28 x 0.023 m$^2$
M1Cylindrical Vertical Collimating Mirror11Si, Rh and Pt coated stripes, $\theta$=2.75 mrad
MonoDouble Crystal Monochromator13.5Cryo-cooled flat Si(111) and Si(311) pairs; Si(111) with sagital bending
M2Cylindrical and Toroidal Focusing Mirror16Rh and Pt coated, $\theta$=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

ParameterValueCondition
Energy range [keV]5 - 30Si(111) and Si(311)
Energy resolution [$\Delta$E/E]$10^{-4}$Si(111)
Energy resolution [$\Delta$E/E]$10^{-5}$Si(311)
Beam size at sample [$\mu \rm m^{2}$, FWHM]1400 x 300at 10 keV
Beam divergence at sample [$\rm mrad^{2}$, FWHM]2.5 x 0.4at 10 keV
Flux density at sample [ph/s/$\rm mm^{2}$]$5 \times 10 ^{12}$at 10 keV

# INSTRUMENTATION

InstrumentTypeModelSpecificationsManufacturer
DetectorAreaPilatus 300KArea 83.8 × 106.5 $\rm mm^{2}$. Pixel size: 172 x 172 $\mu \rm m^{2}$, 1kHz frame rate.Dectris
DetectorFluorescenceSiLi 12 element-PGT
DetectorAreaMarCCD 225-Rayonix
FurnaceCapillaryHTK 1200NMax Temp.: 1200ºC, Temp Rate: 50°C/minAnton Paar
Diffractometer6+2 circle-6 circle diffractometerHuber
Sample CellHigh pressure Diamond anvil cell Membrane and screw drivenCan reach up to 80 GPaLNLS in-house development, Syntek, Princeton
CryostatsJT CryostatMinimum temp.:1.2 KClosed loop cryostatA S Scientific
MagnetSC cryo-free6 T HTS-11Superconducting magnetHTS 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 publications and to inform the Laboratory about any publications, thesis and other published materials. Users must also cooperate by supplying this information upon request.

Support text for acknowledgements:

This research used resources of the Brazilian Synchrotron Light Laboratory (LNLS), an open national facility operated by the Brazilian Centre for Research in Energy and Materials (CNPEM) for the Brazilian Ministry for Science, Technology, Innovations and Communications (MCTIC). The _ _ _ beamline staff is acknowledged for the assistance during the experiments.

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 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.

XDS   XRD2

Marçal, L. A. B.; Richard, M. I.; Persichetti, L. ; Favre-Nicolin, V.; Renevier, H. ; Fanfoni, M. ; Sgarlata, A. ; Schülli, T. U.; Malachias, A.. Modified strain and elastic energy behavior of Ge islands formed on high-miscut Si(001) substrates, Applied Surface Science, v. 466, p. 801-807, 2019. DOI: 10.1016/j.apsusc.2018.10.094

XDS

Silva, T. R.; Oliveira, D. C.; Pal, T.; Domingos, J. B.. The catalytic evaluation of bimetallic Pd-based nanocatalysts supported on ion exchange resin in nitro and alkyne reduction reactions, New Journal of Chemistry, v. 43, n. 18, p. 7083-7092, 2019. DOI: 10.1039/c9nj00285e

XDS

Ferreira, L. M. ; Carneiro, F. B. ; Fontes, M. B. ; Baggio-Saitovich, E.; Veiga, L. S. I.; Mardegan, J. R. L.; Strempfer, J. ; Piva, M. M.; Pagliuso, P. G.; Reis, R. D.; Bittar, E. M.. Pressure effects on the structural and superconducting transitions in La3Co4Sn13, Journal of Alloys and Compounds, v. 773, p. 34-39, 2019. DOI: 10.1016/j.jallcom.2018.09.236

XDS

Noveletto, J. C. ; Ferreira Neto, E. P.; Gonçalves, L. P.; Ullah, S.; Donatti, D. A.; Ribeiro, S. J. L.; Rodrigues-Filho, U. P. Plasmonic silver-based reversible photochromism in Ag+-doped organomodified silicates-phosphotungstate hybrid films, Optical Materials, v. 92, p. 233-242, 2019. DOI: 10.1016/j.optmat.2019.04.034

PGM   XDS

Jesus, J. R.; Garcia, F.; Duque, J. G. L.; Meneses, C. T.. Study of exchange bias in single-phase Dy0.2Nd0.8CrO3, Journal of Alloys and Compounds, v. 779, p. 577-581, 2019. DOI: 10.1016/j.jallcom.2018.10.335

XDS

Lima, T. A.; Faria, L. F. O.; Paschoal, V. H.; Ribeiro, M. C. C.. Exploring the phase diagram of the ionic liquid 1-butyl-1-methylpyrrolidinium bis(trifluoromethanesufonyl)imide, Journal of Molecular Structure, v. 1183, p. 149-156, 2019. DOI: 10.1016/j.molstruc.2019.01.076

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