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Thin Film Calorimetry - Device Development and Application to Lithium Ion Battery Materials

Published online by Cambridge University Press:  01 February 2013

Hendrik Wulfmeier ,
Daniel Albrecht ,
Svetlozar Ivanov ,
Julian Fischer ,
Rolf Grieseler ,
Peter Schaaf ,
Sven Ulrich ,
Andreas Bund  and
Holger Fritze
Hendrik Wulfmeier
Affiliation:
Institute of Energy Research and Physical Technologies, Clausthal University of Technology, Am Stollen 19 B, D-38640 Goslar, Germany
Daniel Albrecht
Affiliation:
Institute of Energy Research and Physical Technologies, Clausthal University of Technology, Am Stollen 19 B, D-38640 Goslar, Germany
Svetlozar Ivanov
Affiliation:
Department of Electrochemistry and Electroplating, Ilmenau University of Technology, Gustav-Kirchhoff-Straße 6, D-98693 Ilmenau, Germany
Julian Fischer
Affiliation:
Institute for Applied Materials (IAM-AWP), Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, D-76344 Eggenstein-Leopoldshafen, Germany
Rolf Grieseler
Affiliation:
Department of Materials for Electrical Engineering, Ilmenau University of Technology, Gustav-Kirchhoff-Straße 6, D-98693 Ilmenau, Germany
Peter Schaaf
Affiliation:
Department of Materials for Electrical Engineering, Ilmenau University of Technology, Gustav-Kirchhoff-Straße 6, D-98693 Ilmenau, Germany
Sven Ulrich
Affiliation:
Institute for Applied Materials (IAM-AWP), Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, D-76344 Eggenstein-Leopoldshafen, Germany
Andreas Bund
Affiliation:
Department of Electrochemistry and Electroplating, Ilmenau University of Technology, Gustav-Kirchhoff-Straße 6, D-98693 Ilmenau, Germany
Holger Fritze
Affiliation:
Institute of Energy Research and Physical Technologies, Clausthal University of Technology, Am Stollen 19 B, D-38640 Goslar, Germany
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Abstract

The work takes advantage of a newly developed measurement system which enables to investigate the thermodynamic properties of thin films including battery layer sequences. This technique, Thin-Film Calorimetry (TFC), is based on the detection of resonance frequency shifts of bulk acoustic wave resonators. Thin films with a thickness of several micrometers of the material of interest are deposited on the resonators. By measuring the temperature dependent shift of the resonance frequency, the device is working as a precise temperature sensor. The production or consumption of latent heat by the active layer(s) results in temperature fluctuations with respect to the furnace where the sensor is placed. Those information enable to extract the temperature and time dependence of phase transformations as well as the associated enthalpies. To cover a temperature range from -20 to 900 °C high-temperature stable piezoelectric resonators made of langasite crystals (La3Ga5SiO14) are applied.

Initially, metallic layers of tin and aluminum are used to test and verify this approach. The temperatures and enthalpies of solid-liquid as well as of solid-solid phase transformation are observed in the correct manner. Further, the thermodynamic data of the battery materials Li(Ni0.8Co0.15Al0.05)O2-δ (NCA) and LiMn2O4-δ (LMO) obtained by TFC are determined and discussed. Both cathode materials are amorphous after deposition and show crystallization during heating at 460 °C (NCA) and 600 °C (LMO). The associated enthalpies are 5.3 kJ/mol (55 J/g) and 17.3 kJ/mol (96 J/g), respectively.

Keywords

calorimetrythin filmenergy storage
Type
Articles
Information
MRS Online Proceedings Library (OPL) , Volume 1496: Symposium J – Materials for Sustainable Development—Challenges and Opportunities , 2013 , mrsf12-1496-j16-06
Copyright
Copyright © Materials Research Society 2013

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References

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