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- Birch, Jens
(författare)
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Single-crystal Mo/V superlattices : growth, structure, and hydrogen uptake
- 1994
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- 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 DMo=Dv=0,31 nm (2 monolayers). A transition from smooth to wavy V-layers was found to occur at a critical V-layer thickness Dc. 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 Dc 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 Dc. 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→AmB, 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-VHx and β-VHx 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 15N 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.
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| 2. |
- Birch, J., et al.
(författare)
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Structural characterization of precious-mean quasiperiodic Mo/V single-crystal superlattices grown by dual-target magnetron sputtering
- 1990
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Ingår i: Physical Review B. - 1098-0121. ; 41:15, s. 10398-10407
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Tidskriftsartikel (refereegranskat)abstract
- A class of quasiperiodic superlattice structures, which can be generated by the concurrent inflation rule A→AmB and B→A (where m=positive integer), has been studied both theoretically and experimentally. Given that the ratios between the thicknesses of the two superlattice building blocks, A and B, are chosen to be γ(m)=[m+(m2+4)1/2]/2 (known as the ‘‘precious means’’), then the x-ray- and electron-diffraction peak positions are analytically found to be located at the wave vectors q=2πΛ−1r[γ(m)]k, where r and k are integers and Λ is an average superlattice wavelength. The analytically obtained results have been compared to experimental results from single-crystalline Mo/V superlattice structures, generated with m=1, 2, and 3. The superlattices were grown by dual-target dc-magnetron sputtering on MgO(001) substrates kept at 700 °C. X-ray diffraction (XRD) and selected-area electron diffraction (SAED) showed that the analytical model mentioned above predicts the peak positions of the experimental XRD and SAED spectra with a very high accuracy. Furthermore, numerical calculations of the diffraction intensities based on a kinematical model of diffraction showed good agreement with the experimental data for all three cases. In addition to a direct verification of the quasiperiodic modulation, both conventional and high-resolution cross-sectional transmission electron microscopy (XTEM) showed that the superlattices are of high crystalline quality with sharp interfaces. Based on lattice resolution images, the width of the interfaces was determined to be less than two (002) lattice-plane spacings (≊0.31 nm).
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