Koji Inukai

Synthesis of highly disperse tetragonal BaTiO3 nanoparticles with core–shell by a hydrothermal method

Abstract In order to synthesize of high-dispersion and tetragonal BaTiO3 (BT) nanoparticle, a hydrothermal method is used in a mixture of chloride metal sources and KOH with polyvinylpyrrolidone (PVP). The properties of BT–PVPs prepared by different reaction temperature and time are investigated via XRD, FE-SEM, DLS, FT-IR, and TEM to clarify the changes of the crystal phase, dispersion, and particle structure. The reaction is finished at 230 °C for 24 h and the critical reaction condition for that the crystal phase of the obtained BT particle changed from the cubic to the tetragonal is found to be 190 °C fixed in reaction time 24 h, and 9 h. During reaction the PVP on the BT surface decomposed to different form, and the PVP plays the role of dispersant in aqueous solution. By the hydrothermal condition of 230 °C for 24 h almost monodisperse BT–PVP with sizes of 83 nm and tetragonality (c/a) of 1.0062 were synthesized. The structure of nanoparticle, core (BT)–shell (PVP) was investigated by FT-IR and direct observed by TEM and the mechanism of particle growth and dispersion was discussed.

Synthesis and size control of monodispersed BaTiO3–PVP nanoparticles

Abstract Monodispersed, spherical nanoparticles of the BaTiO3–polyvinylpyrrolidone (BT–PVP) composite were synthesized through the surface modification of the oxide BT by the polymer PVP, using TiCl4, BaCl2, PVP, and KOH (as the mineralizer) in an aqueous solution. To reduce the size of the particles and ensure that they were monodispersed, the concentrations of the Ba and Ti sources were increased and the reaction parameters such as reaction temperature, reaction time, and KOH concentration were optimized. As a result, monodispersed BT–PVP particles with an average diameter of 114 nm (coefficient of variation, CV = 20.0%) were obtained from a Ba-rich solution ([Ti]/[Ba] = 0.2 M:0.3 M; [KOH] = 1.4 M), and their dynamic light scattering in an aqueous suspension demonstrated that the average diameter was 162 nm (CV = 26.6%). A higher KOH concentration resulted in smaller particles, but the excess KOH promoted particle aggregation and PVP gelation. The mechanism of dispersion and aggregation of BT–PVP will be discussed in detail.

Effect of PVP on the synthesis of high-dispersion core–shell barium-titanate–polyvinylpyrrolidone nanoparticles

Abstract Monodispersed nanoparticles consisting of barium titanate (BaTiO3, BT) as the core and polyvinylpyrrolidone (PVP) as the shell were synthesized in a PVP-assisted low-temperature process in an aqueous solution at ambient pressure. In order to clarify the mechanism of this unique BT–PVP nanoparticle growth and the origin of the dispersion, the concentration and molecular weight of PVP used in the synthesis were varied, and the size and dispersion of the resulting nanoparticles in water were investigated by field-emission scanning electron microscopy and dynamic light scattering. Monodispersed nanoparticles with an average size of 130 nm were obtained by using an intermediate PVP concentration of 100 g/L and a PVP molecular weight of 10,000 g/mol. The thickness of the PVP shell was estimated by thermogravimetric analysis. For the highly dispersed BT–PVP, the thickness of PVP adsorbed on the BT surface was around 3–5 nm. Direct SEM observation of monodispersed BT–PVP in an aqueous solution using a unique sample holder was also demonstrated for the first time.

Thin Film Coating with Highly Dispersible Barium Titanate-Polyvinylpyrrolidone Nanoparticles

Thin BaTiO3 (BT) coating layers are required in various multilayer ceramic technologies, and fine nanosized BT particles with good dispersion in solution are essential for this coating process. In this work, cubic and tetragonal phase monodispersed BT nanoparticles—which were referred to as LBT and HBT-PVP coated on their surface by polyvinylpyrrolidone (PVP) polymer—were prepared by low temperature synthesis (LTS) and hydrothermal method (HT) at 80 and 230 °C, respectively. They were applied for the thin film coating on polyethylene terephthalate (PET) and Si wafer substrates by a simple bar coating. The thickness of BT, LBT-PVP, and HBT-PVP films prepared by their 5 wt % coating agent on Si are around 268, 308, and 263 nm, and their surface roughness are 104.6, 91.6, and 56.1 nm, respectively. The optical transmittance of BT, LBT-PVP, and HBT-PVP films on PET are 55, 66, and 73% at 550 nm wavelength and the haze values are 34.89, 24.70, and 20.53% respectively. The mechanism of dispersant adsorbed on the BT surface for densification of thin film during the drying process of the film was discussed.

Formation Mechanism and Dispersion of Pseudo-Tetragonal BaTiO3-PVP Nanoparticles from Different Titanium Precursors: TiCl4 and TiO2

Nano-sized tetragonal BaTiO3 (BT) particles that are well dispersed in solution are essential for the dielectric layer in multilayer ceramic capacitor technology. A hydrothermal process using TiCl4 and BaCl2, as source of Ti and Ba, respectively, or the precursor TiO2 as seed for the formation of BT, and poly(vinylpyrrolidone) (PVP) as a surfactant, was employed in this study to enhance both the dispersibility and tetragonality (c/a) simultaneously in a single reaction process. The process parameters, i.e., the ratio of TiO2 substitution of TiCl4, the reaction time, and PVP content were systematically studied, and the growth mechanism and relation between the tetragonality and the particle size are discussed. Dynamic light scattering (DLS) analysis was used to show that truncated pseudo-tetragonal BT-PVP particles with an average size of 100 nm, having a narrow size distribution and a coefficient of variation (CV) as low as 20% and being mono-dispersed in water, were produced. The narrow particle size distribution is attributed to the ability of PVP to inhibit the growth of BT particles, and the high c/a of BT-PVP to heterogeneous particle growth using TiO2 seeds.