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Large-scale engineered synthesis of BaTiO3 nanoparticles using low-temperature bioinspired principles

Abstract

We report here a robust, large-scale synthesis of BaTiO3 nanopowders using a bioinspired process that first was developed on a much smaller scale. The most advantageous points of this protocol are that it takes place at nearly room temperature (25 °C), overcomes many limitations encountered in other scale-up processes (such as the need for external drivers, e.g., heat, radiation or pressure), bypasses the use of surfactants and templates and does not necessitate pH adjustment. The use of a single-source, bimetallic alkoxide with the vapor diffusion of a hydrolytic catalyst (H2O) provides the necessary conditions for facile crystallization and growth of small, well-defined BaTiO3 nanoparticles at mild temperatures, yielding batches of up to 250 ± 5 g in a green process. Extension of this method to kilogram-scale production of BaTiO3 nanocrystals in semicontinuous and continuous processes is feasible.

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Figure 1: Schematic representation of the reactor platform used in this protocol.
Figure 2: The scale-up platform and Viscoklick attachment.
Figure 3: Comparative torque data from heated (red) 125 ± 5 g and unheated (blue) 125 ± 5 g syntheses.
Figure 4: Structural characterization of the nanopowder manufactured using the reactor platform described in Figure 1.
Figure 5: XRD analysis monitoring the structural evolution on gradual sintering of the product from 30 to 700 °C (heating rate 50 °C per min, dwell time 25 min, after which XRD data was collected).
Figure 6: Proposed continuous-flow automated scale-up plant (currently under investigation).

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Acknowledgements

This work was supported by contracts from the Power and Energy Division of the US Army's Communications-Electronics Research, Development and Engineering Center (CERDEC); by grants from the US Army Research Office through Grant DAAD19-03-D-0004 to the Institute for Collaborative Biotechnologies and (for support of D.E.M. and M.L.) the US Department of Energy (DEFG03-02ER46006); and by the facilities of UCSB's Materials Research Laboratory (through the National Science Foundation's Materials Research Science and Engineering Centers (MRSEC) Program Grant no. DMR05-20414). We thank Dr. E.J. Plichta, Chief of the Power Division at CERDEC and M. Hendrickson, Chief Engineer at CERDEC, for their vision and support. We also thank R. Bock and S. Kramer for technical assistance.

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All authors contributed equally to this work. T.O.-E. wrote the main paper, conceived and engineered all the scale-up reactors, and executed experimental work with the assistance of M.L., L.K.-R. and K.N. All authors discussed the results and implications, and edited and commented on the manuscript at all stages. M.D. and D.E.M. directed this collaborative research.

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Correspondence to Daniel E Morse.

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The authors declare no competing financial interests.

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Ould-Ely, T., Luger, M., Kaplan-Reinig, L. et al. Large-scale engineered synthesis of BaTiO3 nanoparticles using low-temperature bioinspired principles. Nat Protoc 6, 97–104 (2011). https://doi.org/10.1038/nprot.2010.138

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