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Figure 3
(a) The measured temperature (reference thermocouple) plotted against the calibrated temperature determined by lattice parameters (solid circles) and some melting points (X symbols). (b) The same plot as (a) but as a difference between measured and calibrated. (c) Logged thermocouple data of a ramp to 1000°C and then to 1200°C at 100°C min−1. (d) Contour plot of XRD patterns of Ag collected during a heating ramp to above its melting point (square root of intensity on colour-axis). Reference thermocouple temperature data are shown on the right-hand side of the plot. The phase which appears at around 40 min (941°C on thermocouple, 892°C calibrated, most prominent peak at ∼11.8°) is the quartz capillary crystallising at the elevated temperatures. Data collected at BM01, ESRF. |
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