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Atom probe tomography field evaporation characteristics and compositional corrections of ZrB2
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Department of Physics, Chalmers University of Technology, Göteborg, Sweden.
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2019 (English)In: Materials Characterization, ISSN 1044-5803, E-ISSN 1873-4189, Vol. 156, article id 109871Article in journal (Refereed) Published
Abstract [en]

The microstructure of stoichiometric ZrB2.0 and B over-stoichiometric ZrB2.5 thin films has been studied using atom probe tomography (APT), X-ray diffraction, and transmission electron microscopy. Both films consist of columnar ZrB2 grains with AlB2-type crystal structure. The narrow stoichiometry range of ZrB2 results in the presence of separate disordered B-rich boundaries even in ZrB2.0. At higher average B content, specifically ZrB2.5, the formation of a continuous network around the sides of the ZrB2 columns is promoted. In addition, the APT field evaporation characteristics of ZrB2 and its influence on the measured local composition has been studied and compared to the average composition from elastic recoil detection analysis (ERDA). Differences in the measured average compositions of the two techniques are explained by the APT detector dead-time/space. A new pile-up pairs correction procedure based on co-evaporation correlation data was thus employed here for the APT data and compared with the 10B-method (the B equivalence of the 13C-method), as well as the combination of both methods. In ZrB2.0, all of the applied compositional correction methods were found to reduce the compositional difference when appropriate isotopic abundances were used. In ZrB2.5, the inhomogeneity of the film likely increased the local APT composition to such an extent that even conservative correction procedures overestimated the B content compared to the ERDA reference. The strengths of the pile-up pairs correction compared the 10B and the combined methods are higher precision, due to it being less dependent on the accuracy of estimated isotopic abundances, and that the correction itself is not dependent on careful background correction of the mass spectrum.

Place, publisher, year, edition, pages
Elsevier, 2019. Vol. 156, article id 109871
Keywords [en]
Atom probe tomography (APT), Zirconium diboride (ZrB), Field evaporation characteristics of borides, Elastic recoil detection analysis (ERDA), Compositional correction procedures, Transition metal diborides
National Category
Physical Sciences
Identifiers
URN: urn:nbn:se:liu:diva-160356DOI: 10.1016/j.matchar.2019.109871ISI: 000487565900025OAI: oai:DiVA.org:liu-160356DiVA, id: diva2:1352748
Available from: 2019-09-19 Created: 2019-09-19 Last updated: 2019-11-04Bibliographically approved
In thesis
1. 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)
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Supervisors
Available from: 2019-08-02 Created: 2019-08-01 Last updated: 2019-09-20Bibliographically approved

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Engberg, David L. J.Tengdelius, LinaHögberg, HansHultman, Lars

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