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XRD2 Beamline

The XRD2 beamline an experimental station dedicated to X-ray Diffraction techniques in the hard x-rays range (3 to 17 keV). Several kinds of measurements can be carried out in this beamline, both in monocrystalline or policrystalline samples and thin films with Grazing-Incidence Diffraction (GID), Grazing-Incidence Small-Angle X-ray Scattering (GISAXS) and in-plane diffraction. Applications include crystallographic characterization of monocrystals at low temperatures (2K-400K), microscopic magnetism, orbital ordering studies, and characterization of thin films, quantum dots and heterostructures.

XRD2 source is a 1.67T bending magnet. The diffraction beamline has a versatile 6+2 circles diffractometer allowing to perform a wide range of diffraction/scattering techniques on different sample environments like: furnaces (< 1000°C), cryojet (> 85 K), humidity (or gas flux) chambers and more recently gas/liquid interfaces on a Langmuir trough. The optics is composed by a Rh-coated vertical-focusing mirror and a sagittal-focusing Si 111 double-crystal monochromator. It provides a 0.5 mm x 1.5 mm focus at the sample position with tunable monochromatic beam ranging from 5 to 15 keV.

Some of the usual experiments are multiple x-ray diffraction of single crystals, x-ray reflectometry, reciprocal space mapping of thin films (epitaxial, polycrystalline, textured), grazing incidence small angle x-ray scattering (GISAXS) and diffraction (GID) in supported nanoparticles or gas/liquid interfaces. Phase identification and depth profile of metallurgical alloys.

CONTACT & STAFF

For more information on this beamline, contact us.

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.

  • θ2θ: thin films, polycrystalline bulk (soil, metallic alloys, fossils, tooth, etc.);
  • X-ray reflectivity (XRR) and texture: thin films;
  • Grazing incidence x-ray diffraction (GID):thin films/coatings; nano-particles;
  • Grazing incidence small angle scattering (GISAXS): supported nano-particles;
  • Grazing incidence x-ray off-specular small angle scattering (GIXOS): liquid-air interface;
  • Reciprocal Space Map (RSM): epitaxial thin films;
  • Multiple x-ray diffraction (MXD): single crystals.

LAYOUT & OPTICAL ELEMENTS

Element Type Position [m] Description
SRC Bending Magnet 0.000 Bending Magnet D10 exit A (4°), 1.67T, 0.87mm x 0.17mm
FE Front-end 4.750
S1 White Beam Slits 5.995
M1 Cylindrical Vertical Focusing Mirror 7.048 Rh coated, θ = 20mrad
DCM Double Crystal Monochromator 8.749 Water-cooled Si (111), Sagitally bent
S2 Monochromatic Beam Slits 14.690
S3 Sample Slits 17.100
ES Experimental Station 17.478

PARAMETERS

Parameter Value Condition
Energy range [keV] 5-15
Energy resolution [ΔE/E] 8 x 10-4
Beam size at sample [mm2, FWHM] 0.5×1.5 8 keV, vertical and horizontal focus at sample
Beam divergence at sample [mrad2, FWHM] 0.6×5 8 keV, vertical and horizontal focus at sample
Flux density at sample [ph/s/mm2/100mA] 5.26 x 1010 8 keV at sample

INSTRUMENTATION

Instrument Type Model Manufacturer Specifications
Diffractometer 6+2 circles Huber 92784 Circles: 4 sample (open eulerian cradle); 2 detector; +2 crystal analyzer; +1 incident angle (±5°) Huber
Furnaces F300C 300 to 570K Temp. Rate: up to 20K/min Temp. control: 0.1K LNLS in-house development
Furnaces F1000 300 to 1270K Temp. Rate: up to 20K/min Temp. control: 1K LNLS in-house development
Cryogenic Cryojet5 120 to 450K (shared instrument) Oxford
Detector Punctual Cyberstarx1000 φ=30mm, Ti-doped NaI (NaI(TI)), 106
Detector Linear Mythen 1k Total 1280 pixel with 50 µm each, 2kHz frame rate (shared instrument) Dectris
Detector Linear Mythen 1k Total 1280 pixel with 50 µm each, 2kHz frame rate (shared instrument) Dectris
Detector Area Pilatus 100k 172×172 µm2 pixel area, 487×192 pixel matrix Dectris
Detector Area Pilatus 300k 172×172 µm2 pixel area, 487×619 pixel matrix (shared instrument) Dectris
Langmuir trough Liquid surface analysis 602A 62500 mm2, 350 ml, 500mm x 125mm x 3mm Nima

CONTROL AND DATA ACQUISITION

The beamline is controlled by the use of EPICS (Experimental Physics and Industrial Control System) running on a PXI from National Instruments. All data acquisition and instrumentation use are done using Psic mode on SPEC (software for instrumentation control and data acquisition in X-ray diffraction experiments from Certified Science Software). Some graphical interfaces and beamline devices can be controlled on CSS (Control System Studio).

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.

PUBLICATIONS

XRD2

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 at the SAU Online website.


Arias, J. J. R. ;Mota, I. C. ;Albuquerque, L. S. ;Dahmouche, K.;Marques, M. de F. V.. A GIWAXS study of crystallization in annealed conjugated polymers presenting technological interest for organic solar cell applications, Journal of Materials Science-Materials in Electronics, v.33, p.1838–1850, 2022. DOI:10.1007/s10854-021-07383-3


Prakash, D. J. ;Chen, Y.;Debasu, M. L. ;Savage, D. E.;Tangpatjaroen, C. ;Deneke, C. F.;Malachias, A.;Alfieri, A. D. ;Elleuch, O. ;Lekhal, K. ;Szlufarska, I. ;Evans, P. G. ;Cavallo, F.. Reconfiguration of Amorphous Complex Oxides: A Route to a Broad Range of Assembly Phenomena, Hybrid Materials, and Novel Functionalities, Small, v.18, n.1, p.2105424, 2022. DOI:10.1002/smll.202105424


Neckel, I. T.;Silva, F. M. C. da ;Guedes, E. B.;Dias, C. T. dos S. ;Soares, M. M.;Costa, C. A. R.;Mori, T. J. A.;Björling, A. ;Zakharov, A.;Tolentino, H. C. N.. Unveiling Center-Type Topological Defects on Rosettes of Lead Zirconate Titanate Associated to Oxygen Vacancies, Annalen Der Physik, v.534, n.2, p.2100219, 2022. DOI:10.1002/andp.202100219


Salvador, A. J. ;Neckel, I. T.;Graff, I. L.;Mosca, D. H.. Chemical disorder in polycrystalline Ni2MnGa thin films, Journal of Alloys and Compounds, v. 898, p.162970, 2022. DOI:10.1016/j.jallcom.2021.162970


Costa, D. da S.;Kellermann, G.;Craievich, A. F.;Montoro, L. A.;Oliveira, C. K. B. Q. M.;Afonso, C. R. M.;Huck-Iriart, C.;Giovanetti, L. J.;Requejo, F. G.;Zanella, I. G. ;Mazzaro, I.;Szameitat, E. S. ;Cardoso, R. P.. Highly oriented NiSi2@Si thin-nanocomposite produced by solid state diffusion: Morphological and crystallographic characterization, Surfaces and Interfaces, v.29, p.101763, 2022. DOI:10.1016/j.surfin.2022.101763


Faria, M. V. G. ;Soares, E. A.;Antoniazzi, I. ;Paniago, R.M.;Miwa, R. H.;Lopes, J. M. J.;Malachias, A.;Oliveira Jr., M. H.. Experimental evidence of a mixed amorphous-crystalline graphene/SiC interface due to oxygen-intercalation, Surfaces and Interfaces, v.30, p. 101906, 2022. DOI:10.1016/j.surfin.2022.101906