1. BL04 MSPD Materials Science and Powder Diffraction Aleksandr Missiul
Experiments Division CELLS – ALBA
Carrer de la Llum 2-26, 08290, Cerdanyola del Vallès, Barcelona, Spain

2. BL04 MSPD Introduction Description of the beamline Overview PD station2
Introduction
Description of the beamline
Overview
PD station
HP/MD station
Typical experiments
High resolution powder diffraction
High speed powder diffraction
High pressure diffraction
Microdiffraction

3. BL04 MSPD Introduction Description of the beamline Overview PD station3
Introduction
Description of the beamline
Overview
PD station
HP/MD station
Typical experiments
High resolution powder diffraction
High speed powder diffraction
High pressure diffraction
Microdiffraction

4. What is powder diffraction?4
Incident beam
Sample
Diffracted beam
2θhkl
0D detector
1D detector
2D detector
2𝜃 ℎ 1 𝑘 1 𝑙 1
2𝜃 ℎ 2 𝑘 2 𝑙 2
2𝜃 ℎ 3 𝑘 3 𝑙 3
𝐼 ℎ 1 𝑘 1 𝑙 1
𝐼 ℎ 2 𝑘 2 𝑙 2
𝐼 ℎ 3 𝑘 3 𝑙 3
𝐹𝑊𝐻𝑀 ℎ 3 𝑘 3 𝑙 3
Peak position 2θhkl
Bragg law :
λ=2*dhkl*sinθhkl
information on overall periodical arrangement of atoms
Peak intensity Ihkl
Structure factor:
𝐹 ℎ𝑘𝑙 = 𝑗 𝑓 𝑗 exp⁡ −2𝜋𝑖 𝑥 𝑗 ℎ+ 𝑦 𝑗 𝑘+ 𝑧 𝑗 𝑙
type of atom (fj) in material
positions (xj,yj,zj) of atoms in the structure (unit cell)
Peak FWHMhkl
microstructural features (strain, size, stacking faults, …)

5. How do we treat the diffraction data?5
Data
(input)
Rietveld refinement
Model (input/output)
Ab initio
structure solution
Model (output)
More details at the data analysis session tomorrow

6. BL04 MSPD Introduction Description of the beamline Overview PD station6
Introduction
Description of the beamline
Overview
PD station
HP/MD station
Typical experiments
High resolution powder diffraction
High speed powder diffraction
High pressure diffraction
Microdiffraction

7. Description of the beamline7

8. Description of the beamline

9. Powder Diffraction Station
NaCaAlF3, 20keV, Ø0.5 mm
MultiAnalyzerDetector (10 – 50 keV)
13 channels with 1.5 deg pitch
Si111 or Si220 Bragg reflection
YAP scintillator + PMT
Mirror collimating : beam size 3 x 1.5 mm
Full pattern acquisition : 10 min – 2 hours
Scanning speed : (0.5-1°/min)
-> ° angular resolution
Mythen detector (8 – 30 keV)
Si position sensitive detector
6 modules (1280 channels, 50 μm pitch)
ms time resolution
Mirror focusing: beam size 3 x 0.7 mm
Full pattern acquisition :
~ms: 1 position / trigger mode (stroboscopic)
1-5 sec: 1 position, ~40° range
1 – 10 min: 5 positions , ~60° range
~30min: 20 positions, ~130° range (PDF)
-> ~40° in deg pitch > 0.02° angular resolution
YNiO3
º monoclinic distortion

10. Powder Diffraction Station
Sample Environment:
l-He Dynaflow Cryostat: 5K- RT
700 series lN2 cryostream (OxfordCryosystems) 80K – 450 K*)
FMB Oxford/Cyberstar Hot air blower: RT- 980°C
ICP-ITQ-ICIQ Capillary flow cell: RT-750°C, ≤15 bar
Potentiostat for the electrochemical studies*)
*) Can be used at HP/MD station

11. HP/MD Station HP-MD station (20–50 keV)
2D Rayonix CCD detector ø162 mm
Lorentzian shape focus spot 15x15 μm
mm sample-detector distance > ° angular resolution

12. HP/MD Station: HP measurements
Sample Environment:
Diamond anvil cells (hand screw or gas membrane driven): ≤50GPa
On-line pressure calibration setup (ruby luminescence method)
External heating system: RT – 600 K
External heating vacuum system: RT – 900 K

13. HP/MD Station: MD measurements
On-Axis Sample Imaging System
Positioning tool
5-click centering tool
Sample aware tools and measurement point saving

14. BL04 MSPD Introduction Description of the beamline Overview PD station14
Introduction
Description of the beamline
Overview
PD station
HP/MD station
Typical experiments
High resolution powder diffraction
High speed powder diffraction
High pressure diffraction
Microdiffraction

15. Powder Diffraction Station
Laboratory XRD: orthorhombic unit cell, a = Å, b = Å, c = Å.
Possible space groups: Ima2 (46), I2cm (46), Imam (74), or Imcm (74).
No reasonable structure.
Synchrotron XRD: monoclinic unit cell, a = Å, b = Å, c = Å, β = 90.22°.
Possible space groups: I121 (5), I1m1 (8), and I12/m1(12).
I12/m1 gave a satisfactory solution, consisting of 10 independent Si positions.

16. Powder Diffraction Station

17. Powder Diffraction Station

18. Powder Diffraction Station

19. Powder Diffraction Station

20. BL04 MSPD Introduction Description of the beamline Overview PD station20
Introduction
Description of the beamline
Overview
PD station
HP/MD station
Typical experiments
High resolution powder diffraction
High speed powder diffraction
High pressure diffraction
Microdiffraction

21. HP/MD Station
chalcopyrite
rock salt
spinel

22. HP/MD Station

23. HP/MD Station

24. HP/MD Station

25. Thank you for attention!
Q&A
Thank you for attention!