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Scanning AC nanocalorimetry combined with in-situ x-ray diffraction
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10.1063/1.4811686
/content/aip/journal/jap/113/24/10.1063/1.4811686
http://aip.metastore.ingenta.com/content/aip/journal/jap/113/24/10.1063/1.4811686

Figures

Image of FIG. 1.
FIG. 1.

Schematic of the PnSC device and calorimetry sensor. The detailed view shows the metallization within the 2.5 × 5 mm membrane. The sample deposition region shown in yellow is the same as the calorimeter measurement area. The subset of this area shown in green is the footprint of the x-ray beam.

Image of FIG. 2.
FIG. 2.

Experimental set-up used for the diffraction and nanocalorimetry measurements. The sample is located inside the chamber; the XRD measurements are performed in transmission geometry during the nanocalorimetry scan.

Image of FIG. 3.
FIG. 3.

Schematic of the data acquisition system.

Image of FIG. 4.
FIG. 4.

(a) Heat capacity and (b) corresponding scanning rates as a function of temperature for Bi for three calorimetry scans (solid lines: heating, dashed lines: cooling). The current ( , ) used for the measurements was increased linearly from (20 mA, 20 mA) to (72 mA, 72 mA) and then decreased to (12 mA, 12 mA). Measurements were performed using a frequency of 416.6 Hz. The amplitude of temperature oscillation is 6.1 K at 500 K.

Image of FIG. 5.
FIG. 5.

XRD images taken for the Bi sample at different temperatures during the nanocalorimetry scans. (a) 373 K, (b) 473 K, (c) 673 K (above melting point), and (d) 373 K (after solidification). The XRD image acquisition time was 0.1 s.

Image of FIG. 6.
FIG. 6.

(a) Heat capacity and heating rate for the Bi sample as a function of temperature, the experimental parameters are the same as in Fig. 4 ; (b) correlation of diffraction patterns and peak intensity as a function of temperature. Solid lines are for heating, dashed lines are for cooling. The vertical yellow lines mark alignment of the reaction windows in the PnSC and XRD signals. The image acquisition time was 0.1 s.

Image of FIG. 7.
FIG. 7.

Heat capacity, scanning rates, and XRD intensity for the In sample as a function of temperature for two different scans (solid lines: heating, dashed lines: cooling). (a) and (b) are results for the first measurement and (c) and (d) for second measurement. The current (I, i) used for the two measurements was increased linearly from (27 mA, 18 mA) to (86 mA, 59 mA) and then decreased to (13 mA, 9 mA). The AC frequency used was 416.6 Hz for both scans. The amplitude of temperature oscillation is 9.9 K at 500 K. The XRD image acquisition time was 0.1 s.

Image of FIG. 8.
FIG. 8.

Heat capacity, scanning rates and XRD intensity as a function of temperature for fast and slow scans on Sn (solid lines: heating, dashed lines: cooling). (a) and (b) are results for the fast measurement and (c) and (d) for slow measurement. The current (I, i) used for the fast scan was increased linearly from (20 mA, 20 mA) to (72 mA, 72 mA) and then decreased to (12 mA, 12 mA). The current (I, i) used for the slow scan was increased linearly from (8 mA, 8 mA) to (71 mA, 71 mA) and then decreased to (5 mA, 5 mA). The AC frequency used was 416.6 Hz for the fast scan and 99.2 Hz for the slow scan. The amplitude of temperature oscillation at 500 K is 5.9 K for fast scan and 27.7 K for slow scan. The XRD image acquisition time was 0.1 s for fast scan and 2 s for slow scan.

Image of FIG. 9.
FIG. 9.

Optical image of Sn sample after many melting cycles.

Tables

Generic image for table
Table I.

Sample deposition parameters.

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/content/aip/journal/jap/113/24/10.1063/1.4811686
2013-06-24
2014-04-17
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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: Scanning AC nanocalorimetry combined with in-situ x-ray diffraction
http://aip.metastore.ingenta.com/content/aip/journal/jap/113/24/10.1063/1.4811686
10.1063/1.4811686
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