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Scanning AC nanocalorimetry combined with in-situ x-ray diffraction

Xiao, Kechao and Gregoire, John M. and McCluskey, Patrick J. and Dale, Darren and Vlassak, Joost J. (2013) Scanning AC nanocalorimetry combined with in-situ x-ray diffraction. Journal of Applied Physics, 113 (24). Art. No. 243501. ISSN 0021-8979. PMCID PMC3676369. doi:10.1063/1.4811686.

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Micromachined nanocalorimetry sensors have shown excellent performance for high-temperature and high-scanning rate calorimetry measurements. Here, we combine scanning AC nanocalorimetry with in-situ x-ray diffraction (XRD) to facilitate interpretation of the calorimetry measurements. Time-resolved XRD during in-situ operation of nanocalorimetry sensors using intense, high-energy synchrotron radiation allows unprecedented characterization of thermal and structural material properties. We demonstrate this experiment with detailed characterization of the melting and solidification of elemental Bi, In, and Sn thin-film samples, using heating and cooling rates up to 300 K/s. Our experiments show that the solidification process is distinctly different for each of the three samples. The experiments are performed using a combinatorial device that contains an array of individually addressable nanocalorimetry sensors. Combined with XRD, this device creates a new platform for high-throughput mapping of the composition dependence of solid-state reactions and phase transformations.

Item Type:Article
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URLURL TypeDescription DOIArticle CentralArticle
Gregoire, John M.0000-0002-2863-5265
Additional Information:© 2013 AIP Publishing LLC. Received 23 April 2013; accepted 6 June 2013; published online 24 June 2013. The authors thank Aaron Lyndaker for assistance with the synchrotron experiments and James MacArthur for assistance with the custom electronics. The work presented in this paper was supported by the Air Force Office of Scientific Research under Grant Nos. FA9550-08-1-0374 and FA9550-12-1-0098 and by the Materials Research Science and Engineering Center at Harvard University (NSF-DMR-0820484). The measurements were performed at the Cornell High Energy Synchrotron source (CHESS), which is supported by the National Science Foundation and the National Institutes of Health/National Institute of General Medical Sciences under NSF Award No. DMR-0936384. The sensors were fabricated at the Center for Nanoscale Systems, a member of the National Nanotechnology Infrastructure Network, which is supported by the National Science Foundation under NSF Award No. ECS-0335765. The Center for Nanoscale Systems is part of the Faculty of Arts and Sciences at Harvard University.
Funding AgencyGrant Number
Air Force Office of Scientific Research (AFOSR)FA9550-08-1-0374
Air Force Office of Scientific Research (AFOSR)FA9550-12-1-0098
Subject Keywords:bismuth, calorimetry, cooling, indium, melting, metallic thin films, nanosensors, solidification, tin, X-ray diffraction
Issue or Number:24
Classification Code:PACS: 85.85.+j; 07.20.Fw; 07.10.Cm; 07.07.Df
PubMed Central ID:PMC3676369
Record Number:CaltechAUTHORS:20130830-140035652
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Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:41039
Deposited By: Tony Diaz
Deposited On:30 Aug 2013 21:20
Last Modified:10 Nov 2021 04:25

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