BM08 - XAFS/XRF (X-ray Absorption Fine Structure/X-ray Fluorescence) spectroscopy beamline

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 (BM08) 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 BM08 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). 

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.

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)​​​​​​
  
   

Sample Environment

• 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.

Bending Magnet (D08)

DCM - Si(111)

DCM - Si(311)

VCM

VFM

End Station

Sample

Techniques usage

INFN (Multi SDD)

Detection

Ketek (Singl El. SDD)

Detection

• 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. 

• 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:

• Demeter (Free Software).
• WinXAS .
• FEFF6, FEFF7 (Free Software).
• PyMca (Free Software).

2023 (9), 2022 (10), 2021 (11), 2020 (6), 2019 (4), All (40), Thesis (1)

2023

1. Optimizing the electrochemical activity and understanding the reaction mechanism of Li3.27FeII0.19FeIII0.81V(PO4)3 cathode material for lithium-ion batteries
   Journal of Power Sources, Vol. 575, pp. 233190 (2023)
   H. Aziam, A. Mahmoud, D. Mikhailova, M. Harfouche, I. Saadoune, H. Ben Youcef
   doi: 10.1016/j.jpowsour.2023.233190
   
   
2. Strategy to Probe the Local Atomic Structure of Luminescent Rare Earth Complexes by X-ray Absorption Near-Edge Spectroscopy Simulation Using a Machine Learning-Based PyFitIt Approach
   Inorg. Chem., Vol. 00 - 00, pp. 0000-0000 (2023)
   L.U. Khan, Z.U. Khan, L. Blois, L. Tabassam, H.F. Brito, S.J.A. Figueroa
   doi: 10.1021/acs.inorgchem.2c03850
   
   
3. Colloidal Quantum Dots as an Emerging Vast Platform and Versatile Sensitizer for Singlet Molecular Oxygen Generation
   ACS Omega, Vol. 00, pp. 0000-0000 (2023)
   Z.U. Khan, L.U. Khan, H.F. Brito, M. Gidlund, O.L. Malta, P. Di Mascio
   doi: 10.1021/acsomega.3c03962
   
   
4. SYNCHROTRON-BASED X-RAY FLUORESCENCE ANALYSIS OF BYZANTINE PLASTER FIGURINES FROM JORDAN MUSEUM
   Mediterranean Archaeology and Archaeometry, Vol. 23 - 1, pp. 199-208 (2023)
   S. Al Khasawneh, K. Khasawneh, A. Aldrabee, M. Harfouche
   doi: 10.5281/zenodo.7775790
   
   
5. L-shell x-ray fluorescence relative intensities for elements with 62
   Chinese Physics B, Vol. 32 - 8, pp. 083201 (2023)
   M. Alqadi, S. Al-Humaidi, H. Alkhateeb, F. Alzoubi
   doi: 10.1088/1674-1056/accb46
   
   
6. Local atomic structure order and electrochemical properties of NiO based nano-catalysts for ethanol sensing at room temperature
   Journal of Physics and Chemistry of Solids, Vol. 175, pp. 111201-111211 (2023)
   F Sajid, N Jabeen, LU Khan, M Sohail, A Rehman, Z Akhter
   doi: 10.1016/j.jpcs.2022.111201
   
   
7. Crystal structures, Hirshfeld surfaces, Infrared, and XRF/XAFS studies of Long-chain 2D Lead-free Hybrid Perovskite NH3(CH2)9NH3MCl4 (M = Mn, Co, Cu)
   Journal of Molecular Structure, Vol. 1276, pp. 134757 (2023)
   S.K. Abdel-Aal, M. Harfouche, A. Ouasri, A.S. Abdel-Rahman
   doi: 10.1016/j.molstruc.2022.134757
   
   
8. Singlet Molecular Oxygen Generation via Unexpected Emission Color-Tunable CdSe/ZnS Nanocrystals for Applications in Photodynamic Therapy
   ACS Appl. Nano Mater., Vol. , pp. (2023)
   ZU Khan, LU Khan, MK Uchiyama, FM Prado, RL Faria, IF Costa, S Miyamoto, K Araki, M Gidlund, HF Brito, P Di Mascio
   doi: 10.1021/acsanm.2c05482
   
   
9. Insight into the Local Atomic Structure Order and Luminescence of Rare Earths
   The Nucleus, Vol. 60 - 1, pp. 78-85 (2023)
   L.U. Khan, Z.U. Khan, M.A. Umar
   doi: 10.
   
   

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1. Synthesis and Characterization of a Carbon-Supported Cobalt Nitride Nano-Catalyst
   ChemNanoMat, Vol. 8 - 2, pp. e202100428-17 (2022)
   A Rubab, N Baig, M Sher, M Ali, A Ul-Hamid, N Jabeen, LU Khan, M Sohail
   doi: 10.1002/cnma.202100428
   
   
2. Temperature-Dependent Speciation Analysis of Chromium Immobilized in Calcium Hydroxyapatite Matrix
   International Journal of Environmental Research, Vol. 16 - 4, pp. 40 (2022)
   S Iqbal, Y Faiz, M Harfouche, M Saifullah, J Yun
   doi: 10.2139/ssrn.3926998
   
   
3. Emergence of the first XAFS/XRF beamline in the Middle East: providing studies of elements and their atomic/electronic structure in pluridisciplinary research fields
   Journal of Synchrotron Radiation, Vol. 29 - 4, pp. (2022)
   M Harfouche, M Abdellatief, Y Momani, A Abbadi, M Al Najdawi, M Al Zoubi, B Aljamal, S Matalgah, LU Khan, A Lausi, G Paolucci
   doi: 10.1107/S1600577522005215
   
   
4. Hydrothermal synthesis and characterization of transition metal (Mn/Fe/Cu) co-doped cerium oxide-based nano-additives for potential use in the reduction of exhaust emission from spark ignition engines
   RSC Adv., Vol. 12 - 24, pp. 15564-15574 (2022)
   N Qadeer, N Jabeen, LU Khan, M Sohail, M Zaheer, M Vaqas, A Kanwal, F Sajid, S Qamar, Z Akhter
   doi: 10.1039/D2RA01954J
   
   
5. High Dielectric Transparent Film Tailored by Acceptor and Donor Codoping
   Small, Vol. n/a - n/a, pp. 2107168 (2022)
   D Huang, Y Shi, M Younas, RTA Khan, M Nadeem, K Shati, M Harfouche, U Kentsch, Z Liu, Y Li, S Zhou, A Kuznestov, FC Ling
   doi: 10.1002/smll.202107168
   
   
6. Hierarchical Porous Carbon Nitride-Crumpled Nanosheet-Embedded Copper Single Atoms: An Efficient Catalyst for Carbon Monoxide Oxidation
   ACS Appl. Mater. Interfaces, Vol. 14 - 36, pp. 40749-40760 (2022)
   K. Eid, M.H. Sliem, M. Alejji, A.M. Abdullah, M. Harfouche, R.S. Varma
   doi: 10.1021/acsami.2c06782
   
   
7. Coupling between [gamma]-irradiation and synchrotron-radiation-based XAFS techniques for studying Mn-doped ZnO nanoparticles
   Journal of Synchrotron Radiation, Vol. 29 - 5, pp. (2022)
   NG Imam, M Harfouche, AA Azab, S Solyman
   doi: 10.1107/S1600577522006439
   
   
8. Ag/AgCl Clusters Derived from AgCu Alloy Nanoparticles as Electrocatalyst for Oxygen Reduction Reaction
   Sustainable Energy Fuels, Vol. , pp. (2022)
   T. Balkan, H. Küçükkeçeci, D. Aksoy, M. Harfouche, O. Metin, K. Sarp
   doi: 10.1039/D2SE00472K
   
   
9. Electronic and crystal structure analyses of boron doped LiFeO2 cathode material by the XAFS spectroscopy
   Materials Today Communications, Vol. 31, pp. 103571 (2022)
   S Gunaydin, M Harfouche, OM Ozkendir
   doi: 10.1016/j.mtcomm.2022.103571
   
   
10. Wide visible-range activatable fluorescence ZnSe:Eu3+/Mn2+@ZnS quantum dots: local atomic structure order and application as a nanoprobe for bioimaging
    J. Mater. Chem. B, Vol. 10 - 2, pp. 247-261 (2022)
    ZU Khan, MK Uchiyama, LU Khan, K Araki, H Goto, MCFC Felinto, AO de Souza, HF de Brito, M Gidlund
    doi: 10.1039/D1TB01870A
    
    

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1. 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
   
   
2. Synchrotron X-ray fluorescence and X-ray absorption near edge structure of low concentration arsenic in ambient air particulates
   J. Anal. At. Spectrom., Vol. 36 - 5, pp. 981-992 (2021)
   AA Shaltout, M Harfouche, FAS Hassan, D Eichert
   doi: 10.1039/D0JA00504E
   
   
3. 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
   
   
4. 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
   
   
5. Seed-mediated synthesis and characterization of ZnO-Fe2O3 nanospheres: Building up the core-shell model
   Journal of Crystal Growth, Vol. 572, pp. 126279 (2021)
   S.I. Ahmed
   doi: 10.1016/j.jcrysgro.2021.126279
   
   
6. Synthesis and comparative evaluation of optical and electrochemical properties of Ni+2 and Pr+3 ions co-doped mesoporous TiO2 nanoparticles with undoped Titania
   Applied Nanoscience, Vol. 11 - 9, pp. 2397-2413 (2021)
   A Bashir, U Rafique, R Bashir, S Jamil, F Bashir, M Sultan, M Mubeen, Z Mehmood, A Iqbal, Z Akhter
   doi: 10.1007/s13204-021-02049-2
   
   
7. 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. 4 - 3, pp. 2049-2055 (2021)
   LU Khan, N Jabeen, I Jabbar, S Jamil, A Kanwal, Z Akhter, M Usman, MZ Abid, M Harfouche
   doi: 10.1021/acsaem.0c02676
   
   
8. Magnetic Properties and Environmental Temperature Effects on Battery Performance of Na0.67Mn0.5Fe0.5O2
   Energy Technology, Vol. 9 - 5, pp. 2001130 (2021)
   S. Altin, A. Bayri, E. Altin, E. Oz, S. Yasar, S. AltundaAY, M. Harfouche, S. Avci
   doi: 10.1002/ente.202001130
   
   
9. 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
   
   
10. Geochemical changes of Mn in contaminated agricultural soils nearby historical mine tailings: Insights from XAS, XRD and, SEP
    Chemical Geology, Vol. 573, pp. 120217 (2021)
    A Morales-Pérez, V Moreno-Rodríguez, R Del Rio-Salas, NG Imam, B González-Méndez, T Pi-Puig, F Molina-Freaner, R Loredo-Portales
    doi: 10.1016/j.chemgeo.2021.120217
    
    
11. 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. 879, 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
    
    

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1. Investigation of Ti-substitution effects on structural and electrochemical properties of Na0.67Mn0.5Fe0.5O2 battery cells
   International Journal of Energy Research, Vol. 44 - 14, pp. 11794-11806 (2020)
   S Altin, S Altundag, E Altin, E Oz, M Harfouche, A Bayri
   doi: 10.1002/er.5820
   
   
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. 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. 31 - 22, pp. 20527-20538 (2020)
   A Bayri, E Gocer, E Altin, S Altundag, E Oz, M Harfouche, S Altin, S Avci
   doi: 10.1007/s10854-020-04572-4
   
   
4. Local lattice relaxation around Tl substitutional impurities in a NaI(Tl) scintillator crystal
   Radiation Physics and Chemistry, Vol. 177, pp. 108992 (2020)
   A Filipponi, G Profeta, N Di Marco, V Zema, K Schäffner, F Reindl, M Harfouche, A Trapananti, A Di Cicco
   doi: 10.1016/j.radphyschem.2020.108992
   
   
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. 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
   
   

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1. 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
   
   
2. 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
   
   
3. 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
   
   
4. 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
   
   

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2021

1. Fabrication and Exploration of Efficacious Transition Metal Oxides (TMO) based Nano-catalysts: Headway to Green Energy, (2021)
   S. JAMIL
   
   

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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)