Synthesis of the heptagonal approximant γ-Gallium Master Project

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Presentation transcript:

Synthesis of the heptagonal approximant γ-Gallium Master Project Michele Zahner 26.03.2010 Laboratory for Crystallography ETHZ

Quasicrystals and Approximants Periodic Quasiperiodic 1 2 3 4 6 5 7 8 10 12 7-fold rotational symmetry: not known, but approximants exist. Approximant: γ-Gallium

Motivation γ-Gallium: heptagonal approximant made of just one element! Interesting candidate for the synthesis of 7-fold quasicrystals. Goals: Synthesis of γ-Gallium Synthesis protocol for µm-sized Gallium particles Single-crystal experiment

Gallium Low melting point Polymorphism Vsolid > Vmelt (like H2O)

γ-Gallium metastable Orthorhombic oC40 a = 10.593 Å b = 13.523 Å Tm = -35.6 °C z = ¾ z = 0, ½, 1 Bosio, L., A. Rimsky, et al. (1972). Acta Cryst. B 28: 1974-1975.

Synthesis Small droplets: less impurities + size effect => easier supercooling Mix Ga drop, ethanol and emulsifier (SDS) SDS: Sodium dodecyl sulfate Heat to 50 °C Shaking by hand Sonication 3. Decantation of solvent, fill up with pure EtOH

Single particle diffraction Typical size: 30 µm Heating: lamp Cooling: cryojet Quenching in situ Reversible

Single particle diffraction Oxford Diffraction Xcalibur 4-circle diffractometer CryoJet: N2-Gas cooling unit for in situ experiments For this work: T = 164K (-110 °C) http://xray.chm.jhu.edu/gallery

Results (164 K) orthorombic; a = 10.568 Å b = 13.560 Å c = 5.116 Å Section hk0 Section 0kl Section h0l

Intergrowth – reciprocal space Section hk0 Crystallite 1: 0° Crystallite 2 ~77.1° around c*

Intergrowth – real space 0° 1 ⋅ 25.7° 2 ⋅ 25.7° = 51.4° 3 ⋅ 25.7° = 77.1° 1/14 ⋅ 2π = 25.7° Best match at 3/14 ⋅ 2π

Satellite reflections h,l sections Not attributed to additional crystallites or phases Satellites? Main reflections Satellites Section h1l

Reconstruction Integration of dataset with main reflections only Structure solution by charge-flipping (Superflip) ED map of CF result with super- imposed γ-Gallium structure ED-section at z = ¾ Palatinus, L. et al. (2007). Journal of Applied Cryst. 40: 786-790. Oszlanyi, G. et al. (2004). Acta Cryst. A 60: 134-141.

Summary µm- to sub-µm-sized Gallium particles were synthesized A Suitable setup for the synthesis of γ-Gallium was developed (principal task) γ-phase was obtained reliably at 164 K Single crystal data were collected and processed Literature was confirmed but additional features were observed (satellites may indicate modulation) Outlook: Extending the work to binary alloys in order to find new approximants and quasicrystals