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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.

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.

  • 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

ElementTypePosition [m]Description
SRCBending Magnet0.000Bending Magnet D10 exit A (4°), 1.67T, 0.87mm x 0.17mm
FEFront-end4.750-
S1White Beam Slits5.995-
M1Cylindrical Vertical Focusing Mirror7.048Rh coated, RT=?, $ \theta$ = 20mrad
DCMDouble Crystal Monochromator8.749Water-cooled Si (111), Sagitally bent
S2Monochromatic Beam Slits14.690-
S3Sample Slits17.100-
ESExperimental Station17.478-

PARAMETERS

ParameterValueCondition
Energy range [keV]5-15-
Energy resolution [$ \Delta$E/E]$ 8 \times 10^{-4}$-
Beam size at sample [$ \rm mm^{2}$, FWHM]0.5x1.58 keV, vertical and horizontal focus at sample
Beam divergence at sample [$ \rm mrad^{2}$, FWHM]0.6x58 keV, vertical and horizontal focus at sample
Flux density at sample [ph/s/$ \rm mm^{2}$/100mA]$ 5.26 \times 10^{10}$8 keV at sample

INSTRUMENTATION

InstrumentTypeModelManufacturerSpecifications
Diffractometer6+2 circlesHuber 92784Circles: 4 sample (open eulerian cradle); 2 detector; +2 crystal analyzer; +1 incident angle ($ \pm$ 5°) Huber
Furnaces-F300C300 to 570K Temp. Rate: up to 20K/min Temp. control: 0.1KLNLS in-house development
Furnaces-F1000300 to 1270K Temp. Rate: up to 20K/min Temp. control: 1KLNLS in-house development
Cryogenic-Cryojet5120 to 450K (shared instrument)Oxford
DetectorPunctualCyberstarx1000$ \phi$=30mm, Ti-doped NaI (NaI(TI)), $ 10^6$-
DetectorLinearMythen 1kTotal 1280 pixel with $ 50 \mu m$ each, 2kHz frame rate (shared instrument)Dectris
DetectorLinearMythen 1kTotal 1280 pixel with $ 50 \mu \rm m$ each, 2kHz frame rate (shared instrument)Dectris
DetectorAreaPilatus 100k172x172 $ \mu \rm m^{2}$ pixel area, 487x192 pixel matrixDectris
DetectorAreaPilatus 300k172x172 $ \mu \rm m^{2}$ pixel area, 487x619 pixel matrix (shared instrument)Dectris
Langmuir troughLiquid surface analysis602A62500 $ \rm mm^{2}$, 350 ml, 500mm x 125mm x 3mmNima

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 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 and Innovations (MCTI). The _ _ _ beamline staff is acknowledged for the assistance during the experiments.

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.


Martins, F. H.; Paula, F. L. O.; Gomes, R. C.; Gomes, J. A.; Aquino, R.; Porcher, F.; Perzynski, R.; Depeyrot, J.. Local Structure Investigation of Core-Shell CoFe2O4@gamma-Fe2O3 Nanoparticles, Brazilian Journal of Physics, v.51, p. 47–59, 2021. DOI:10.1007/s13538-020-00829-9


Silva, L. F. da; Catto, A. C.; Bernardini, S.; Fiorido, T.; Palma, J. V. N. de ; Avansi Jr., W.; Aguir, K.; Bendahan, M.. BTEX gas sensor based on hematite microrhombuses, Sensors and Actuators B-Chemical, v. 326, p. 128817, 2020. DOI:10.1016/j.snb.2020.128817


Pereira, M. O.; Felix, V. de S. ; Oliveira-Carvalho, A. L.; Ferreira, D. S. R.; PImenta, A. R. ; Carvalho, C. S.; Silva, F. L. e; Pérez, C. A.; Galante, D.; Freitas, R. P. de. Investigating counterfeiting of an artwork by XRF, SEM-EDS, FTIR and synchrotron radiation induced MA-XRF at LNLS-BRAZIL, Spectrochimica Acta Part A-Molecular and Biomolecular Spectroscopy, v. 246, p. 118925, 2021. DOI:10.1016/j.saa.2020.118925


Lopes, N. A. ; Mertins, O.; Pinilla, C. M. B. ; Brandelli, A.. Nisin induces lamellar to cubic liquid-crystalline transition in pectin and polygalacturonic acid liposomes, Food Hydrocolloids, v. 112, p.106320, 2021. DOI:10.1016/j.foodhyd.2020.106320


Coura, R, L. C. ; Andrade, A. B.; Monteiro, T. de J.; Novais, S. M. V.; Macedo, Z. S.; Valerio, M. E. G.. Photoluminescent properties of BaF2 scintillator-polystyrene composite films under vacuum ultraviolet radiation, Materials Research Bulletin, v.135, p. 111159, 2021. DOI:10.1016/j.materresbull.2020.111159


Moreno, H.; Cortes, J. A. ; Praxedes, F. M. ; Freitas, S. M. de; Rezende, M. V. dos S.; Simões, A. Z. ; Teixeira, V. C.; Ramírez, M. A.. Tunable photoluminescence of CaCu3Ti4O12 based ceramics modified with tungsten, Journal of Alloys and Compounds, v.850, p. 156652, 2021. DOI:10.1016/j.jallcom.2020.156652


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