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. 2022 Feb 22;15(5):1635.
doi: 10.3390/ma15051635.

Ag Surface and Bulk Segregations in Sputtered ZrCuAlNi Metallic Glass Thin Films

Michael K Steinhoff  1 , Damian M Holzapfel  1 , Soheil Karimi Aghda  1 , Deborah Neuß  1 , Peter J Pöllmann  1 , Marcus Hans  1 , Daniel Primetzhofer  2 , Jochen M Schneider  1 , Clio Azina  1
Affiliations

Ag Surface and Bulk Segregations in Sputtered ZrCuAlNi Metallic Glass Thin Films

Michael K Steinhoff et al. Materials (Basel). .

Abstract

We report on the formation of Ag-containing ZrCuAlNi thin film metallic glass (nano)composites by a hybrid direct-current magnetron sputtering and high-power pulsed magnetron sputtering process. The effects of Ag content, substrate temperature and substrate bias potential on the phase formation and morphology of the nanocomposites were investigated. While applying a substrate bias potential did not strongly affect the morphological evolution of the films, the Ag content dictated the size and distribution of Ag surface segregations. The films deposited at low temperatures were characterized by strong surface segregations, formed by coalescence and Ostwald ripening, while the volume of the films remained featureless. At higher deposition temperature, elongated Ag segregations were observed in the bulk and a continuous Ag layer was formed at the surface as a result of thermally enhanced surface diffusion. While microstructural observations have allowed identifying both surface and bulk segregations, an indirect method for detecting the presence of Ag segregations is proposed, by measuring the electrical resistivity of the films.

Keywords: electrical resistivity; nanocomposites; segregation; thin film metallic glass.

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Conflict of interest statement

The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to publish the results.

Figures

Figure 1
Figure 1
Schematic of target positioning in the ultra-high vacuum (UHV) chamber. The grey disc, on the right-hand side, represents the fourth magnetron of the chamber which was not used during depositions.
Figure 2
Figure 2
(a) High-angle annular dark field scanning transmission electron microscopy (HAADF STEM) image of the ZrCuAlNi film deposited at 200 °C with direct current magnetron sputtering (DCMS) and (b) energy-dispersive X-ray spectroscopy (EDX) line scan measured along the arrow represented in (a). (c) X-ray diffraction of thin-film metallic glasses (TFMGs) deposited at 60, 200 and 400 °C.
Figure 3
Figure 3
X-ray diffractograms (XRD) of TFMG and Ag-containing TFMGs deposited without substrate bias potential at (a) 60 and (b) 200 °C.
Figure 4
Figure 4
Scanning electron microscopy (SEM) surface micrographs of films of different Ag contents deposited at (a–c) floating potential; 60 °C, (d–f) −80 V; 60 °C, (g–i) floating potential; 200 °C, and (j–l) −80 V; 200 °C.
Figure 5
Figure 5
STEM cross-sectional HAADF images and corresponding EDX line scans of the films deposited at 200 °C, under floating potential, containing (a,b) 7.5, (c,d) 15, and (e,f) 30 at.% Ag.
Figure 6
Figure 6
(a) Elemental reconstruction of Zr, Cu, Al, and Ni positions, and (b) concentration profile of the cylindrical region indicated in (a), of the pure TFMG, deposited without bias at 60 °C. (c) Reconstruction of Zr, Cu, Al, Ni, and Ag positions, and (d) concentration profile of the cylindrical region indicated in (c), of the TFMG containing 30 at.% Ag, deposited without bias at 60 °C.
Figure 7
Figure 7
Electrical resistivities of films deposited with (continuous lines) and without (dotted lines) bias at 60 (blue) and 200 °C (red), for the different Ag contents, accompanied by corresponding cross-section SEM (30 at.% Ag, floating, 60 °C) and STEM images (7.5–30 at.% Ag, floating, 200 °C).
See this image and copyright information in PMC

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