ID09 - MS/XPD (Materials Science/X-ray Powder Diffraction) beamline

Welcome to the Materials Science/X-ray Powder Diffraction (MS/XPD) beamline at SESAME.

The MS/XPD beamline is based on components previously installed at the Swiss Light Source donated to SESAME by the Paul Scherrer Institute. It is used for X-Ray Powder Diffraction (XRPD) applications. Its flexible optical design spans a wide energy range of the order of 5 to 25 keV. A two-circle goniometer installed in the experimental hutch accommodates standard XRPD experiments.

At the MS/XPD beamline, The XRPD technique may be applied to material phase identification, quantitative analysis, atomic structural determinations, the characterization of a material’s microstructural properties such as structure imperfections or, domain size, and kinetic studies. 

This beamline, which has been hosting users since December 2020, may be used in a wide range of research fields stretching from materials science and engineering to chemistry, physics, and archeometry.

Information for users

Please cite the following reference paper in all publications that include in any part data obtained at the MS/XPD beamline. The reference papers to be cited in your papers following measurements at the MS/XPD beamline are:

• “Operational status of the X-ray powder diffraction beam­line at the SESAME synchrotron” 
  M. Abdellatief, M. A. Najdawi, Y. Momani, B. Aljamal, A. Abbadi, M. Harfouche and G. Paolucci J. Synchrotron Rad. (2022). 29. doi.org/10.1107/S1600577521012820
  
  or
• “The SESAME materials science beamline for XRD applications” 
  M Abdellatief, L Rebuffi, H Khosroabadi, M Najdawi, T Abu-Hanieh, M Attal, G Paolucci. Powder Diffraction Journal, Vol. 32 - S1, pp. S6-S12 (2017). doi: 10.1017/S0885715617000021

Source

MS/XPD is based on a wiggler source operated at 12 mm magnetic gap equivalent to 1.38 T. the flux produced from the wiggler is high compared to a bending magnet source. The main components of the front end are

1. Fixed mask for defining the beamline acceptance angles
2. Photon shutter to stop the photon beam whenever necessary 
3. Rotating filter 
4. White beam slits
5. Radiation stopper

Optical Layout

The MS/XPD beamline optical layout consist of a cylindrically collimated Rhodium coated mirror fixed aligned to 3 m rad grazing angle. Then Kozhu Si (111) double-crystal fixed exit monochromator is located to select the energy, with second sagittal crystal to focus the beam horizontally at the sample location. Then a second cylindrical Rhodium coated mirror to focus the beam vertically.

Experimental station

The MS/XPD experimental station is based on a refurbished two circle diffractometer previously was installed at I19 beamline at Diamond synchrotron. The inner rotary (theta) is for the sample rotation while the second rotary (2theta) is for the detector rotation. A homemade spinner for transmission experiments is fixed on a translational XY stage attached on the theta rotary. 

Pilatus 300K detector (donated by DECTRIS company) is the main detector in use at MS/XPD end station, it has a very good time resolution together with a reasonable angular resolution gained by fixing the detector at 740 mm distance from the sample.

Heating and cooling samples in capillaries are possible at MS/XPD using a hot gas blower and liquid nitrogen cryostat respectively, moreover further sample environmental stages can be added to the experimental station.

W61

DCM

Collimating Mirror

Refocusing Mirror

Diffractometer

Sample

Techniques usage

Sample Environment

Sample Holders

Dectris Pilatus 300K

Detection

• Powder samples filled in glass capillaries (Boro Silicate for room temperature; Quartz for temperature dependent)
• Capillary spinner 
• Gas blower for temperature dependent experiments (RT – 1000 C)
• Liquid nitrogen cryostat (to be ready soon)

• Output data type as (2D images , Ascii (xy) files)
• PDF-4 database 
• “Match!” software for phase matching analysis is available
• Several refinement software for structural analysis (e.g. GSAS-II, Fullprof)

An analytical calibration procedure to convert 2D TIFF images to Ascii(xy) files is used through a macro script of ImageJ software. Then a simple executable Python-based code is then used to merge all data files for each experiment to create one merged file (Zubi & Abdellatief, 2021: https://github.com/SESAME-Synchrotron/2thetaFilesMerger).
 

2023 (1), 2022 (5), 2021 (1), 2017 (1), All (8)

2023

1. Functionality-Induced Locking of Zeolitic Imidazolate Frameworks
   Chem. Mater., Vol. , pp. (2023)
   T. Xu, B. Zhou, Y. Tao, Z. Shi, W. Jiang, M. Abdellatief, KE. Cordova, Y. Zhang
   doi: 10.1021/acs.chemmater.2c02832
   
   

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1. Zeolite NPO-Type Azolate Frameworks
   Angewandte Chemie International Edition, Vol. n/a - n/a, pp. e202207467 (2022)
   X Zha, X Li, AA Al-Omari, S Liu, C Liang, A Al-Ghourani, M Abdellatief, J Yang, HL Nguyen, B Al-Maythalony, Z Shi, KE Cordova, Y Zhang
   doi: 10.1002/anie.202207467
   
   
2. Hydrogen adsorption on Co2+ - and Ni2+- exchanged -US-Y and -ZSM-5. A combined sorption, DR UV-Vis, synchrotron XRD and DFT study
   International Journal of Hydrogen Energy, Vol. , pp. (2022)
   N. Sarohan, M.O. Ozbek, Y. Kaya, M. Abdellatief, B. Ipek
   doi: 10.1016/j.ijhydene.2022.07.130
   
   
3. Operational status of the X-ray powder diffraction beamline at the SESAME synchrotron
   Journal of Synchrotron Radiation, Vol. 29, pp. (2022)
   M. Abdellatief, M. A. Najdawi, Y. Momani, B. Aljamal, A. Abbadi, M. Harfouche, G. Paolucci
   doi: 10.1107/S1600577521012820
   
   
4. Effect of vanadium and tungsten doping on the structural, optical, and electronic characteristics of TiO2 nanoparticles
   Journal of Materials Science, Vol. , pp. (2022)
   Z.K. Heiba, M. B.Mohamed, A. Badawi, M. Abdellatief
   doi: 10.1007/s10854-022-08027-w
   
   
5. Environmentally adaptive MOF-based device enables continuous self-optimizing atmospheric water harvesting
   Nature Communications, Vol. 13 - 1, pp. 4873 (2022)
   H.A. Almassad, R.I. Abaza, L. Siwwan, B. Al-Maythalony, K.E. Cordova
   doi: 10.1038/s41467-022-32642-0
   
   

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1. Robust Barium Phosphate Metal Organic Frameworks Synthesized under Aqueous Conditions
   ACS Materials Lett., Vol. , pp. 1010-1015 (2021)
   K.A. Salmeia, S. Dolabella, D. Parida, T.J. Frankcombe, A.T. Afaneh, K.E. Cordova, B. Al-Maythalony, S. Zhao, R. Civioc, A. Marashdeh, B. Spingler, R. Frison, A. Neels
   doi: 10.1021/acsmaterialslett.1c00275
   
   

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1. The SESAME materials science beamline for XRD applications
   Powder Diffraction, Vol. 32 - S1, pp. S6-S12 (2017)
   M Abdellatief, L Rebuffi, H Khosroabadi, M Najdawi, T Abu-Hanieh, M Attal, G Paolucci
   doi: 10.1017/S0885715617000021
   
   

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Mahmoud ABDELLATIEF
MS/XPD Beamline Principal Scientist
Email: mahmoud.abdellatief@sesame.org.jo
Work Tel: +962 5 351 1348  (Ext. 275)

Philipp HANS
MS/XPD Beamline Scientist
Email: philipp.hans@sesame.org.jo
Work Tel: +962 5 351 1348  (Ext. 276)