How to measure routinely specific heats of solids below 150K?

Gmelin, E.; Ripka, K.

doi:10.1016/0040-6031(85)85576-3

Cited by 5 publications

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“…The measurement of the heat capacity Cp provides the fundamental thermal parameters concerning the energy states of solids and liquids, thermodynamic functions and phase transitions. In spite of the rapid development in instrumentation and automatization in the last 15 years [1][2][3][4], the overwhelming number of calorimetric investigations still remains restricted to temperatures above 120 K. Nevertheless, design and handling of adiabatic low temperature calorimeters for routine measurements were simplified and the necessary sample masses were reduced substantially to 0.2-0.5 g [5][6][7]. In order to determine s'till smaller heat capacities, in particular of very small samples, (m < 50 mg) new experimental techniques were developed.…”

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Disc — A differential isoperibol scanning calorimeter

Brill

Gmelin

1988

Journal of Thermal Analysis

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The construction and operation of a new fully automated microcalorimeter is described. This instrument allows specific heat measurements to be performed on small samples in the I0 mgrange at low temperatures (10 K < T <: 350 K). The new method consists of combining the nonadiabatic relaxation-time'calorimetry with a twin arrangement and simultaneous temperature scanning. Some experimental details of the calorimeter and sample holders are presented. The accuracy of the calorimeter was verified by calibration measurements on 56 mg of copper. An energy resolution of 0.t #J/K has been reached near 12 K. To demonstrate the reliability of the microcalorimeter the heat capacity of the new high Tc superconductor YBa2CU3OT_y was determined.Calorimetry is a powerful tool for the entire field of natural science. The measurement of the heat capacity Cp provides the fundamental thermal parameters concerning the energy states of solids and liquids, thermodynamic functions and phase transitions. In spite of the rapid development in instrumentation and automatization in the last 15 years [1][2][3][4], the overwhelming number of calorimetric investigations still remains restricted to temperatures above 120 K. Nevertheless, design and handling of adiabatic low temperature calorimeters for routine measurements were simplified and the necessary sample masses were reduced substantially to 0.2-0.5 g [5][6][7]. In order to determine s'till smaller heat capacities, in particular of very small samples, (m < 50 mg) new experimental techniques were developed. Among these techniques the non-adiabatic AC-method [8] and the relaxation-time method [9] tumed out to be the most profitable ones. Both have found a wide spread application and have been further developed and modified [10,11]. A focal point for todays materials science research is to make calorimetric measurements in the extreme small mass regime (1-50 mg) more routine and more accurate. In this contribution we describe some essential features as the principle, construction and operation of a new automated microcalorimeter [12]. In our opinion this instrument meets all requirements to determine heat capacities of small samples in the 10 mg range between 10 K room temperature.

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