Calorimetric measurements on refractory metals and alloys by means of electromagnetic levitation (Paper No. 42)

Conventional calorimetric measurements for determining the enthalpy of solid and liquid metals or alloys have an upper temperature limit of around 1800-2000deg C. This limit is given by the thermal durability of the crucible material. To avoid these disadvantages, combination of levitation melting and drop calorimeter (levitation calorimetry) was performed in the last years. A critical analysis of the published works, however, shows that the temperature measurement and the determination of the temperature loss of the specimen during its falling period is still the problem. In consideration of these special circumstances, a levitation calorimeter was built in the Institute of Metallurgy of Technical University, Berlin. It consists of an evacuable levitation chamber. The levitation coil is connected via a transformator to a 25 KVA 500 KHz generator. The temperature of the specimen (weight 4-9 g) is measured and recorded by two different optical ways. The connected drop calorimeter is working isoperibolic. Its main part is a block of copper with a conical borehole for accepting the specimen. This copper block lies within a greater steel container which itself is in a water thermostat of a temperature 25deg C. In order to determine the calorimeter constant the calibration can be done by electrical means. To determine the temperature loss (5-10% error in enthalpy values) during the falling period between levitation coil and calorimeter many theoretical works and practical experiments have been done. First experiments on solid molybdenum in the temperature range of 2280-2750 K show a high accuracy of the measured values. Deviation from proposed ''best curve'' of Hultgreen is better than 0.3%. (auth.)