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Synthesis and Characterization of Ferroelectric NanomaterialsDu, Hongchu 14 August 2008 (has links) (PDF)
In this dissertation, BaTiO3 nanocrystals, Bi4Ti3O12 nanostructured microspheres, and cosubstituted Bi4Ti3O12 nanoparticles and ceramics were prepared using solvothermal, hydrothermal and citrate-gel methods. The ferroelectric properties of the prepared cosubstituted Bi4Ti3O12 ceramics were studied using P–E hysteresis loop, leakage, and polarization fatigue measurements. A two-phase solvothermal synthesis approach for the preparation of hydrophobic BaTiO3 nanocrystals was developed. The two-phase method is based on the growth of nanocrystals at the oil/water interface by the reaction between metal surfactant complexes in the oil phase and a mineralizer in the water phase. Three kind of organic solvents, hexadecene, toluene, and heptane were used as the oil phase and compared to each other with respect to the product quality. The BaTiO3 particles are crystalline with a mean size of 3.7 nm and can be dispersed in a variety of organic solvents forming highly transparent dispersions. A hydrothermal method was developed for the synthesis of Bi4Ti3O12 nanostructured microspheres consisting of granular nanoparticles and nano-platelets. The precursor powder was prepared using a diethylene glycol mediated coprecipitation method. Tailoring of the morphology was achieved by changing the precursor quantity, sodium hydroxide concentration, and reaction time. The formation mechanism of the nanostructured microspheres probably involves aggregation, followed by dissolution and recrystallization. Bi3.25Pr0.75Ti2.97V0.03O12 (BPTV) and Bi3.25La0.75Ti3-xMxO12, (BLTMx, M = Mo, W, Nb, V, x = 0.0–0.12) ferroelectric nanoparticles and ceramics were synthesized using a modified citrate-gel method that has a crystallization temperature as low as 450 °C. The synthesized nanoparticles were spherical ranging from 30 to 100 nm. Except Nb5+, other donor cations were introduced using the corresponding oxides that have advantages in terms of high purity, low cost, and availability. The Bi3.25Pr0.75Ti2.97V0.03O12 ceramic is orthorhombic and its 2Pr and 2Ec values measured at 300 kV/cm were 35 μC/cm2 and 148 kV/cm respectively. The texture, microstructure, and ferroelectric properties of the prepared Bi3.25La0.75Ti3-xMxO12, (BLTMx, M = Mo, W, Nb, V, x = 0.0–0.12) ceramics depend on x. The maximum 2Pr (30–32 μC cm−2) was achieved at an optimum cosubstitution level (x = 0.025 for M6+, x = 0.03 for M5+). The high remanent polarization, low leakage current, and low polarization fatigue render the prepared ceramics promising for practical applications.
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Synthesis and Characterization of Ferroelectric NanomaterialsDu, Hongchu 02 July 2008 (has links)
In this dissertation, BaTiO3 nanocrystals, Bi4Ti3O12 nanostructured microspheres, and cosubstituted Bi4Ti3O12 nanoparticles and ceramics were prepared using solvothermal, hydrothermal and citrate-gel methods. The ferroelectric properties of the prepared cosubstituted Bi4Ti3O12 ceramics were studied using P–E hysteresis loop, leakage, and polarization fatigue measurements. A two-phase solvothermal synthesis approach for the preparation of hydrophobic BaTiO3 nanocrystals was developed. The two-phase method is based on the growth of nanocrystals at the oil/water interface by the reaction between metal surfactant complexes in the oil phase and a mineralizer in the water phase. Three kind of organic solvents, hexadecene, toluene, and heptane were used as the oil phase and compared to each other with respect to the product quality. The BaTiO3 particles are crystalline with a mean size of 3.7 nm and can be dispersed in a variety of organic solvents forming highly transparent dispersions. A hydrothermal method was developed for the synthesis of Bi4Ti3O12 nanostructured microspheres consisting of granular nanoparticles and nano-platelets. The precursor powder was prepared using a diethylene glycol mediated coprecipitation method. Tailoring of the morphology was achieved by changing the precursor quantity, sodium hydroxide concentration, and reaction time. The formation mechanism of the nanostructured microspheres probably involves aggregation, followed by dissolution and recrystallization. Bi3.25Pr0.75Ti2.97V0.03O12 (BPTV) and Bi3.25La0.75Ti3-xMxO12, (BLTMx, M = Mo, W, Nb, V, x = 0.0–0.12) ferroelectric nanoparticles and ceramics were synthesized using a modified citrate-gel method that has a crystallization temperature as low as 450 °C. The synthesized nanoparticles were spherical ranging from 30 to 100 nm. Except Nb5+, other donor cations were introduced using the corresponding oxides that have advantages in terms of high purity, low cost, and availability. The Bi3.25Pr0.75Ti2.97V0.03O12 ceramic is orthorhombic and its 2Pr and 2Ec values measured at 300 kV/cm were 35 μC/cm2 and 148 kV/cm respectively. The texture, microstructure, and ferroelectric properties of the prepared Bi3.25La0.75Ti3-xMxO12, (BLTMx, M = Mo, W, Nb, V, x = 0.0–0.12) ceramics depend on x. The maximum 2Pr (30–32 μC cm−2) was achieved at an optimum cosubstitution level (x = 0.025 for M6+, x = 0.03 for M5+). The high remanent polarization, low leakage current, and low polarization fatigue render the prepared ceramics promising for practical applications.
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