Abstract
Here, we show that wet impregnation of ZrO2 nanoparticles with 10% and 20% Eu oxide followed by thermal anneal in air above 500 °C produces full stabilization of the tetragonal phase of ZrO2 without evidencing any phase separation. The bare ZrO2 nanoparticles were obtained using three synthetic methods: oil in water microemulsion, rapid hydrothermal, and citrate complexation methods. The homogeneity of the solid solutions was assessed using X-ray diffraction, Raman spectroscopy, high resolution transmission electron microscopy, and advanced luminescence spectroscopy. Our findings show that wet impregnation, which is a recognized method for obtaining surface doped oxides, can be successfully used for obtaining doped oxides in the bulk with good homogeneity at the atomic scale. The limits of characterization technique in detecting minor phases and the roles of dopant concentration and host structure in formation of phase stabilized solid solutions are also analyzed and discussed.
Highlights
Zirconium oxide (ZrO2) is a well-established ceramic material where the physical and chemical properties depend strongly on the structural phase leading to a variety of applications [1,2]
Otherwise a well-known method used for synthesis of heterogeneous catalysts, exposes the host oxide to a liquid containing the precursor of the dopant, which is dried and heated in air
We show that wet impregnation of ZrO2 with 10% and 20% Eu oxide followed by thermal anneal in air above 500 ◦C leads to solid solutions of tetragonal phase that are homogenous at the atomic scale
Summary
Zirconium oxide (ZrO2) is a well-established ceramic material where the physical and chemical properties depend strongly on the structural phase leading to a variety of applications [1,2]. Both tetragonal and cubic phases can be stabilized at ambient temperatures upon doping with trivalent ions such as Y3+ or lanthanides (Ln) [3,4]. According to Li et al [4], the oversized aliovalent lanthanide metals are effective for the stabilization of tetragonal and cubic phases at room temperature via generation of the oxygen ion vacancies. To maintain its effective coordination number close to 7, as required by the (partial) covalent nature of the Zr–O bond, the ZrO2 lattice assumes a crystal structure, which offers an 8- coordination number (typically tetragonal or cubic structures) and simultaneously incorporates the generated oxygen vacancies into the lattice as the nearest neighbors to Zr4+ cations, and next- nearest neighbors to the trivalent Ln
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