Low-Temperature Synthesis of Perovskite-Type (Na,K)NbO₃ through Nb₆O₁₉⁸⁻ Clusters by Dissolution–Precipitation Method

  • Shibata Kengo
    Department of Materials Chemistry, Ryukoku University
  • Yamazoe Seiji
    Department of Materials Chemistry, Ryukoku University Department of Chemistry, School of Science, The University of Tokyo
  • Wada Takahiro
    Department of Materials Chemistry, Ryukoku University

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タイトル別名
  • Low-Temperature Synthesis of Perovskite-Type (Na,K)NbO<sub>3</sub> through Nb<sub>6</sub>O<sub>19</sub><sup>8−</sup> Clusters by Dissolution–Precipitation Method

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We successfully synthesized perovskite-type (Na1−xKx)NbO3 materials from a Na3NbO4 precursor at low temperature by dissolution–precipitation method. The Nb6O198− cluster was formed as an intermediate by the dissolution of Na3NbO4 into a buffer solution (pH 7). White powders were precipitated by the addition of 1 M NaOH/KOH mixed aqueous solution. We found that the morphology and crystal structure depended on the NaOH/KOH ratio. When the concentration of KOH [CKOH = KOH/(NaOH + KOH)] was low (0 ≤ CKOH ≤ 0.3), rod-like (Na,K,H3O)8Nb6O19·14H2O was precipitated. In the case of high CKOH (0.5 ≤ CKOH ≤ 0.9), (Na0.5K0.5)8Nb6O19·9H2O, whose morphologies changed from hexagonal plate-like to truncated hexagonal bipyramidal structures with the increase in the CKOH, was formed. The (Na,K,H3O)8Nb6O19·14H2O and (Na0.5K0.5)8Nb6O19·9H2O mixture was precipitated using a NaOH/KOH solution with CKOH = 0.4. No precipitation was obtained by the addition of the KOH solution. These precipitations transformed into perovskite-type (Na,K)NbO3 while maintaining their morphology by calcination at 500 °C. The excess Na and/or K were washed out with water. From the lattice constants, the rod-like (Na1−xKx)NbO3 with 0 ≤ x ≤ 0.2 and the hexagonal plate-like or the truncated hexagonal bipyramidal (Na0.5K0.5)NbO3 were synthesized from the rod-like (Na,K,H3O)8Nb6O19·14H2O (0 ≤ CKOH ≤ 0.3) and the hexagonal plate-like or the truncated hexagonal bipyramidal (Na0.5K0.5)8Nb6O19·9H2O (0.5 ≤ CKOH ≤ 0.9), respectively.

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