XRD and EXAFS studies on the structure of Er{sup 3+}-doped SiO{sub 2}-HfO{sub 2} glass-ceramic waveguides: Er{sup 3+}-activated HfO{sub 2} nanocrystals

Abstract

This paper describes the structure of Er{sup 3+}-doped SiO{sub 2}-HfO{sub 2} waveguides containing nanocrystals of HfO{sub 2}. Pure and 1 mol% Er{sup 3+}-doped 70SiO{sub 2}-30HfO{sub 2} films were deposited by the sol-gel method on amorphous SiO{sub 2} substrates using the dip-coating technique. Each waveguide has experienced a single thermal treatment at temperatures ranging from 900 to 1200 deg. C, for either short (30 min) or long (24 h) durations. Crystallization and microstructure were studied by x-ray diffraction (XRD). The local environments of hafnium and erbium ions were determined, respectively, from Hf and Er L{sub 3}-edges extended x-ray absorption fine structure (EXAFS) experiments. Both XRD and EXAFS results demonstrate the substitution of Hf{sup 4+} by Er{sup 3+} ions in the crystalline structure. XRD shows the nucleation of tetragonal HfO{sub 2} nanocrystals after heat treatment at 1000 deg. C for 30 min in the pure waveguide, and at 900 deg. C for 24 h in the waveguide doped with Er{sup 3+}. In both series, partial transformation from tetragonal to monoclinic HfO{sub 2} nanocrystals starts after heat treatment at 1100 deg. C for 24 h. The average crystallite size and size distribution can be controlled by thermal annealing temperature and duration, respectively, with brief treatment yielding a more homogeneous nanocrystal size.