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. 2025 Feb 21;15(3):68.
doi: 10.3390/membranes15030068.

Titanium Nitride as an Intermetallic Diffusion Barrier for Hydrogen Permeation in Palladium-Vanadium Composite Membranes

Cameron M Burst  1 , Chao Li  2 , Douglas Way  2 , Colin A Wolden  1   2
Affiliations

Titanium Nitride as an Intermetallic Diffusion Barrier for Hydrogen Permeation in Palladium-Vanadium Composite Membranes

Cameron M Burst et al. Membranes (Basel). .

Abstract

Hydrogen purification is a critical industrial process, and there are ongoing efforts to develop low-cost alternatives to palladium foil membranes. Titanium nitride (TiN) is studied as an interdiffusion barrier to enable hydrogen permeation in composite palladium-vanadium membranes. TiN was deposited via reactive sputtering, and films with the desired (200) orientation were obtained in the metallic regime at 400 °C under a 200 V bias to the substrate. The permeability of thin-film TiN was determined with palladium-based sandwich structures. TiN layers up to 10 nm resulted in a minimal decrease in flux (~20%) relative to a freestanding PdCu foil, which was attributed to the interfacial resistance. At greater thicknesses, the TiN layer was rate-limiting, and it was found that the effective permeability of the sputtered TiN thin films was ~6 × 10-12 mol s-1 m-1 Pa-0.5. Composite Pd|TiN|V|TiN|Pd membranes exhibited permeability values up to three times greater than pure palladium, exhibiting stability at 450 °C for over 100 h, with the lack of intermetallic diffusion and alloy formation being confirmed with XRD. The membranes were unstable at 500 °C, which was attributed to the instability of the thin Pd layer and loss of catalytic activity.

Keywords: diffusion barrier; hydrogen membranes; intermetallic diffusion; palladium; titanium nitride; vanadium.

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Conflict of interest statement

The authors declare no conflicts of interest.

Figures

Figure 1
Figure 1
The measured deposition rate of TiN as a function of the sputter ambient concentration at both room temperature (blue) and 400 °C (red). Samples deposited at 0% N2 are metallic titanium and indicated with triangles to distinguish from TiN (circles).
Figure 2
Figure 2
The XRD pattern of 100 nm thick TiN deposited on silicon at room temperature and at 400 °C with no applied bias.
Figure 3
Figure 3
(a) The measured deposition rate (red, left axis) and resistivity (blue, right axis) of 100 nm TiN films on glass as a function of applied reverse RF bias. (b) XRD patterns of 100 nm TiN films on silicon as a function of applied bias.
Figure 4
Figure 4
H2 permeance versus inverse TiN thickness for Pd|TiN|PdCu membranes at 400 °C. The value of an uncoated PdCu foil is included for reference.
Figure 5
Figure 5
The H2 permeability through a 5 nm Pd|TiN|V|TiN|Pd composite membrane as a function of time at selected temperatures. The horizontal lines indicate the theoretical permeability of pure Pd at the selected temperature.
Figure 6
Figure 6
Arrhenius plot comparing the permeability of Pd|TiN|V|TiN|Pd membranes with values of Pd and V from the literature.
Figure 7
Figure 7
XRD patterns of composite membranes before and after H2 permeation testing at (a) 400 °C and (b) 500 °C.
See this image and copyright information in PMC

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