Elsevier

Cryogenics

Volume 51, Issue 8, August 2011, Pages 460-464
Cryogenics

A sample-saving method for heat capacity measurements on powders using relaxation calorimetry

https://doi.org/10.1016/j.cryogenics.2011.04.011Get rights and content
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Abstract

An experimental method is described for determining the low-temperature heat capacity (Cp) of mg-sized powder samples using the Quantum Design “Physical Properties Measurement System” (PPMS). The powder is contained in an Al pan as an ∼1 mm thick compressed layer. The sample is not mixed with Apiezon N grease, as compared to other methods. Thus, it is not contaminated and can be used for further study. This is necessary for samples that are only available in tiny amounts. To demonstrate the method various samples, all insulating in nature, were studied including benzoic acid, sapphire and different silicate minerals. The measurements show that the method has an accuracy in Cp to better than 1% at T above 30–50 K and ±3–5% up to ±10% below. The experimental procedure is based on three independent PPMS and three independent differential scanning calorimetry (DSC) measurements. The DSC Cp data are used to slightly adjust the PPMS Cp data by a factor CpDSC/CpPPMSat298K. This is done because heat capacities measured with a DSC device are more accurate around ambient T (⩽0.6%) than PPMS values and is possible because the deviation of PPMS heat capacities from reference values is nearly constant between about 50 K and 300 K. The resulting standard entropies agree with published reference values within 0.21% for the silicates, by 0.34% for corundum, and by 0.9% for powdered benzoic acid. The method thus allows entropy determinations on powders with an accuracy of better than 1%. The advantage of our method compared to other experimental techniques is that the sample powder is not contaminated with grease and that heat capacity values show less scatter at high temperatures.

Highlights

► A method for low-temperature heat capacity measurements on powders is presented. ► The method is based on combined PPMS and DSC measurements. ► It allows entropy determinations on powders with an accuracy of better than 1%. ► The sample is not mixed with Apiezon N grease during measurement. ► This is useful for samples that are only available in tiny amounts.

Keywords

Relaxation calorimetry
Powder
PPMS
Low-temperature heat capacity

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