Fundamental studies concerning the growth, structural characterization and hydrogen uptake of single-crystal (00 l )-oriented Mo/V superlattices have been performed. The superlattices were grown by dual-target magnetron sputtering in pure Ar-atmosphere < 6·10^-3 Torr on (001)-oriented MgO substrates. X-ray diffraction (XRD), X-ray and neutron reflectivity, high resolution (HR) as well as ordinary crosssectional transmission electron microscopy (XTEM) and selected area electron diffraction (SAED) were used for the structural characterization. Hydrogen depth-profiling was performed by the ¹⁵N method.

For growth of periodic Mo/V superlattices, it is shown that substrate temperatures in the range of 600-700 °C is feasible for epitaxy. At higher growth temperatures substantial interdiffusion occurred. Furthermore, simulations of XRDpatterns gave the width of the interfaces to be ±1 monolayer (±0,154 nm) which was confirmed by XRD and HRXTEM analyses of a superlattice grown with layer thicknesses D_Mo=D_v=0,31 nm (2 monolayers). A transition from smooth to wavy V-layers was found to occur at a critical V-layer thickness D_c. In superlattices where the relative amount of V is large, De is large and vice versa for superlattices containing thin V-layers. In superlattices with equally thick Mo- and V-layers D_c was found to be ~2,5 nm. Mo was found to grow with a uniform thickness following the surface of the V-layers. The layer thickness fluctuations are non-accumulative and disappear if the periodicity of a growing Mo/V superlattice is changed so that Dv becomes smaller than D_c. The origin of the 3D evolution is explained in terms of surface strain and the roughening transition. The interfaces of Mo/V superlattices grown under the influence of energetic ion bombardment ranging from about 15 eV to 250 eV was studied by HRXTEM and XRD. Both techniques indicated a continous deterioration of the interface quality and an increasing amount of defects with increasing ion energy.

The diffraction peaks from a clas of quasi-periodic superlattices which can be generated by the inflation rules A→A^mB, B→A (m = positive integer) was analytically, experimentally and numerically found to be located at the wavevectors q = 2πɅ^-1rγ(m)^k where r and k are integers and A is an average superlattice period. The ratios, γ(m), between the thicknesses of the two superlattice building blocks, A and B, must be chosen such that γ(m) = (m + (m² + 4) ^1/2 )/2.

The uptake of hydrogen in the superlattices is found to decrease with decreasing A and for ≤5,5 nm the transition between α-VH_x and β-VH_x is not observed. A model is proposed which explains the A-dependent behaviour of the hydrogen uptake by a transfer of interstitial electrons from Mo to V, creating a 0,49 nm wide H-free interface layer. The existence of this layer is shown both by the 15_N method performed on samples containing several A:s and by combining simulations of X-ray and neutron reflectivities with measurements on superlattices loaded with either hydrogen or deuterium. The structural change of Mo/V(OOl) superlattices upon H-loading was measured by a method derived in this work which utilises a combination of X-ray reflectivity and reciprocal space mapping by XRD. The lattice parameters in the layers are measured in the growth direction as well a in the plane of the sample. It is found that the V lattice expands in the growth direction and that the hydrogenation process is associated with relaxation of coherency strain.