2025 Volume 66 Issue 4 Pages 419-425
In this study, we explored a method for preparing evaluation samples for hydrogen analysis, aiming to advance hydrogen analysis technology in metallic materials. Titanium-titanium hydride sintered specimens with varying hydrogen concentrations were prepared via spark plasma sintering (SPS) using titanium powder and titanium hydride powder, and the hydrogen concentration and distribution in the sintered specimens were evaluated. The obtained results are summarized below. SPS proved to be an effective technique for producing dense sintered compacts in a short time, allowing for easy control of the hydrogen concentration. Furthermore, most hydrogen existed as titanium hydride in the titanium-titanium hydride sintered compact, and high densification with a relative density of 98% or higher was confirmed. In addition, the hydrogen distribution in the upper, inner, and lower parts of the sample was measured using glow discharge optical emission spectrometry (GD-OES). The relative standard deviation of the hydrogen emission intensity in the titanium-titanium hydride sintered body was less than 5%, indicating that the hydrogen was uniformly distributed throughout the sintered body. These results suggest that titanium-titanium hydride sintered by SPS is useful as an evaluation sample for hydrogen analysis and is expected to be particularly effective for hydrogen analysis in GD-OES.
