I09 - MS (Materials Science) beamline

Tab

MS

Welcome to the power diffraction beamline at SESAME

The SESAME MS 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.

The XRPD technique of the MS beamline may be applied to material phase identification, quantitative analysis, atomic structural determinations, and the characterization of material microstructural properties such as structure imperfections, domain size determination, 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.

Source

MS 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
Flux produced by MS wiggler

Flux produced by MS wiggler

 

Optical Layout

The MS 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.

 

MS beamline layout

MS beamline layout

 

 

Beam focused at the sample location

Beam focused at the sample location

 

 

Experimental station

The MS 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 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 using hot gas blower and liquid nitrogen cryostat respectively, moreover further sample environmental stages can be added the experimental station.

 

the MS diffractometer

the MS diffractometer

 

 

Instrumental resolution at MS obtained by NIST Si (640 f) standard
​​​​​Instrumental resolution at MS obtained by NIST Si (640 f) standard

 

Beamline Energy Resolution
2 [eV] @ 10000 [eV]
Beamline Energy Range
5 - 25 [keV]
Max Flux On Sample
1 * 1013 [ph/s] @ 10 [keV]

W61

Type
Wiggler
Deflection Parameter K
7.8
Total Power
6 * 103 [W]
Number Of Periods
33
Period
60.5 [mm]

DCM

Energy Range
5 - 25 [keV]
Type
Si(111) Double Crystal Monochromator with sagittaly bent 2nd crystal.

Collimating Mirror

Description
Rh coated, 1.0 mt long cylindrical mirror, Dynamically Bended to 5-11 km radius
optical surface facing up

Refocusing Mirror

Description
Rh coated, 1.0 mt long cylindrical mirror, Dynamically Bended to 5-11 km radius
optical surface facing down

Diffractometer

Diffractometer
2-circle diffractometer, with motorised translation stage to align the capillary to the spinner.
Detectors Available
Dectris Pilatus 300K

Sample

Sample Type
Powder
Mounting Type
Capillary

Techniques usage

Diffraction / Powder diffraction
Transmission mode with sample in capillary.

Sample Environment

Temperature
300 - 1300 [K]

Sample Holders

Description
500 rpm

Dectris Pilatus 300K

Type
Si 2D pixel detector
Pixel Size
X = 172 [um], Y = 172 [um]
Array Size
X = 487 [pixel], Y = 619 [pixel]
Thickness
450 [um]
Passive or Active (Electronics)
Active
Dynamic Range
2 * 106 [counts/s]

Detection

Detected Particle
Photon

  • 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 

  • Output data type as 2D images
  • DAWN software for image processing to convert 2D to Ascii (xy) files
  • Phase software for phase matching analysis is available
  • PDF-4 database 
  • GSAS software for structural analysis
  • FullProf software for structural analysis

2021

  1. Robust Barium Phosphonate 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


2017
  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


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