Rapid Sintering of Li₂O-Nb₂O₅-TiO₂ Solid Solution by Air Pressure Control and Clarification of Its Mechanism

Materials (Basel). 2018 Jun 11;11(6):987. doi: 10.3390/ma11060987.

Abstract

We first successfully synthesized Li1+x−yNb1−x−3yTix+4yO₃ (LNT) solid solutions (0.13 ≤ x ≤ 0.18, 0 ≤ y ≤ 0.06) rapidly at 1373 K for one hour under 0.35 MPa by the controlling of air pressure using an air-pressure control atmosphere furnace. The composition is a formation area of a superstructure for LNT, in which the periodical intergrowth layer was formed in the matrix, and where it can be controlled by Ti content. Therefore, the sintering time depended on Ti content, and annealing was repeated for over 24 h until a homogeneous structure was formed using a conventional electric furnace. We clarified the mechanism of the rapid sintering using various microscale to nanoscale characterization techniques: X-ray diffraction, a scanning electron microscope, a transmission electron microscope (TEM), a Cs-corrected scanning TEM equipped with electron energy-loss spectroscopy, and X-ray absorption fine structure spectroscopy.

Keywords: HAADF-STEM; TEM; X-ray diffraction; crystal structure; oxide materials; rapid sintering.