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

Micromachined nanocalorimetry sensors have shown excellent performance for hightemperature 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. a) e-mail address: [email protected] b) This research was performed while the author was at the School of Engineering and Applied Sciences, Harvard University, 29 Oxford Street, Cambridge, MA 02138, USA c) These authors contributed equally to this work.