D08 - XAFS/XRF (X-ray Absorption Fine Structure/X-ray Fluorescence) spectroscopy beamline

Tab

XAFS

Welcome to the XAFS/XRF beamline at SESAME

XAFS/XRF is a beamline dedicated to X-ray Absorption Spectroscopy. It is built on the bending magnet at the eighth cell of the SESAME storage ring (D08) and allows access to a wide energy range: from 4.7 to 30 keV, with high photon flux (109-1012 ph/s) and high beam stability. This meets the needs of a large number of researchers.

The XAFS/XRF beamline is designed for X-ray spectroscopic studies in all fields of science.

The monochromatic X-ray beam of XAFS/XRF, combined with the highly-sensitive 64 element silicon drift detector, and the ionization chambers and motorized stages for sample and detector movements offers the synergistic application of X-Ray Absorption and Fluorescence Spectroscopy for multidisciplinary applications.

This instrument, which has been hosting users since July 2018, may be used in numerous fields of research among which: environmental science, energy storage, cultural heritage, and catalysis, as well as solid state physics and bio-chemistry. 

Beamline Optical Layout

The XAFS/XRF beamline is located at the bending-magnet port D08 of the SESAME storage ring. The beamline optics uses horizontally a fan of 3.0 mrad of synchrotron radiation of the SESAME bending magnet (1.45 T magnetic field with a critical energy 6.05 keV). 

 

XAFS/XRF beamline - General view
XAFS/XRF beamline - General view

 

Front End

The first beamline element, after the photon shatter, is a water-cooled fixed mask, which defines the acceptance of the beam line (3.0 mrad horizontally and 0.6 mrad vertically) and reduces the heat load on the optical components by cutting off the off-axis radiation. This mask is followed by a pair of water-cooled white beam slits to define the primary beam size and a water-cooled copper rod equipped with three filters of different thickness for heat management. The beamline vacuum is separated from the ring vacuum by a CVD window (250 µm thickness). To further protect the storage ring vacuum from ruptures of the beam line vacuum a fast closing shutter is installed in the front-end section. Its sensor is placed just before the CVD window in the optical hutch. 

Beamline Optics 

The main elements are a fixed-exit double-crystal monochromator (DCM) located between a collimating and focusing cylindrically bent mirrors installed before and after the monochromator, respectively; each of the mirrors is double coated Si and Pt. The primary water-cooled slits are located at 12.8 m from the source after the fixed, they define the horizontal and vertical dimensions of the polychromatic beam impinging the collimating mirror (VCM, first mirror). diagnostic tools are installed after each major component such as beam position wire monitors located after the VCM and DCM and an x-ray sensitive screen that can be inserted just after the vertically focusing mirror (VFM, second mirror). Both mirrors are tilted to grazing angles (~ 2.8 mrad) in order to optimize simultaneously the angular acceptance of the incoming beam and the mirror reflectivity. Finally, a monochromatic shutter is installed at the end of the hutch for allowing the experimenter to access experimental hutches while keeping a constant heat load on the optics.

 

Top view of the beamline optics
Top view of the beamline optics

 

Mirrors reflectivity at 2.8 mrad incident beam angle for Pt and Si coating for the Si coating so that the Pt L edges artifacts in the beam are covered
Mirrors reflectivity at 2.8 mrad incident beam angle for Pt and Si coating
for the Si coating so that the Pt L edges artifacts in the beam are covered

 

Sample manipulator

Sample manipulator

Experimental Station (End Station)

An optical table with 6-axis of freedom is used as support for different detectors (ICs, XRF detectors) as well as the support for some sample manipulator and other sample environment devises.

The standard sample manipulator consists of several modules including a horizontal and vertical translation stages as well as rotational stages covering 360° in addition to swivelling stage. The manipulator can take up to 10kg load and allow the installation and alignment of most in-situ experimental setups.

 

 

Detectors and experimental setup:

XAFS data can be collected in both transmission and fluorescence mode:

  • Transmission mode:
    3 ionization chambers are used. Two ICs (15 cm) are used downstream and upstream the sample for recording I0 and It and a third one (30 cm) used for recording the reference.
  • Fluorescence mode:
    Two detectors are available for use in fluorescence mode:

    Multi-element SDD state-of-the-art and unique fluorescence detector developed by INFN for samples with extreme low content (down to few ppm)

    • 64 elements
    • High count rate (~15 M cts/s)
    • Higher efficiency (low deadtime)

    •  
    Single element SDD for samples with concentration (>100 ppm)

    • 1 element D-XAS Ketek 
    • “DXP-Mercury” electronics from XIA
    • ICR (~1 Mcts/s)​​​​​​

    •  
    ​​​​​

 

The experimental setup in transmission and fluorescence mode for XAFS data acquisition

The experimental setup in transmission and fluorescence mode for XAFS data acquisition

     

    Sample Environment

    LN2 Cryojet for cooling sample (~95 K)
     
     LN2 Cryojet for cooling sample (~95 K)
    • LN2 Cryojet to cool down the sample to a temperature of about 95 K.
    • Users can bring their own equipment for in-situ experiment (Cell, furnace, etc.) can be adapted to the beamline experimental station. 
      • Please note that the spatial resolution of the bam on sample doesn´t allow any experiment with small beam such as high-pressure using diamond cells or elemental XRF mapping. 
    • All forms of samples are accepted whether solid (bulk or powder), liquid and/or gas. If holders do not exist yet at the beamline, they can be fabricated at the SESAME workshop.

    Users are reminded that they should contact the XRF/XAFS beamline scientists when drafting their proposal to discuss the sample environments and beamline characteristcs.

     

     

    Beamline Energy Range
    4.7 - 30 [keV]
    Max Flux On Sample
    5 * 1011 [ph/s] @ 8 [keV]
    Spot Size On Sample Hor
    1 - 20 [mm]
    Spot Size On Sample Vert
    1 - 5 [mm]

    Bending Magnet (D08)

    Type
    Bending Magnet
    Source Divergence Sigma
    X = 266.6 [urad], Y = 11.5 [urad]
    Source Size Sigma
    X = 232.3 [um], Y = 81 [um]

    DCM - Si(111)

    Energy Range
    4.7 - 30 [keV]
    Type
    Fixed Exit Beam
    Resolving Power
    1 * 10-4 [deltaE/E]

    DCM - Si(311)

    Energy Range
    4.7 - 30 [keV]
    Type
    Fixed Exit Beam
    Resolving Power
    5 * 10-5 [deltaE/E]

    VCM

    Description
    Vertical Collimating Mirror

    Dimensions (mm): 1200 x 70
    Active area (mm): 1000 x 70
    Coatings : Double coating Si and Pt
    Angle of incidence (mrad) : 2.8 (can vary)
    Substrate: Silicon single crystal
    Cooling: Water cooled
    Flatness: Cylindrical
    Type of bender: Pneumatic
    Minimum radius (km): 5.3

    VFM

    Description
    Vertical Focusing Mirror

    Dimensions (mm): 1200 x 70
    Active area (mm): 1000 x 70
    Coatings : Double coating Si and Pt
    Angle of incidence (mrad) : Variable
    Substrate: ZERODUR
    Cooling: Uncooled
    Flatness: Cylindrical
    Type of bender: Pneumatic
    Minimum radius (km): 5.3

    End Station

    Description
    The experimental station is equipped with an optical table with 6 axis of freedom and used as support for different detectors (ICs, XRF detectors) as well as for the sample manipulator and other sample environmental devises.
    Endstation Operative
    Yes

    Sample

    Sample Type
    Crystal, Amorphous, Powder, Gel, Liquid, Gas

    Techniques usage

    Absorption / EXAFS
    XAFS data can be collected in Transmission and Fluorescence mode

    INFN (Multi SDD)

    Type
    A Multi Silicon Drift Detector (64 SDDs)
    Description
    Fluorescence Detector based on 64 SDDs
    Operating temperature range: +24 to -45 °C
    Signal output: Low noise preamplifier
    sensitive area: 9 mm2 per SDD
    Total collimated sensitive area: : 499 mm2
    Resolution (FWHM) @5.9keV: < 150 eV (1Mcps with 1.6 μs pt)
    Sampling rate: up to 15 Mcps
    Output Readout Software
    FICUS (developed by INFN, Elettra, SESAME)

    Detection

    Detected Particle
    Photon

    Ketek (Singl El. SDD)

    Type
    AXAS-D VITUS SDD (Single Element)
    Description
    Operating temperature range: 0 to +50°C
    Signal output: Low noise preamplifier
    Peaking time range: 0.1 to 24 μs in 24 steps
    Active Area: 20 mm2
    Resolution (FWHM) @5.9keV - 125 eV (100 Kcps with 2 μs picking time)
    Output Readout Software
    EPICS based MEDM with Graphical User Interface

    Detection

    Detected Particle
    Photon

    • Sample Type: Crystal, Amorphous, Powder, Gel and Liquid.
    • A modest set of tools for sample preparation can be used to prepare samples such as spatulas, balance, mortars, hydraulic press for pallets (12 mm dies), binders, etc. 

     

    sample

    Fig. - Different tools for sample preparation

     

    • Users are offered the help to calculate the thickness of the samples and to prepare pallets.
    • Data are collected using a home developed (Python based) software.
    • XAFS (XANES & EXAFS) data are saved in an ASCII format.
    • XRF data are saved in JSON, CSV or HDF5 formats.

    Many software can be used for Software for XAFS and XRF data analyses. Available on beamline platform are:

    2021

    1. Investigating Local Structure of Ion-Implanted (Ni2+) and Thermally Annealed Rock Salt CoO Film by EXAFS Simulation Using Evolutionary Algorithm
      ACS Appl. Energy Mater., Vol. , pp. (2021)
      LU Khan, N Jabeen, I Jabbar, S Jamil, A Kanwal, Z Akhter, M Usman, MZ Abid, M Harfouche
      doi: 10.1021/acsaem.0c02676

    2. Synthesis and Comparative Evaluation of Optical and Electrochemical Properties of Efficacious Heterostructured-Nanocatalysts of ZnSe with Commercial and Reduced Titania
      Journal of Alloys and Compounds, Vol. , pp. 160449 (2021)
      S Jamil, N Jabeen, LU Khan, A Bashir, N Janjua, M Harfouche, M Sohail, AH Siddique, A Iqbal, N Qadeer, Z Akhter
      doi: 10.1016/j.jallcom.2021.160449

    3. Geochemical changes of Mn in contaminated agricultural soils nearby historical mine tailings: Insights from XAS, XRD and, SEP
      Chemical Geology, Vol. , pp. 120217 (2021)
      A Morales-Perez, V Moreno-Rodriguez, RD Rio-Salas, NG Imam, B Gonzalez-Mendez, T Pi-Puig, F Molina-Freaner, R Loredo-Portales
      doi: 10.1016/j.chemgeo.2021.120217

    4. The significance of the local structure of cobalt-based catalysts on the photoelectrochemical water oxidation activity of BiVO4
      Electrochimica Acta, Vol. 366, pp. 137467 (2021)
      M Barzgar Vishlaghi, A Kahraman, S Apaydin, E Usman, D Aksoy, T Balkan, S Munir, M Harfouche, H Ogasawara, S Kaya
      doi: 10.1016/j.electacta.2020.137467

    5. Magnetic Properties and Environmental Temperature Effects on Battery Performance of Na0.67Mn0.5Fe0.5O2
      Energy Technology, Vol. n/a - n/a, pp. 2001130 (2021)
      S Altin, A Bayri, E Altin, E Oz, S Yasar, S AltundaAY, M Harfouche, S Avci
      doi: 10.1002/ente.202001130

    6. Synchrotron XANES and EXAFS evidences for Cr+6 and V+5 reduction within the oil shale ashes through mixing with natural additives and hydration process
      Heliyon, Vol. 7 - 4, pp. e06769 (2021)
      T. El-Hasan, M. Harfouche, A. Aldrabee, N. Abdelhadi, N. Abu-Jaber, G. Aquilanti
      doi: 10..1016/j.heliyon.2021.e06769

    7. Carbide-Supported PtRu Catalysts for Hydrogen Oxidation Reaction in Alkaline Electrolyte
      ACS Catal., Vol. 11 - 2, pp. 932-947 (2021)
      ER Hamo, RK Singh, JC Douglin, S Chen, MB Hassine, E Carbo-Argibay, S Lu, H Wang, PJ Ferreira, BA Rosen, DR Dekel
      doi: 10.1021/acscatal.0c03973

    8. Synchrotron X-ray fluorescence and X-ray absorption near edge structure of low concentration arsenic in ambient air particulates
      J. Anal. At. Spectrom., Vol. , pp. (2021)
      A.A. Shaltout, M. Harfouche, F.A.S. Hassan, D. Eichert
      doi: 10.1039/D0JA00504E

    9. Study on crystallographic and electronic structure of micrometre-scale ZnO and ZnO:B rods via X-ray absorption fine-structure spectroscopy
      Journal of Synchrotron Radiation, Vol. 28, pp. 448-454 (2021)
      S. Erat, O.M. Ozkendir, S. Yildirimcan, S. Gunaydin, M. Harfouche, B. Demir, A. Braun
      doi: 10.1107/S1600577520015866


    2020
    1. Local lattice relaxation around Tl substitutional impurities in a NaI(Tl) scintillator crystal
      Radiation Physics and Chemistry, Vol. , pp. (2020)
      A. Filipponi, G. Profeta, N. Di Marco, V. Zema, K. Schaffner, F. Reindl, H. Messaoud, A. Trapananti, A. Di Cicco
      doi: 10.1016/j.radphyschem.2020.108992

    2. An investigation of the improvement in energy storage performance of Na2/3Mn1/2Fe1/2O2 by systematic Al-substitution
      Journal of Materials Science: Materials in Electronics, Vol. 31 - 17, pp. 14784-14794 (2020)
      S Altin, S AltundaAY, E Altin, M Harfouche, A Bayri
      doi: 10.1007/s10854-020-04042-x

    3. Electronic structure and electrochemical analysis of the Li2Mn1-xSexO3 materials on April 02, 2020.
      Solid State Ionics, Vol. 349, pp. 115299 (2020)
      O.M. Ozkendir, G. Celik, S. Ates, S. Aktas, S. Gunaydin, M. Harfouche, F. Bondino, E. Magnano, H. Baveghar, I. Ulfat
      doi: 10.1016/j.ssi.2020.115299

    4. An investigation of Ti-substitution effects of Na0.67Mn0.5Fe0.5O2 battery cells for structural and electrochemical properties
      International Journal of Energy Research, Vol. , pp. (2020)
      S Altin, S AltundaAY, E Altin, E Oz, M Harfouche, A Bayri
      doi: 10.1002/er.5820

    5. Highly efficient 3D-ZnO nanosheet photoelectrodes for solar-driven water splitting: Chalcogenide nanoparticle sensitization and mathematical modeling
      Journal of Alloys and Compounds, Vol. 828, pp. 154472 (2020)
      CT Altaf, M Faraji, A Kumtepe, N Abdullayeva, N Yilmaz, E Karagoz, A Bozbey, H Kurt, M Sankir, ND Sankir
      doi: 10.1016/j.jallcom.2020.154472

    6. LiNi0.8Co0.15Ti0.05O2: synthesis by solid state reaction and investigation of structural and electrochemical properties with enhanced battery performance
      Journal of Materials Science: Materials in Electronics, Vol. , pp. (2020)
      A Bayri, E Gocer, E Altin, S Altundag, E Oz, M Harfouche, S Altin, S Avci
      doi: 10.1007/s10854-020-04572-4


    2019
    1. Lyotropic Liquid Crystalline Mesophases Made of Salt-Acid-Surfactant Systems for the Synthesis of Novel Mesoporous Lithium Metal Phosphates
      ChemPlusChem, Vol. 84, pp. 1-11 (2019)
      I. Uzunok, J. Kim, T. O. Colak, D. S. Kim, H. Kim, M. Kim, Y. Yamauchi, O. Dag
      doi: 10.1002/cplu.201900435

    2. Synthesis and water oxidation electrocatalytic and electrochromic behaviours of mesoporous nickel oxide thin film electrodes
      Journal of Materials Chemistry A, Vol. 7 - 38, pp. 22012-22020 (2019)
      A. Amirzhanova, I. Karakaya, C. B. Uzundal, G. Karaoglu, F. Karadas, O. Dag
      doi: 10.1039/c9ta07693j

    3. Exceptionally active and stable catalysts for CO2 reforming of glycerol to syngas
      Applied Catalysis B: Environmental, Vol. 256 - 117808, pp. (2019)
      S. Bac, Z. Say, Y. Kocak, K.E. Ercan, M. Harfouche, E. Ozensoy, A.K. Avci
      doi: 10.1016/j.apcatb.2019.117808

    4. Boron activity in the inactive Li2MnO3 cathode material
      Journal of Electron Spectroscopy and Related Phenomena, Vol. 235, pp. 23-28 (2019)
      O.M. Ozkendir, M. Harfouche, I. Ulfat, C. Kaya, G. Celik, S. Ates, S. Aktas, H. Bavigar, T. Colak
      doi: 10.1016/j.elspec.2019.06.011


    Messaoud HARFOUCHE
    XAFS/XRF Beamline Senior Scientist
    Email: Messaoud.Harfouche@sesame.org.jo
    Work Tel: +962 5 351 1348  (Ext. 303)

    Latif Ullah KHAN
    XAFS/XRF Beamline Scientist
    Email: latifullah.khan@sesame.org.jo
    Work Tel: +962 5 3511348  (Ext 347)