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Self-organized Nanostructuring in Zr0.64Al0.36N Thin Films Studied by Atom Probe Tomography
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Dept. of Applied Physics, Chalmers University of Technology, Göteborg, Sweden.
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2016 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, p. 233-238Article in journal (Refereed) Published
Abstract [en]

We have applied atom probe tomography (apt) to analyze the selforganized structure of wear-resistant Zr0.64Al0.36N thin films grown by magnetron sputtering. Transmission electron microscopy shows that these films grow as a two-dimensional nanocomposite, consisting of interleaved lamellae in a labyrinthine structure, with a size scale of ∼ 5 nm. The structure was recovered in the Al apt signal, while the Zr and N data lacked structural information due to severe local magnification effects. The onset of the self-organized growth was observed to occur locally by nucleation, at 5-8 nm from the MgO substrate, after increasing Zr-Al compositional fluctuations. Finally, it was observed that the self-organized growth mode could be perturbed by renucleation of ZrN.

Place, publisher, year, edition, pages
Elsevier, 2016. p. 233-238
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-84258DOI: 10.1016/j.tsf.2016.07.034ISI: 000381939700037OAI: oai:DiVA.org:liu-84258DiVA, id: diva2:558393
Note

Funding agencies: VINN Excellence Center on Functional Nanoscale Materials; Swedish Research Council; Swedish Government Strategic Faculty Grant in Materials Science (SFO Mat-LiU) at Linkoping University; Swedish Governmental Agency for Innovation Systems (Vinnova) [2011-0

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Available from: 2012-10-03 Created: 2012-10-03 Last updated: 2019-08-02Bibliographically approved
In thesis
1. Inside The Miscibility Gap: Nanostructuring and Phase Transformations in Hard Nitride Coatings
Open this publication in new window or tab >>Inside The Miscibility Gap: Nanostructuring and Phase Transformations in Hard Nitride Coatings
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis is concerned with self-organization phenomena in hard and wear resistant transition-metal nitride coatings, both during growth and during post deposition thermal annealing. The uniting physical principle in the studied systems is the immiscibility of their constituent parts, which leads, under certain conditions, to structural variations on the nanoscale. The study of such structures is challenging, and during this work atom probe tomography (apt) was developed as a viable tool for their study. Ti0.33Al0.67N was observed to undergo spinodal decomposition upon annealing to 900 °C, by the use of apt in combination with electron microscopy. The addition of C to TiSiN was found to promote and refine the feather-like microstructure common in the system, with an ensuing decrease in thermal stability. An age-hardening of 36 % was measured in arc evaporated Zr0.44Al0.56N1.20, which was a nanocomposite of cubic, hexagonal, and amorphous phases. Magnetron sputtering of Zr0.64Al0.36N at 900 °C resulted in a self-organized and highly ordered growth of a two-dimensional two-phase labyrinthine structure of cubic ZrN and wurtzite AlN.The structure was analyzed and recovered by apt, although the ZrN phase suffered from severe trajectory aberrations, rendering only the Al signal useable.The initiation of the organized growth was found to occur by local nucleation at 5-8 nm from the substrate, before which random fluctuations in Al/Zr content increased steadily from the substrate. Finally, the decomposition of solid-solution TiB0.33N0.67 was found, by apt, to progress through the nucleation of TiB0.5N0.5 and TiN, followed by the transformation of the former into hexagonal TiB2.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2012. p. 69
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1472
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-84263 (URN)978-91-7519-809-5 (ISBN)
Public defence
2012-10-19, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2012-10-03 Created: 2012-10-03 Last updated: 2016-08-31Bibliographically approved
2. Atom Probe Tomography of Hard Nitride and Boride Thin Films
Open this publication in new window or tab >>Atom Probe Tomography of Hard Nitride and Boride Thin Films
2019 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Hard ceramic thin films, including TiSiN, ZrAlN, ZrB2, and ZrTaB2, with applications for wear-resistant coatings, have been studied using atom probe tomography and correlated with several other analytical techniques, including X-ray diffraction, electron microscopy, and elastic recoil detection analysis. Outstanding obstacles for quantitative atom probe tomography of ceramic thin films have been surmounted.

Mass spectral overlaps in TiSiN, which make 28Si indistinguishable from 14N, was resolved by isotopic substitution with 15N, and the nanostructural distribution of elements was thus revealed in 3-D, which enabled the identification of additional structural elements within the nanostructured Ti0.81Si0.1915N film. Improvements to the growth model of TiSiN by cathodic arc deposition was suggested.

A self-organized nanolabyrinthine structure of ZrAlN, consisting of standing lamellae of fcc-ZrN and hexagonal AlN, was investigated with focus on the onset and limits of the self-organization. The local crystallographic orientational relationships were (001)ZrN || (0001)AlN and <110>ZrN || <2-1-10>AlN. Close to the MgO substrates, a smooth transition region was formed, going from segregated and disordered to the self-organized nanolabyrinthine structure. With increased growth temperature, coarse (111)-oriented ZrN grains occasionally precipitated and locally replaced the nanolabyrinthine structure. Significant local magnification effects rendered the Zr and N signals unusable, thereby inhibiting quantitative compositional analysis of the constituent phases, but the nanostructure was resolved using the Al signal.

Ceramic materials are often affected by correlated evaporation, which can result in losses due to the detector dead-time/space. A compositional correction procedure was suggested, tested against an established procedure, and applied to ZrB2. The correction was found to be less dependent on the isotope abundances and background correction compared to the established procedure. While losses due to dead-time/space occur in atom probe tomography of all materials, the correlative field evaporation behavior of ceramics significantly increases the compositional error. The evaporation behavior of ZrB2 was therefore thoroughly investigated and evidence of preferential retention, correlated evaporation, and inhomogeneous field distributions at a low-index pole was presented. The high mass resolution, relatively low multiple events percentage, and quality of the co-evaporation correlation data was partly attributed to the crystal structure and film orientation, which promoted a layer-by-layer field evaporation.

The evaporation behavior of the related ZrTaB2 films was found to be similar to that of ZrB2. The distribution of Ta in relation to Zr was investigated, showing that the column boundaries were both metal- and Ta-rich, and that there was a significant amount of Ta in solid solution within the columns.

In addition, an instrumental artefact previously not described in atom probe tomography was found in several of the materials investigated in this thesis. The artefact consists of high-density lines along the analysis direction, which cannot be related to pole artefacts. The detection system of the atom probe was identified as the cause, because the artefact patterns on detector histograms coincided with the structure of the microchannel plate. Inconsistencies in the internal boundaries of the microchannel plate multifibers from the manufacturing process can influence the signal to the detector and locally increase the detection efficiency in a pattern characteristic to the microchannel plate in question.

Altogether, this thesis shows that atom probe tomography of nitride and boride thin films is burdened by several artefacts and distortions, but that relevant material outcomes can nevertheless be achieved by informed choices of film isotopic constituents and analytical parameters, exclusion of heavily distorted regions (such as pole artefacts), and the use of compositional correction procedures when applicable.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2019. p. 79
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1995
Keywords
Materials science, Atom probe tomography (APT), Ceramics, Nitrides, Borides
National Category
Physical Sciences Materials Engineering Ceramics
Identifiers
urn:nbn:se:liu:diva-159187 (URN)10.3384/diss.diva-159187 (DOI)9789176850435 (ISBN)
Public defence
2019-09-13, Planck, Fysikhuset, Campus Valla, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2019-08-02 Created: 2019-08-01 Last updated: 2019-09-20Bibliographically approved

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Johnson, LarsGhafoor, NaureenEngberg, DavidOdén, MagnusHultman, Lars

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