# OVERVIEW

BACK

The XRD1 beamline is an experimental facility dedicated to X-ray powder diffraction analysis in the hard x-rays energy range (5.5 to 14 keV). It focus on the determination of structural parameters of polycrystalline samples, with applications to physics, chemistry, materials science, materials engineering, geosciences, pharmacy, biology, etc. It is also possible to study the samples in a large range of temperatures (100 – 1070 K).

XRD1 is operational since 1998 and installed on a 1.67 T bending magnet. Recently, the beamline was upgraded and its commissioning is entirely performed. The XRD1 beamline has two experimental stations since 2010. The second experimental station consists of a facility built around an advanced thermo-mechanical simulator, the Gleeble®Synchrotron system, which allows the material of interest to be subject to a wide range of thermo-mechanical conditions.

The first experimental station was built in 1997. With the upgrade process, the old diffractometer was replaced by the 3-circle heavy-duty diffractometer from Newport®. Furthermore, the installation of the MYTHEN 24K system, from Dectris®, and a robotic arm sample changer allowed relatively fast X-ray powder diffraction measurements. The measurement times vary typically between 30 and 400 seconds, depending on the sample and the investigation aims.

Applications include the determination of the lattice parameters of polycrystalline materials as a function of the temperature, resonant X-ray diffraction from K-edge of vanadium to K-edge of bromine and from L­3-edge of cerium to L­3-edge of polonium, and in-situ experiments with powder and liquid samples.

# CONTACT & STAFF

Beamline Phone Number: +55 19 3512 1133
Beamline E-mail: xrd1@lnls.br

Coordinator: Alexandre Magnus Gomes Carvalho
Number: +55 19 3517 5137
E-mail: alexandre.carvalho@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 DIFFRACTION (XRD)

The XRD1 beamline is optimized for structural characterization by X-ray diffraction experiments in Debye-Scherrer geometry, i. e. transmission mode of low absorption materials. Besides, XRD1 is able to obtain high-quality data for high-absorption materials. It is possible to change the energy to perform resonant X-ray diffraction from K-edge of vanadium to K-edge of bromine and from L3-edge of cerium to L3-edge of polonium. The XRD1 beamline is equipped with two different devices to perform X-ray powder diffraction as a function of the temperature (from 100 K to 1070 K). The beamline is also equipped with a capillary cell, which is used for experiments with powder and gas flux or with liquids.

# LAYOUT & OPTICAL ELEMENTS

ElementTypePosition[m]Description
SRCBending Magnet0.0Bending Magnet D12 exit A (4°), 1.67 T
FEFront-end--
S1White Beam Slits4.5Water-cooled
M1Vertical Focusing Mirror5.4Rh coated
DCMDouble Crystal Monochromator6.7Si(111)
S2Slits12.5-
S3Slits15.5-
ESExperimental Station18.2-

# PARAMETERS

ParameterValueCondition
Energy range [keV]5.5-14Si(111)
Energy resolution [$\Delta$E/E]$3 \times 10^{-4}$Si(111)
Beam size at sample [$\rm mm^{2}$, FWHM]2.0 x 0.7at 12 keV
Vertical Beam divergence at sample [$\mu \rm rad$, FWHM]116at 8 keV
Flux density at sample [ph/s/$\rm mm^{2}$]$2.4 \times 10^{10}$at 8 keV

# INSTRUMENTATION

InstrumentTypeModelSpecificationsManufacturer
Diffractometer3 circleN3050-P1$2 \theta_{\rm max} = 150^{\circ}$Newport
DetectorsLinearMythen24K$50 \mu \rm m$ pixel 24 modulesDectris
CryojetCooler and HeaterCryojetHT100 - 450 K at sampleOxford Instruments
Gas BlowerHeaterGSB1300RT - 1070 K at sampleFMB Oxford
Capillary Cell--Use capillaries with diameters up to 2 mmLNLS 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.

# APPLYING FOR BEAMTIME

Submission calls are usually announced twice per year, one for each semester. All the academic research proposals must be submitted electronically through the SAU Online portal. Learn more about how to submit a proposal here.

Important: This beamline is available for fast-track submission. Learn more about how to submit your proposal as a fast-track submission here.

# HOW TO CITE THIS BEAMLINE

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 the XRD1 beamline, please cite the following publication.

A. M. G. Carvalho, D. H. C. Araújo, H. F. Canova, C. B. Rodella, D. H. Barrett, S. L. Cuffini, R. N. Costa, R. S. Nunes, X-ray powder diffraction at the XRD1 beamline at LNLS, J. Synchrotron Rad. 23, 1501-1506 (2016). DOI: 10.1107/S1600577516012686

Various upgrades have been completed at the XRD1 beamline at the Brazilian synchrotron light source (LNLS). The upgrades are comprehensive, with changes to both hardware and software, now allowing users of the beamline to conduct X-ray powder diffraction experiments with faster data acquisition times and improved quality. The main beamline parameters and the results obtained for different standards are presented, showing the beamline ability of performing high-quality experiments in transmission geometry. XRD1 operates in the 5.5-14 keV range and has a photon flux of $\rm 7.8 \times 10^{9} photons.s^{-1}$ (with 100 mA) at 12 keV, which is one of the typical working energies. At 8 keV (the other typical working energy) the photon flux at the sample position is $\rm 3.4 \times 10^{10} \rm photons.s^{-1}$ and the energy resolution $\rm \Delta E/E = 3 \times 10^{-4}$.

# 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.

MORE PUBLICATIONS

XRD1

Serrano-Alfaro, P. ; Estevez-Rams, E.; Lora-Serrano, R.; Aragon-Fernandez, B.. Determination of stacking ordering in disordered close-packed structures from pairwise correlation functions, Acta Crystallographica A-Foundation and Advances, v. 75, part 1, p. 71-81, 2019. DOI: 10.1107/S2053273318014080

XRD1

Testa, C. G. ; Prado, L. D. ; Costa, R. N. ; Costa, M. L. ; Linck, Y. G. ; Monti, G. A. ; Cuffini, S. L.; Rocha, H. V. A.. Challenging identification of polymorphic mixture: Polymorphs I, II and III in olanzapine raw materials, International Journal of Pharmaceutics, v. 556, p. 125-135, 2019. DOI: 10.1016/j.ijpharm.2018.12.008

TGM   XAFS1   XAFS2   XRD1

Machado, I. P. ; Teixeira, V. C.; Pedroso, C. C. S.; Brito, H. F.; Rodrigues, L. C. V.. X-ray scintillator Gd2O2S:Tb3+ materials obtained by a rapid and cost-effective microwave-assisted solid-state synthesis, Journal of Alloys and Compounds, v. 777, p. 638-645, 2019. DOI: 10.1016/j.jallcom.2018.10.348

XRD1

Fiuza, T. E. R.; Borges, J. F. M.; Cunha, J. B. M.; Antunes, S. R. M.; Andrade, A. V. C.; Antunes, A. C.; Souza, E. C. F.. Iron-based inorganic pigments from residue: Preparation and application in ceramic, polymer, and paint, Dyes and Pigments, v. 148, p. 319-328, 2018. DOI: 10.1016/j.dyepig.2017.09.025

XRD1

Lan, Z.; Calligaris, G. A.; Menezes, A. S.; Santos, A. O.; Lai, X.; Cardoso, L.; Roberts, K. J.. Characterization of the Structural Environment of Dithionate Ions Associated with Their Role in the Crystal Habit Modification of Sodium Chlorate, Crystal Growth & Design, v. 18, n. 6, 3328-3338, 2018. DOI: 10.1021/acs.cgd.7b01770

XRD1

Rubio-Marcos, F.; Del Campo, A.; Rojas-Hernandez, R. E.; Ramírez, M. O.; Parra, R.; Ichikawa, R. U. ; Ramajo, L. A.; Bausá, L. E.; Fernández, J. F.. Experimental evidence of charged domain watts in lead-free ferroelectric ceramics: light-driven nanodomain switching, Nanoscale, v. 10, n. 2, p. 705-715, 2018. DOI: 10.1039/c7nr04304j

MORE PUBLICATIONS