Measurement of Al Freezing-Point Temperature: Effect of Initiation Process

Abstract

In CCT documents it is stated that "…for the freezing curves of the metallic fixed points, the maximum observed temperature on the plateau should be taken as the best approximation of the liquidus temperature. The fixed points should be realized with the inner and outer liquid-solid interfaces and extend past the maximum by 10 % to 20 % of the fraction frozen, to clearly establish the value of the maximum and the resolution of its determination." Also, it is accepted that "…the inner interface is essentially static. It is the temperature of the inner liquid/solid interface that is measured by the thermometer." The analysis of freezing curves obtained by the standard method of fixed-point realization shows that the parameters of the initial part of the freezing curve, the mean temperature value of which is usually taken as the liquidus temperature, depend on how the inner interface is initiated. Variations in the duration and intensity of initiation cause changes in the initial part of the freezing curve and in the resulting SPRT measurement. Moreover, the relation between the duration of the initial section of the plateau with a minor temperature change and the duration of its final section with a significant slope also depend on the initiation method used and on the furnace temperature. The effect of freezing initiation conditions on the measurement result is individual for each fixed point because of the differences in thermophysical properties of metals and in conditions of the heat transfer from the liquid-solid interface to the thermometer. Aluminum has a maximum value of the melting specific heat in comparison with other metals used in ITS-90 fixed points; in the present study, the effect of the intensity and duration of the inner liquid-solid interface initiation was investigated both experimentally and through calculation.

Improved Initiation Technique for the Metal Fixed Points

“…3 and 5 have been observed in zinc by Ivanova and Il'in [18] and in aluminum by Abasov et al [19]. As shown in the figures, there is an increase in the realized temperature with increasing cooling of the thermometer well.…”

Measurement of the in freezing-point temperature: Effect of the liquid-solid interface structure

“…Estimates of the thickness were obtained from the amount of heat removed by the rod using the calculation method similar to that in [12]. The discrepancy between experimental and calculation data is caused by the fact that the evaluation of the thickness was performed on the principle that all the mass of frozen indium is accumulated in the film on the well surface.…”