On the robustness of the Kelvin probe based potentiometric hydrogen electrode method and its application in characterizing effective hydrogen activity in metal: 5 wt. % Ni cold-rolled ferritic steel as an example

Quantitative detection of hydrogen in metal is important in providing a better basis for fundamental investigations of hydrogen embrittlement and hydrogen-related corrosion phenomena. Thermal desorption spectroscopy (TDS) has long been used in characterizing different hydrogen traps inside materials. However, in TDS measurements, the diffusible hydrogen (hydrogen at interstitial sites and weakly bound hydrogen) is usually not detected. The Davanathan-Starchurski permeation technique can cover this shortage. However, for such experiments, the stability of the palladium at the exit side, i.e. in aqueous solution under high potential polarization is an important issue. Alternatively, a Kelvin probe-based (KP-based) potentiometric method developed a few years ago has shown to allow quantitative determination of hydrogen in metal. This method is based on measuring the hydrogen electrode potential on the Pd-coated surface. The aim of this work is to check the reliability of this method and to demonstrate its potential applications in determining the hydrogen amount distributed in both shallow and deep traps in steel. The results reveal that different crystallographic orientation, grain shapes and grain sizes of the deposited palladium film (in the range of variation in this work) do not cause relevant effects on the KP-based hydrogen detection. It is shown in this work that the time lag and permeation rate derived from the permeation curves obtained by this method show a very good reliability and the calculated hydrogen amount shows a good agreement with TDS results. 5 wt.% Ni ferritic steel is used as a model material in this work.