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Optical Identification of Materials Transformations in Oxide Thin Films

Sutherland, Duncan R. and Connolly, Aine Boyer and Amsler, Maximilian and Chang, Ming-Chiang and Gann, Katie Rose and Gupta, Vidit and Ament, Sebastian and Guevarra, Dan and Gregoire, John M. and Gomes, Carla P. and van Dover, R. Bruce and Thompson, Michael O. (2020) Optical Identification of Materials Transformations in Oxide Thin Films. ACS Combinatorial Science, 22 (12). pp. 887-894. ISSN 2156-8952. doi:10.1021/acscombsci.0c00172.

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Recent advances in high-throughput experimentation for combinatorial studies have accelerated the discovery and analysis of materials across a wide range of compositions and synthesis conditions. However, many of the more powerful characterization methods are limited by speed, cost, availability, and/or resolution. To make efficient use of these methods, there is value in developing approaches for identifying critical compositions and conditions to be used as a priori knowledge for follow-up characterization with high-precision techniques, such as micrometer-scale synchrotron-based X-ray diffraction (XRD). Here, we demonstrate the use of optical microscopy and reflectance spectroscopy to identify likely phase-change boundaries in thin film libraries. These methods are used to delineate possible metastable phase boundaries following lateral-gradient laser spike annealing (lg-LSA) of oxide materials. The set of boundaries are then compared with definitive determinations of structural transformations obtained using high-resolution XRD. We demonstrate that the optical methods detect more than 95% of the structural transformations in a composition-gradient La-Mn-O library and a Ga2O3 sample, both subject to an extensive set of lg-LSA anneals. Our results provide quantitative support for the value of optically detected transformations as a priori data to guide subsequent structural characterization, ultimately accelerating and enhancing the efficient implementation of micrometer-resolution XRD experiments.

Item Type:Article
Related URLs:
URLURL TypeDescription
Connolly, Aine Boyer0000-0002-2721-5621
Amsler, Maximilian0000-0001-8350-2476
Chang, Ming-Chiang0000-0003-1880-6654
Gupta, Vidit0000-0002-4869-5820
Guevarra, Dan0000-0002-9592-3195
Gregoire, John M.0000-0002-2863-5265
Gomes, Carla P.0000-0002-4441-7225
van Dover, R. Bruce0000-0002-6166-5650
Additional Information:© 2020 American Chemical Society. Received: August 13, 2020; Revised: October 3, 2020; Published: October 29, 2020. The authors acknowledge the Air Force Office of Scientific Research for support under award FA9550-18-1-0136. This work is based upon research conducted at the Materials Solutions Network at CHESS (MSN-C), which is supported by the Air Force Research Laboratory under award FA8650-19-2-5220. This work was also performed in part at the Cornell NanoScale Facility, a member of the National Nanotechnology Coordinated Infrastructure (NNCI), which is supported by the National Science Foundation (Grant NNCI-2025233). M.A. acknowledges support from the Swiss National Science Foundation (project P4P4P2-180669). Author Contributions: D.R.S. and A.B.C. contributed equally to this work. The authors declare no competing financial interest.
Funding AgencyGrant Number
Air Force Office of Scientific Research (AFOSR)FA9550-18-1-0136
Air Force Office of Scientific Research (AFOSR)FA8650-19-2-5220
Swiss National Science Foundation (SNSF)P4P4P2-180669
Subject Keywords:laser spike annealing, reflectance spectroscopy, high-throughput experimentation, materials transformations, metastable phases
Issue or Number:12
Record Number:CaltechAUTHORS:20201030-105644203
Persistent URL:
Official Citation:Optical Identification of Materials Transformations in Oxide Thin Films. Duncan R. Sutherland, Aine Boyer Connolly, Maximilian Amsler, Ming-Chiang Chang, Katie Rose Gann, Vidit Gupta, Sebastian Ament, Dan Guevarra, John M. Gregoire, Carla P. Gomes, R. Bruce van Dover, and Michael O. Thompson. ACS Combinatorial Science 2020 22 (12), 887-894; DOI: 10.1021/acscombsci.0c00172
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:106356
Deposited By: Tony Diaz
Deposited On:30 Oct 2020 18:14
Last Modified:16 Nov 2021 18:53

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