CONTACT & STAFF
For more information on this beamline, contact us.
The XRF beamline is an experimental station dedicated to X-ray Fluorescence Microscopy (XRFM), X-ray Fluorescence Tomography (XFCT) and Total Reflection X-ray Fluorescence (TXRF) analysis in the hard X-rays energy range (5 to 20 keV). The beamline’s focus is on the determination and mapping of trace chemical elements in samples with applications in the fields of analytical chemistry, biomedicine, environmental geochemistry and materials science.
XRF’s source is a 1.67T bending magnet. The monochromator vacuum chamber can be laterally displaced, so that the whole synchrotron spectra can also be used to excite the samples. The experimental facilities include one station consisting of a high vacuum chamber in which grazing incidence x-ray fluorescence experiments can be carried out. The chamber is equipped with remote-controlled XY$\rm \theta$y sample stages and a HPGe solid state detector, optimised for the detection of light element. The whole setup is mounted in the motorised lift table, which allows vertical positioning of the instruments on the plane where the incoming beam is mostly linearly polarized.
Applications include 2D XRF mapping and speciation of trace elements at 20 microns resolution, 3D information of elements in volumetric samples, analysis of very small masses deposited on flat substrate, trace impurities on surfaces of flat samples, chemical depth profiling surface analysis (from sub nm to mm range).
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.
X-ray Fluorescence (XRF) is a well-established bulk analytical method for qualitative as well as quantitative determination of several elements in a sample, independent of their chemical form. Depending on the detection system configuration, can be classified as Energy Dispersive (EDXRF) or Wavelength Dispersive (WDXRF) systems.
Setup: X-ray Fluorescence Microscopy (XRFM)
This setup allows performing experiments with an X-ray microbeam. The microfocusing optics consists of a pair of bendable mirrors arranged in the so called Kirkpatrick-Baez configuration (KB). The X-ray microbeam is around 12 microns (vertical) by 22 microns (horizontal) in size. Fully remote-controlled XYZz sample stages can operate in air or under a nitrogen gas environment. The $\rm \mu$-XRF setup also includes an optical microscope and a Silicon Drift Detector (SSD).
Other setups include:
| Element | Type | Position [m] | Description |
|---|---|---|---|
| SOURCE | Bending Magnet | 0.0 | Bending Magnet D09 exit B (15°), 1.67 T , 0.92 mm x 0.57 mm |
| Mono | Double Crystal Monochromator | 11.2 | Si(111), Si(220), channel-cut type |
| M1 | Elliptical Vertical Micro- focusing Mirror | 14.9 | Rh coated, RT=334m (center), θ=4 mrad |
| M2 | Elliptical Horizontal Microfocusing Mirror | 15.3 | Rh coated, RT=334m (center), θ=4 mrad Rh coated, RT = 176m (center), θ
=4 mrad |
| Parameter | Value | Condition |
|---|---|---|
| Energy range [keV] | 5-20 | Si(111) / Si(220) |
| Energy resolution [ΔE/E] | 10-4 | Si(111) |
| Beam size at sample [µm2, FWHM] | 22 x 12 | at 10 keV |
| Beam divergence at sample [mrad2, FWHM] | 10 x 1 | at 10 keV |
| Flux density at sample [ph/s/mm2/100 mA] | 2 x 108 | at 10 keV |
| Flux density at spot [ph/s/100mA] | 2 x 1012 | White beam |
| Instrument | Type | Model | Manufacturer | Specifications |
|---|---|---|---|---|
| Detector | Silicon drift | AXAS-A | 30 mm2 SDD, FWHM ≤ 139eV at 5.9keV | KETEK GmbH |
| Detector | Silicon drift | AXAS-A | 7 mm2 SDD, FWHM ≤ 139eV at 5.9keV | KETEK GmbH |
| Detector | HPGe | GUL0035 | 30 mm2 Ultra-LGe, FWHM = 140 eV at 5.9keV | Canberra |
| Cryostat | Cryostream Cooler | 700 Series | Minimum of 173K, with a gas stability of 0.1K | Oxford |
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) are used as a graphical interface to display and control the beamline devices. Point-to-point or continuous scanning (“on-the-fly”) modes of operation can be used for data acquisition in 2D/3D experiments.
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.
PÉREZ, C. A., RADTKE, M., SÁNCHEZ, H. J., TOLENTINO, H., NEUENSCHWANDER, R. T., BARG, W., RUBIO, M., BUENO, M. I. S., RAIMUNDO I. M. & ROHWEDDER, J. J. R., Synchrotron Radiation X-Ray Fluorescence at the LNLS: Beamline Instrumentation and Experiments, X-Ray Spectrometry 28, 320–326 (1999). doi: 10.1002/(SICI)1097-4539(199909/10)28:53.0.CO;2-1
The x-ray fluorescence beamline of the Laboratorio Nacional de Luz S´ıncrotron (LNLS) is described. The main optical component of the beamline is a silicon (111) channel-cut monochromator, which can tune energies between 3 and 14 keV. A general description of two experimental stations is given. Beam characterization was done by measuring experimental parameters such as vertical profile and monochromatic flux. These results show that the photon flux at 8 keV in an area of 20 mm2 is 4.2 × 109 photons s−1. The possibility of achieving fine tuning of energies (high resolution) was confirmed. This paper presents some original results derived from the commissioning of the beamline, such as a comparison of detection limits in different experimental conditions, and a novel mechanical system to align capillaries together with a semi-automatic adjustment procedure. So far, there have been several proposals to perform a variety of experiments at this beamline, covering different fields, such as physics, chemistry, geology and biology.
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.
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
Português: Câmara de vácuo mostrando o arranjo de TXRF.
English:Vacuum chamber showing the TXRF setup.
Português:Porta-amostras do arranjo da microssonda de raios X.
English: Sample holder of the x-ray microprobe setup.
Português: Cabana experimental.
English: Experimental hutch
Português: Cabana experimental
English: Experimental hutch
Português: Montagem de amostra no arranjo da microssonda de raios X.
English: Sample mounting on the x-ray microprobe setup.
Português:Instalação de suporte para usuários.
English:User support facility.
Português: Sala de controle da linha.
English: Beamline control room.