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Zeilinger A, Todt J, Krywka C, et al. In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation. Sci Rep. 2016;6:22670doi: 10.1038/srep22670.
Zeilinger, A., Todt, J., Krywka, C., Müller, M., Ecker, W., Sartory, B., Meindlhumer, M., Stefenelli, M., Daniel, R., Mitterer, C., & Keckes, J. (2016). In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation. Scientific reports, 622670. https://doi.org/10.1038/srep22670
Zeilinger, Angelika, et al. "In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation." Scientific reports vol. 6 (2016): 22670. doi: https://doi.org/10.1038/srep22670
Zeilinger A, Todt J, Krywka C, Müller M, Ecker W, Sartory B, Meindlhumer M, Stefenelli M, Daniel R, Mitterer C, Keckes J. In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation. Sci Rep. 2016 Mar 07;6:22670. doi: 10.1038/srep22670. PMID: 26947558; PMCID: PMC4780078.
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Sci Rep. 2016 Mar 07;6:22670. doi: 10.1038/srep22670.

In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation.

Scientific reports

Angelika Zeilinger, Juraj Todt, Christina Krywka, Martin Müller, Werner Ecker, Bernhard Sartory, Michael Meindlhumer, Mario Stefenelli, Rostislav Daniel, Christian Mitterer, Jozef Keckes

Affiliations

  1. Materials Center Leoben Forschung GmbH, Leoben, Austria.
  2. Department of Materials Physics, Montanuniversität Leoben, Austria.
  3. Ruprecht Haensel Laboratory, University of Kiel, Germany.
  4. Helmholtz Zentrum Geesthacht, Geesthacht, Germany.
  5. Department of Physical Metallurgy and Materials Testing, Montanuniversität Leoben, Austria.

PMID: 26947558 PMCID: PMC4780078 DOI: 10.1038/srep22670

Abstract

Load-displacement curves measured during indentation experiments on thin films depend on non-homogeneous intrinsic film microstructure and residual stress gradients as well as on their changes during indenter penetration into the material. To date, microstructural changes and local stress concentrations resulting in plastic deformation and fracture were quantified exclusively using numerical models which suffer from poor knowledge of size dependent material properties and the unknown intrinsic gradients. Here, we report the first in-situ characterization of microstructural changes and multi-axial stress distributions in a wedge-indented 9 μm thick nanocrystalline TiN film volume performed using synchrotron cross-sectional X-ray nanodiffraction. During the indentation, needle-like TiN crystallites are tilted up to 15 degrees away from the indenter axis in the imprint area and strongly anisotropic diffraction peak broadening indicates strain variation within the X-ray nanoprobe caused by gradients of giant compressive stresses. The morphology of the multiaxial stress distributions with local concentrations up to -16.5 GPa correlate well with the observed fracture modes. The crack growth is influenced decisively by the film microstructure, especially by the micro- and nano-scopic interfaces. This novel experimental approach offers the capability to interpret indentation response and indenter imprint morphology of small graded nanostructured features.

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