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

BL04 MSPD Introduction Description of the beamline Overview PD station 2 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

BL04 MSPD Introduction Description of the beamline Overview PD station 3 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

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, …)

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

BL04 MSPD Introduction Description of the beamline Overview PD station 6 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

Description of the beamline 7

Description of the beamline

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) -> 0.005° 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 0.005 deg pitch -> 0.02° angular resolution YNiO3 90.0754 º monoclinic distortion

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

HP/MD Station HP-MD station (20–50 keV) 2D Rayonix CCD detector ø162 mm Lorentzian shape focus spot 15x15 μm 150-500 mm sample-detector distance -> 0.05-0.08° angular resolution

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

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

BL04 MSPD Introduction Description of the beamline Overview PD station 14 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

Powder Diffraction Station Laboratory XRD: orthorhombic unit cell, a = 17.937 Å, b = 17.516 Å, c = 12.375 Å. Possible space groups: Ima2 (46), I2cm (46), Imam (74), or Imcm (74). No reasonable structure. Synchrotron XRD: monoclinic unit cell, a = 17.511 Å, b = 17.907 Å, c = 12.367 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.

Powder Diffraction Station

Powder Diffraction Station

Powder Diffraction Station

Powder Diffraction Station

BL04 MSPD Introduction Description of the beamline Overview PD station 20 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

HP/MD Station chalcopyrite rock salt spinel

HP/MD Station

HP/MD Station

HP/MD Station

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