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Improvement of Solid Through Improved Solutions and Gels (1): Utilization of Reduction Agent and Reduced Atmosphere

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Abstract

In Sect. 12.1, a novel low-temperature crystallization path for perovskite lead zirconate titanate (PZT) from solution is reported. The modification of a PZT solution with monoethanolamine (MEA) resulted in a change in the crystallization behavior. MEA was strongly coordinated to the metal ions, resulting in reduction of Pb2+ into Pb0 because of a reducing environment at 200–300 °C. Nanoscopic separations of Pb0 were later transformed into uniformly distributed PbO nanocrystals and clusters in the amorphous Zr/Ti–O matrix and finally crystallized into perovskite at 400–500 °C. On the other hand, pyrochlore phase appeared in the conventional crystallization process. The avoidance of pyrochlore formation is a key for the low-temperature crystallization of perovskite. X-ray absorption fine structure (XAFS) analysis was performed to reveal the structures in solutions and amorphous phases.

In Sect. 12.2, a new reaction path for the low-temperature crystallization of device-quality PZT films was described. The essential aspect of this path is to circumvent pyrochlore formation at approximately 300 °C as the temperature is increased to 400 °C. In this approach, MEA was not used. Pb2+ was reduced to Pb0 by maintaining the presence of sufficient carbon via pyrolysis at 210 °C, which is well below the temperature for pyrochlore formation. This process led to insufficient Pb2+ in the film to form pyrochlore. The films were successfully crystallized onto metals and metal/oxide hybrids at 400–450 °C.

In Sect. 12.3, the same method as in Sect. 12.1 was used to form highly conductive ruthenium metal (Ru0) and ruthenium oxide (RuO2) films. Those solutions were prepared from ruthenium(III) nitrosyl acetate and amines. Ru0 and RuO2 thin films were formed when annealed under an inert atmosphere (nitrogen or vacuum) and under an oxygen atmosphere, respectively. The effects of different amine structures were compared, and alkanolamine and amino acids were found to produce Ru0 films of higher quality than films formed by alkyl amines. These results were correlated with the structures of ruthenium complexes. The resistivity values of Ru0 and RuO2 thin films prepared from ruthenium–alkanolamine complexes were 2.1 × 10−5 and 4.3 × 10−4 Ω cm, respectively, similar to those of vacuum-processed Ru0 and RuO2 ones. The Ru0 film showed high stability against oxidation during further annealing in oxygen, even at nanometer thickness (e.g., 25 nm).

In Sect. 12.4, highly conductive RuO2 thin films were prepared by a low-temperature solution process combined with green laser annealing (GLA). This process enabled the production of RuO2 films at a relatively low temperature of 250 °C. GLA led to effective sintering of the film, significantly improving its crystallinity and density, resulting in grain joining; consequently, the conductivity was dramatically increased by one order of magnitude or more. The RuO2 thin films exhibited a low resistivity (e.g., 7.6 × 10−5 Ωcm for a 40-nm-thick film), which was approximately only two times greater than that of single-crystalline RuO2. Such resistivity has not previously been achieved if thermal annealing soley used even at a temperature of 800 °C and is similar to or lower than that of vacuum-deposited RuO2 films.

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    Tatsuya Shimoda

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Shimoda, T. (2019). Improvement of Solid Through Improved Solutions and Gels (1): Utilization of Reduction Agent and Reduced Atmosphere. In: Nanoliquid Processes for Electronic Devices. Springer, Singapore. https://doi.org/10.1007/978-981-13-2953-1_12

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