3 years ago

Ammonothermal Synthesis of Crystalline Oxonitride Perovskites LnTaON2 (Ln=La, Ce, Pr, Nd, Sm, Gd)

Ammonothermal Synthesis of Crystalline Oxonitride Perovskites LnTaON2 (Ln=La, Ce, Pr, Nd, Sm, Gd)
Niklas Cordes, Wolfgang Schnick
The perovskite type oxonitridotantalates LnTaON2 with Ln=La, Ce, Pr, Nd, Sm, and Gd were synthesized by the ammonothermal method employing custom-built autoclaves made of nickel-based superalloy. Metal powders were reacted with NaOH and NaN3 as mineralizers under supercritical conditions with purified ammonia at temperature range of 870–1070 K and pressure values of 150–300 MPa. Crystal structures and the space groups were determined by using powder X-ray diffraction and refined by the Rietveld method. The refined lattice parameters are for LaTaON2 (a=5.7156(1), b=8.0675(1), c=5.7465(1) Å, Rwp=0.0471), CeTaON2 (a=5.6761(11), b=8.0386(16), c=5.7891(12) Å, Rwp=0.183), PrTaON2 (a=5.6920(1), b=8.0197(1), c=5.6804(1) Å, Rwp=0.0349), NdTaON2 (a=5.6884(1), b=8.0037(2), c=5.6554(1) Å, Rwp=0.026), SmTaON2 (a=5.6827(1), b=7.9656(2), c=5.6103(1) Å, Rwp=0.042), GdTaON2 (a=5.6160(10), b=7.9359(12), c=5.5962(10) Å, Rwp=0.118). LaTaON2 crystallizes in space group Imma (no. 74) and the other compounds LnTaON2 with Ln=Pr, Nd, Sm, Gd in Pnma (no. 62). SEM measurements were performed to investigate the elemental composition and morphology of the oxonitride perovskites. The bandgap values of the oxonitrides (LaTaON2 1.8 eV, CeTaON2 1.7 eV; PrTaON2 1.9 eV, NdTaON2 2.0 eV, SmTaON2 2.0 eV, GdTaON2 1.8 eV) were estimated by using UV/Vis measurements and the Kubelka–Munk function. Perovskite phases: Highly crystalline oxonitride perovskites (LnTaON2 Ln=La, Ce, Pr, Nd, Sm, Gd) were synthesized by the ammonothermal approach in custom-built high-pressure autoclaves at relatively low temperatures between 870–1070 K and pressures of up to 300 MPa. This more sophisticated route requires no precursor and gave cube-like crystals up to 15 μm (see scheme).

Publisher URL: http://onlinelibrary.wiley.com/resolve/doi

DOI: 10.1002/chem.201702231

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