Welcome to the new version of CaltechAUTHORS. Login is currently restricted to library staff. If you notice any issues, please email coda@library.caltech.edu
Published August 16, 2019 | Accepted Version + Supplemental Material
Journal Article Open

Additive Manufacturing of 3D-Architected Multifunctional Metal Oxides

Abstract

Additive manufacturing (AM) of complex three‐dimensional (3D) metal oxides at the micro‐ and nanoscales has attracted considerable attention in recent years. State‐of‐the‐art techniques that use slurry‐based or organic–inorganic photoresins are often hampered by challenges in resin preparation and synthesis, and/or by the limited resolution of patterned features. A facile process for fabricating 3D‐architected metal oxides via the use of an aqueous metal‐ion‐containing photoresin is presented. The efficacy of this process, which is termed photopolymer complex synthesis, is demonstrated by creating nanoarchitected zinc oxide (ZnO) architectures with feature sizes of 250 nm, by first patterning a zinc‐ion‐containing aqueous photoresin using two‐photon lithography and subsequently calcining them at 500 ºC. Transmission electron microscopy (TEM) analysis reveals their microstructure to be nanocrystalline ZnO with grain sizes of 5.1 ± 1.6 nm. In situ compression experiments conducted in a scanning electron microscope show an emergent electromechanical response: a 200 nm mechanical compression of an architected ZnO structure results in a voltage drop of 0.52 mV. This photopolymer complex synthesis provides a pathway to easily create arbitrarily shaped 3D metal oxides that could enable previously impossible devices and smart materials.

Additional Information

© 2019 WILEY‐VCH. Issue Online: 13 August 2019; Version of Record online: 24 June 2019; Manuscript revised: 07 June 2019; Manuscript received: 27 February 2019. M.L.L. and D.W.Y. contributed equally to this work. The authors would like to thank the following people: J. H. Kang and the Davis lab at Caltech for performing TGA analysis, M. T. Johnson and the Faber lab at Caltech for assistance with our preliminary thermal process, R. A. Gallivan for her assistance with the electromechanical experiments and thoughtful discussions, C. M. Garland for her assistance with TEM imaging, and A. Vyatskikh for helpful discussions. The authors gratefully acknowledge the financial support from the National Institutes of Health (Grant No. 1R01CA194533), the Gwangju Institute of Science and Technology (Grant No. CG2014), and the U.S. Department of Defense through J.R.G.'s Vannevar‐Bush Fellowship. The authors would also like to acknowledge the support granted by the National Institutes of Health Biotechnology Leadership Training Program (Grant No. T32GM112592). M.L.L., D.W.Y., and J.R.G. conceived and designed the experiments; D.W.Y. developed the polymer chemistry and fabricated the microstructures using two‐photon lithography; D.W.Y. and M.L.L. developed the heating profile and performed SEM analyses; D.W.Y. performed the EDS data collection and analysis. M.L.L. performed the XRD and TEM analyses; M.L.L. built the electromechanical set‐up and performed and analyzed the in situ open circuit voltage response electromechanical measurements. B.W.E. performed and analyzed the in situ mechanical compression experiments. The authors declare no conflict of interest.

Attached Files

Accepted Version - nihms-1040171.pdf

Supplemental Material - downloadSupplement_doi=10.1002_2Fadma.201901345_file=adma201901345-sup-0001-S1.avi

Supplemental Material - downloadSupplement_doi=10.1002_2Fadma.201901345_file=adma201901345-sup-0001-S1.pdf

Files

nihms-1040171.pdf
Files (1.2 MB)
Name Size Download all
md5:332c9caa32163b8b2268c785bccc116d
1.2 MB Preview Download

Additional details

Created:
August 19, 2023
Modified:
October 20, 2023