Examination of the reliability of X-ray techniques for determining hydrogen-induced volume changes

The Bragg peaks in x-ray diffraction experiments are generally taken to be a reliable measure of the average lattice distance in crystals. We show that this assumption can be misleading when determining hydrogen-induced volume changes. Experiments based on simultaneous determination of the position of the Bragg peak and the sample volume of an Fe/V(001) superlattice while expanding the lattice by in situ hydrogen loading serve as an illustration of this counter-intuitive effect.