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High-temperature chip calorimeter with atmosphere control

Guenther, G. ; Aulbach, E. ; Hahn, H. ; Guillon, O. (2011):
High-temperature chip calorimeter with atmosphere control.
In: Thermochimica Acta, 522 (1-2), pp. 77-85. Elsevier Science Publishing Company, ISSN 00406031,
[Article]

Abstract

A nanocalorimeter operating in various gas atmospheres and under controllable pressure at temperatures at least up to 1093 K is presented. It was developed to investigate nano-sized samples like nanoparticles and thin films under variable conditions. A special chip with two facing measurement cells for differential measurements was designed. Each cell consists of a thin, free-standing beam of silicon nitride instead of a continuous membrane. Joule heaters and temperature sensors are located at the tip of the SiN cantilevers. The calorimeter chip is mounted in a mobile measurement chamber that allows for preparation of surface-sensitive materials in a glove box. Subsequently the chamber is transferred to the measurement device. The chips are operated as AC calorimeter for sensitive detection of phase transitions. The functionality was demonstrated by calibration with different reference substances. Frequency scans with varying temperatures and gas atmospheres were performed to test the frequency dependency of the chip.

Item Type: Article
Erschienen: 2011
Creators: Guenther, G. ; Aulbach, E. ; Hahn, H. ; Guillon, O.
Title: High-temperature chip calorimeter with atmosphere control
Language: English
Abstract:

A nanocalorimeter operating in various gas atmospheres and under controllable pressure at temperatures at least up to 1093 K is presented. It was developed to investigate nano-sized samples like nanoparticles and thin films under variable conditions. A special chip with two facing measurement cells for differential measurements was designed. Each cell consists of a thin, free-standing beam of silicon nitride instead of a continuous membrane. Joule heaters and temperature sensors are located at the tip of the SiN cantilevers. The calorimeter chip is mounted in a mobile measurement chamber that allows for preparation of surface-sensitive materials in a glove box. Subsequently the chamber is transferred to the measurement device. The chips are operated as AC calorimeter for sensitive detection of phase transitions. The functionality was demonstrated by calibration with different reference substances. Frequency scans with varying temperatures and gas atmospheres were performed to test the frequency dependency of the chip.

Journal or Publication Title: Thermochimica Acta
Journal volume: 522
Number: 1-2
Publisher: Elsevier Science Publishing Company
Uncontrolled Keywords: Nanocalorimetry, AC calorimetry, Instrument, High temperature, Nanoscaled samples, Oxides
Divisions: 11 Department of Materials and Earth Sciences > Material Science > Joint Research Laboratory Nanomaterials
11 Department of Materials and Earth Sciences > Material Science > Nonmetallic-Inorganic Materials
11 Department of Materials and Earth Sciences > Material Science
11 Department of Materials and Earth Sciences
Date Deposited: 19 Feb 2013 09:07
Official URL: http://dx.doi.org/10.1016/j.tca.2011.03.013
Additional Information:

Special Issue: Interplay between Nucleation, Crystallization, and the Glass Transition

Identification Number: doi:10.1016/j.tca.2011.03.013
Funders: We acknowledge the financial support of the Deutsche Forschungsgemeinschaft (DFG) within the frame of the Emmy Noether program (GU 993/1-1)., The authors are grateful to the “Joint Research Laboratory Nanomaterials Karlsruhe Institure of Technology and Technische Universität Darmstadt” and the State of Hessen for funding the calorimeter setup as a joint research project., We thank Xensor Integration for the joint chip development process.
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