Abstract
Currently, standard samples with high hydrogen concentrations that meet the requirements of hydrogen extraction in an inert atmosphere are not currently available on the market. This article describes the preparation of Ti-H standard samples and the calibration of RHEN602, a hydrogen analyzer, using LECO (LECO, Saint Joseph, MI, USA). Samples of technically pure titanium alloy were chosen as the material for sample production. The creation procedure includes five main steps: sample preparation (polishing to an average roughness of 0.04 μm using sandpaper), annealing, hydrogenation, maintenance in an inert gas atmosphere, and characterization of the samples. The absolute hydrogen concentration in the samples was determined by two methods: volumetric and mass change after the introduction of hydrogen. Furthermore, in-situ X-ray diffraction, temperature programmed desorption (TPD) analysis, and thermogravimetric analysis were used during measurements to investigate the phase transitions in the samples. As a result of this work, a series of calibration samples were prepared in a concentration range up to 4 wt % hydrogen, optimal parameters for measuring high concentrations of hydrogen. The calibration line was obtained and the calibration error was 10%.
Highlights
An important task for the extension of the hydrogen economy is the development of promising hydrogen storage materials [1–6]
The material used for the preparation of samples with known high hydrogen content and tested with the hydrogen analyzer calibration must have a number of properties: High sorption rates under hydrogenation conditions; a stable state of hydrogen without the possibility of desorption under standard temperature and pressure; cost-effectiveness; accessibility; and safety when handling
Stepwise heating was used to analyze the samples with high hydrogen concentration without exceeding the upper threshold of sensitivity of the thermocondimetric cell
Summary
An important task for the extension of the hydrogen economy is the development of promising hydrogen storage materials [1–6]. In order to possess high rates of hydrogen sorption and desorption, advanced hydrogen storage materials should have optimal elemental and phase composition. They should accumulate a large amount of hydrogen and be cyclically stable [7–11]. Metal hydrides have a high bulk density of hydrogen atoms, a wide range of operating pressures and temperatures, catalytic activity, and are the most used materials for hydrogen storage [12–20]. Intermetallic compounds based on hydride-forming metals—such as Zr, Ti, Pd, and V—can accumulate up to four mass % of hydrogen [21–30] and are widely used for hydrogen storage. Measurement of the hydrogen concentration in hydrogen storage materials is an important stage in the development and testing of materials
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