XRD1’s 3-circle diffractometer (on the left) and the robotic arm holding the Cryojet system (on the right).

OVERVIEW

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.

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

Element	Type	Position [m]	Description
SRC	Bending Magnet	0.0	Bending Magnet D12 exit A (4°), 1.67 T
FE	Front-end	-	-
S1	White Beam Slits	4.5	Water-cooled
M1	Vertical Focusing Mirror	5.4	Rh coated
DCM	Double Crystal Monochromator	6.7	Si(111)
S2	Slits	12.5	-
S3	Slits	15.5	-
ES	Experimental Station	18.2	-

PARAMETERS

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

INSTRUMENTATION

Instrument	Type	Model	Specifications	Manufacturer
Diffractometer	3 circle	N3050-P1	$2 \theta_{\rm max} = 150^{\circ} $	Newport
Detectors	Linear	Mythen24K	$50 \mu \rm m$ pixel 24 modules	Dectris
Cryojet	Cooler and Heater	CryojetHT	100 - 450 K at sample	Oxford Instruments
Gas Blower	Heater	GSB1300	RT - 1070 K at sample	FMB Oxford
Capillary Cell	-	-	Use capillaries with diameters up to 2 mm	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 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 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.

XRD1

Rodrigues, C. ; Naasani, L. I. S.; Zanatelli, C; Paim, T. C.; Azevedo, J. G. ; Lima, J. C. de; Fernandes, M. da C.; Buchner, S.; Wink, M. R.. Bioglass 45S5: Structural characterization of short range order and analysis of biocompatibility with adipose-derived mesenchymal stromal cells in vitro and in vivo, Materials Science & Engineering C-Materials for Biological Applications, v. 103, 9. 109781, 2019. DOI: 10.1016/j.msec.2019.109781

XRD1

Cardoso, J. L. ; Mandel, M.; Krüger, L. ; Herculano, L. F. G. ; Lima Neto, P. de ; Silva, M. J. G. da. Corrosion Behavior of Austenitic Stainless Steels in CO2-Saturated Synthetic Oil Field Formation Water, Materials Research-Ibero-american Journal of Materials, v. 22, n. 4, p. UNSP e20180334, 2019. DOI: 10.1590/1980-5373-MR-2018-0334

XRD1 XTMS

Coury, F. G.; Santana, D. ; Guo, Y.; Copley, J.; Otani, L.; Fonseca, S. T.; Zepon, G.; Kiminami, C. S.; Kaufman, M. J.; Clarke, A.. Design and in-situ characterization of a strong and ductile co-rich multicomponent alloy with transformation induced plasticity, Scripta Materialia, v. 173, p. 70-74, 2019. DOI: 10.1016/j.scriptamat.2019.07.045

XRD1

Antunes, L. H. M.; Hoyos, J. J.; Fonseca, E. B.; Béres, M.; Farina, P. F. S.; Lopes, E. S. N.; Maciel Filho, R.; Jardini, A. L.. Effect of phase transformation on ductility of additively manufactured Co-28Cr-6Mo alloy: An in situ synchrotron X-ray diffraction study during mechanical testing, Materials Science and Engineering A-Structural Materials Properties Microstructure and Processing, v. 764, p. 138262, 2019. DOI: 10.1016/j.msea.2019.138262

XRD1 XTMS

Izumi, M. T. ; Hoyos, J. J.; Crivoi, M. ; Maeda, M. Y. ; Namur, R. S. ; Aguiar, D. J. M. de ; Cintho, O. M.. In Situ X-Ray Diffraction Analysis of Face-Centered Cubic Metals Deformed at Room and Cryogenic Temperatures, Journal of Materials Engineering and Performance, v. 28, n. 8, p. 4658-4666, 2019. DOI: 10.1007/s11665-019-04226-5

XRD1

Campos, M.; Souza, S. de ; Davim, J. P. ; Souza, S. D.; Olzon-Dionysio, M.. Influence of the Gas Pressure of Plasma Nitriding on the Structural, Mechanical and Tribological Surface Properties of AISI 316L, Materials Research-Ibero-american Journal of Materials, v. 22, n. 4, p. UNSP e20190302, 2019. DOI: 10.1590/1980-5373-MR-2019-0302

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