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Barium titanate thin films were deposited via chemical solution deposition using a hybrid-chelate chemistry directly on copper foil substrates. A process was developed to crystallize and densify the ferroelectric films at 900C by using a reductive atmosphere containing nitrogen, hydrogen, water vapor, and oxygen impurities such that film constituents were oxidized to form barium titanate and the foil substrate remained metallic. The crystallized films are polycrystalline with equiaxed morphology and average grain diameters in excess of 100 nm. The dielectric properties exhibit permittivities in excess of 1800 at room temperature and zero bias with tunabilites of greater than 90% and high field loss tangents of less than 1%. A series of samples was prepared with varying grain and crystallite sizes by dividing and processing a single film over a range of temperature from 700 to 900C. This ensures that the chemical composition and film thickness is invariant for each sample. It is shown that the grain size increases with higher process temperatures and results in a concomitant increase in permittivity and tunability. These enhancements, combined with the constant paraelectricD erroelectric phase transition temperature, indicated that a combination of film crystallinity and grain size is responsible for diminished performance. The phase transition temperature and temperature coefficient of capacitance modified by partially substituting zirconium, hafnium, and tin for titanium. The resulting films were single phase and the phase transition shifts were consistent with bulk materials. A reduction in permittivity was observed for increasing substituent level and was attributed to a reduction in grain size for both barium titanate zirconate and barium titanate hafnate. Processing conditions were chosen to stabilize Sn2+ during the firing process in an attempt to flux the system and increase grain size. The barium titanate stannate films had less reduction in grain size.
Ferroelectric BaTiO3 (BTO) thin films were deposited on polycrystalline nickel disks and silicon wafer substrates by rf magnetron sputtering. Nickel oxide (NiO) and nanocrystalline nickel (nc-Ni) layers were used as interfacial buffer layers. Microstructural studies with X-ray diffraction and transmission electron microscopy reveal that the BTO films deposited at temperatures lower than 700°C have an amorphous structure. However, the BTO films sputtered at temperatures higher than 700°C are partially crystalline. BTO films have a good and continuous interface with both interfacial layers with no interdiffusion or reaction with the substrates. In the case of BTO deposition with nc-Ni interlayer at higher deposition temperature of 800°C, a thin NiO layer forms between the nc-Ni and BTO films. Having nc-Ni as an interfacial layer enhances surface morphology and decreases surface roughness. This study shows that nc-Ni can act as a proper interfacial layer between a ceramic like BTO and the metallic substrates and is a better alternative for NiO buffer layer.
Keywords: hafnium, tin, zirconium, flux, copper, equilibria, grain size, size effects, sol-gel, barium titanate, film, ferroelectric, doping.