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. 2021 May 15;11(5):360.
doi: 10.3390/membranes11050360.

Production Strategies of TiNx Coatings via Reactive High Power Impulse Magnetron Sputtering for Selective H2 Separation

Cecilia Mortalò  1 , Silvia Maria Deambrosis  1 , Francesco Montagner  1 , Valentina Zin  1 , Monica Fabrizio  1   2 , Luca Pasquali  3   4   5 , Raffaella Capelli  3   4   5 , Monica Montecchi  3 , Enrico Miorin  1
Affiliations

Production Strategies of TiNx Coatings via Reactive High Power Impulse Magnetron Sputtering for Selective H2 Separation

Cecilia Mortalò et al. Membranes (Basel). .

Abstract

This scientific work aims to optimize the preparation of titanium nitride coatings for selective H2 separation using the Reactive High Power Impulse Magnetron Sputtering technology (RHiPIMS). Currently, nitride-based thin films are considered promising membranes for hydrogen. The first series of TiNx/Si test samples were developed while changing the reactive gas percentage (N2%) during the process. Obtained coatings were extensively characterized in terms of morphology, composition, and microstructure. A 500 nm thick, dense TiNx coating was then deposited on a porous alumina substrate and widely investigated. Moreover, the as-prepared TiNx films were heat-treated in an atmosphere containing hydrogen in order to prove their chemical and structural stability; which revealed to be promising. This study highlighted how the RHiPIMS method permits fine control of the grown layer's stoichiometry and microstructure. Moreover, it pointed out the need for a protective layer to prevent surface oxidation of the nitride membrane by air and the necessity to deepen the study of TiNx/alumina interface in order to improve film/substrate adhesion.

Keywords: TiNx film membranes; chemical robustness under h2; high power impulse magnetron sputtering; porous ceramic substrates.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
HiPIMS peak current variation (pulse time = 25 μs) while changing the nitrogen flux during the deposition process. The example cases of TiN2 (1 sccm N2), TiN3 (1.2 sccm), TiN4 (1.5 sccm N2), and TiN5 (2 sccm N2) are shown.
Figure 2
Figure 2
SEM top views and sections of samples TiN1, TiN2, and TiN5 as the deposition temperature and the percentage of reactive process gas vary.
Figure 3
Figure 3
SEM micrographs of samples TiN4A deposited on alumina.
Figure 4
Figure 4
XRD spectra deposited with N2 > 1.2 sccm.
Figure 5
Figure 5
XRD patterns collected from samples TiN1, TiN2, and TiN3, deposited at low nitrogen flow.
Figure 6
Figure 6
TiN4A XRD spectrum acquired using the grazing angle configuration.
Figure 7
Figure 7
Ti 2p XPS spectra of TiN4 (a), TiN3 (b) and TiN1 (c) samples. The spectra are shown before and after a Shirley-type background (red curves) subtraction. The spectra are also shown decomposed into Voigt-doublets (green), according to the spin-orbit splitting of Ti 2p levels. Panel (d): N 1s spectra of the three samples (without background subtraction).
Figure 8
Figure 8
SEM micrographs of samples TiN1, TiN2, TiN3, TiN4 after thermal treatment at 500 °C under H2-containig atmosphere for 20 h.
Figure 9
Figure 9
XRD spectra of samples (a) TiN2, (b) TiN3 and (c) TiN4 before and after thermal treatment at 500 °C under H2-containig atmosphere for 20 h.
Figure 9
Figure 9
XRD spectra of samples (a) TiN2, (b) TiN3 and (c) TiN4 before and after thermal treatment at 500 °C under H2-containig atmosphere for 20 h.
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