Microstructural study of ytterbium zirconate pyrochlore synthesized by the mixed method: sintering/chemical infiltration

Dalila Moudir; Yasmina Mouheb; Nouar Bensemma; Youssef Larbah; Fairouz Aouchiche; Amina Amrane; Aicha Maachou

Dalila Moudir Algiers Nuclear Research Centre, 2. Bd Frantz Fanon, B.P:399, Algiers, Algeria
Yasmina Mouheb Algiers Nuclear Research Centre, 2. Bd Frantz Fanon, B.P:399, Algiers, Algeria
Nouar Bensemma Berine Nuclear Research Centre Ain Oussera.Bp 180, Djelfa, Algeria
Youssef Larbah Algiers Nuclear Research Centre, 2. Bd Frantz Fanon, Bp 399, Algiers, Algeria
Fairouz Aouchiche Algiers Nuclear Research Centre, 2. Bd Frantz Fanon, Bp 399, Algiers, Algeria
Amina Amrane Draria Nuclear Research Centre Sebala. Draria, Bp 43, Algiers, Algeria
Aicha Maachou Algiers Nuclear Research Centre, 2. Bd Frantz Fanon, Bp 399, Algiers, Algeria

Keywords: pyrochlore, ytterbium, zirconate, infiltration, XRD, SEM, FTIR

Abstract

In this study, a zirconate pyrochlore with the chemical formula (Yb₀.₁Ba₀.₉)₂Zr₂O₇ was synthesized and stabilized by ytterbium nitrate. The used synthesis method combined between calcination and infiltration procedure where the considered infiltration parameters were concentration of ytterbium solution set at C=390 g/L, infiltration temperature and T= 105°C. However the thermal cycle of sintering in two stages, calcination at 550°C for 4 h, then a sintering of 1200°C for 24h. The characterization of the synthesized material was carried out by several analysis techniques. Archimedes' density using a hydrostatic balance gave a value of 4.001 g/ cm³ for the raw ceramic and 4.665g/cm³ for the sintered one. X-ray diffraction (XRD) analysis was used to track the progress of the synthesis and confirm its success through the formation of the ZrO₂ structure, the main framework of the pyrochlore material. Observation using a scanning electron microscope (SEM) allowed us to observe the distribution of grains and pores and estimate the quality of sintering, combined with analysis using X-ray energy dispersive spectrometry (EDX), which allowed us to check the global chemical composition of the sintered matrix. Fourier transform infrared (FTIR) analysis of pyrochlore (Yb₀.₁Ba₀.₉)₂Zr₂O₇ shows essential absorption bands between 400-4000 cm⁻¹.Two absorption bands can be seen at 470 cm⁻¹corresponding to Zr-O vibrations, and an absorption band at 682 cm⁻¹ corresponding to Ba-O vibrations.

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