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Multifunctional properties of Mn and Fe co-doped lead-free BCT perovskite ceramics synthesized via solid-state combustion
(2025-10-01)
Kornphom, Chittakorn
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Sonchaopri, Nutkamon
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Yimsabai, Sununta
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Jantaratana, Pongsakorn
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Pinitsoontorn, Supree
There is a growing demand to improve the performance of multiferroic lead-free ceramics. Good ferroelectric and magnetic properties are key parameters for achieving high magnetoelectric coupling (ME). In this work, Mn and Fe were co-doped into lead-free Ba<inf>0.96</inf>Ca<inf>0.04</inf>Ti<inf>(1-x)</inf>(Mn<inf>0.5</inf>Fe<inf>0.5</inf>)<inf>x</inf>O<inf>3</inf> (BCT-xMF) ceramics with 0 ≤ x ≤ 0.030 mol%, synthesized by the solid-state combustion technique. X-ray diffraction (XRD) analysis and Rietveld refinement confirmed the formation of a pure phase with coexisting tetragonal and cubic phases in all compositions. As the Mn/Fe content increased, the percentage of the tetragonal phase decreased while the cubic phase increased, consistent with Raman spectroscopy results. Increasing Mn/Fe content also led to more oxygen vacancies and defects, and a decrease in average grain size. Analysis of the temperature-dependent dielectric constant revealed a reduction in the Curie temperature from 116 to 67 °C, corresponding to the tetragonal-to-cubic phase transformation. The ceramic with x = 0.015 showed the highest dielectric constant at the Curie temperature (ε<inf>c</inf>), maximum saturated polarization (P<inf>s</inf>), remnant polarization (P<inf>r</inf>), saturation magnetization (M<inf>s</inf>), and remnant magnetization (M<inf>r</inf>), with values of 4583, 14.09 μC/cm2, 9.31 μC/cm2, 0.0127 emu/g, and 0.006 emu/g, respectively. These results indicate that Fe/Mn co-doping into BCT ceramics enhanced both ferroelectric and ferromagnetic properties, resulting in a high magnetoelectric coefficient (α<inf>ME</inf>∼1.27 mV/cm Oe) at room temperature, making these ceramics candidates for multiferroic applications.
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PHASE FORMATION AND ELECTRICAL PROPERTIES OF Ba0.91Ca0.09Ti0.916Sn0.084O3-0.1WT%ZnO -0.1WT%MnO2 LEAD-FREE FERROELECTRIC CERAMICS SYNTHESIZED VIA THE SOLID-STATE COMBUSTION METHOD
(2025-01-01)
Yimsabai, Sununta
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Somsri, Widchaya
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Vittayakorn, Naratip
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Charoenthai, Nipaphat
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Suthapintu, Aekasit
This work investigated the effect of firing temperatures on the phase formation, microstructure, and electrical properties of Ba0.91Ca0.09Ti0.916Sn0.084O3-0.1wt%ZnO-0.1wt%MnO2 (BCTS-ZnMn) lead-free ferroelectric ceramics synthesized via the solid-state combustion method. Glycine was used as fuel to reduce the synthesis temperature. The samples were calcined at temperatures from 1050 to 1250°C (in 50°C increments) for 3 h and sintered from 1250 to 1450°C (in 50°C increments) for 3 h. A pure perovskite phase was found in the powders calcined above 1100°C. The phase structure, microstructure, dielectric and ferroelectric properties of the ceramics were examined. The X-ray diffraction (XRD) analysis for the ceramics revealed the presence of tetragonal (T) and orthorhombic (O) phases in all the ceramics. The average particle size and average grain size increased with increasing firing temperatures. The density, dielectric constant at the Curie temperature (ɛc), Pr and Ps tended to increase with increasing sintering temperatures, up to 1400°C, and then decreased at 1450°C. The ceramic sintered at 1400°C exhibited the highest density (5.89 g/cm3), dielectric response (ɛc = 13324) and good ferroelectric behavior (Pr = 8.67 μC/cm2, Ps = 17.92 μC/cm2 and Ec = 0.99 kV/cm).
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Phase Formation, Microstructure and Electric Properties of Vanadium Doped Lead-Free BaTi0.91Sn0.09O3 Ceramics
(2023-01-01)
Pattanakasem, Wiwat
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Charoenthai, Nipaphat
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Vittayakorn, Naratip
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Bongkarn, Theerachai
Lead-free Ba(Ti<inf>0.91</inf>Sn<inf>0.09</inf>)<inf>1-x</inf>V<inf>x</inf>O<inf>3</inf> (BTSV, x = 0, 0.005,0.010, 0.015, and 0.020) ceramics were prepared by the conventional solid-state sintering method with a calcination temperature of 1200 °C for 2 h and a sintering temperature between 1350 °C and 1400 °C for 4 h. The effect of vanadium (V) doping on the phase formation, microstructure and electrical properties of the ceramics was investigated. X-ray diffraction (XRD) measurements revealed that the ceramics with x = 0 and 0.005 had pure perovskite structures with no detectable impurity, while the ceramics with x ≥ 0.010 exhibited perovskite structures and had secondary impurity phases. Coexisting orthorhombic and tetragonal phases were observed and the Rietveld refinement analysis suggested that the tetragonal phase increased with increased V5+ substitution. When x increased from 0 to 0.010, the average grain size increased from 47 to 62 µm and then dropped, while the density (ρ) decreased from 5.98 to 5.64 g/cm3 when x increased. Furthermore, the BTSV ceramics exhibited increased porosity, Curie temperatures (T <inf>C</inf> ∼ 42 °C to 52 °C) and coercive field (E <inf>c</inf>), while the dielectric constant at the Curie temperature (ε<inf>C</inf>) and the remnant polarization (P <inf>r</inf>) of the ceramics decreased (∼18023 to 6110 and ∼7.42 to 4.88 µC/cm2, respectively) when V5+ doping increased.
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Phase formation and evolution of Cu:Zn partials in binary metal pyrophosphates Cu(2-x)Zn(x)P2O7; X ≈ 1
(2014-11-20)
Baitahe, Rattanai
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Vittayakorn, Naratip
Binary metal pyrophosphate powders were prepared by the solid state reaction method and subsequently calcined at 400, 500, 600, 700, and 800 °C in order to study Cu:Zn partial evolution to the final CuZnP<inf>2</inf>O<inf>7</inf> product. Synchrotron X-ray absorption, X-ray diffraction, Raman, FT-IR spectroscopy, and thermogravimetric analysis were used in this investigation. Phase evolution of the reaction products was investigated systemically. The results showed that complicated mixtures contributed to the reaction of synthesis temperature. The reaction comprised 3CuO·2P<inf>2</inf>O<inf>5</inf>·0.3NH<inf>3</inf>·0.2H<inf>2</inf>O, Cu<inf>2</inf>P<inf>2</inf>O<inf>7</inf>, Zn<inf>2</inf>P<inf>2</inf>O<inf>7</inf>, and Zn<inf>2</inf>P<inf>2</inf>O<inf>7</inf>·3H<inf>2</inf>O intermediates. Decreasing percentage of 3CuO·2P<inf>2</inf>O<inf>5</inf>·0.3NH<inf>3</inf>·0.2H<inf>2</inf>O intermediates was related directly to an increasing final product. Cu:Zn contents changed in Cu<inf>(2-x)</inf>Zn<inf>(x)</inf>P<inf>2</inf>O<inf>7</inf> in the temperature range of 400-600 °C, when x ≈ 1 clearly was related linearly to the reaction temperature. The final product was confirmed by EXAFS fitting spectra as solid solution between the Cu and Zn atom in the CuZnP<inf>2</inf>O<inf>7</inf> structure, and it indicated environment around metal atoms.
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Effect of firing temperatures on phase formation and microstructure of Ba(Zr0.3Ti0.7)O3 ceramics prepared via mixed oxide method
(2009-12-01)
Bongkarn, Theerachai
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Phungjitt, Nalinee
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Vittayakorn, Naratip
Ba(Zr0.3Ti0.7)O3 (BZT) ceramics were fabricated by a mixed oxide synthetic route. The effect of calcination and sintering temperatures on phase formation and the microstructure of the ceramics were investigated. The pure perovskite phase of BZT powders was obtained with a calcination condition of 1300°C for 4 h. The sintered pellets showed a pure peroverskite cubic phase in all samples. The microstructure of the powders exhibited an almost-spherical morphology and had a porous agglomerated form. The average particle sizes and the average grain sizes were increased from 0.2 to 1.1 μm and 3.9 to 25.1 μm with increasing calcination and sintering temperatures, respectively. The densest and the highest maximum dielectric constant was found in the BZT ceramic sintered at 1550°C. Copyright © Taylor & Francis Group, LLC.

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