Quantitative electron tomography is proposed to characterize porous materials at a nanoscale. To achieve reliable three-dimensional (3D) quantitative information, the influence of missing wedge artifacts and segmentation methods is investigated. We are presenting the "Discrete Algebraic Reconstruction Algorithm" as the most adequate tomography method to measure porosity at the nanoscale. It provides accurate 3D quantitative information, regardless the presence of a missing wedge. As an example, we applied our approach to nanovoids in La2Zr2O7 thin films.

Nanodomains formed by microphase separation in thin films of the diblock copolymers poly(styrene-b-2-vinylpyridine) (PS-b-P2VP) and poly(styrene-b-ethyleneoxide) (PS-b-PEO) were imaged by means of infrared scattering-type near-field microscopy. When probing at 3.39 mum (2950 cm(-1)), contrast is obtained due to spectral differences between the C--H stretching vibrational resonances of the respective polymer constituents. An all-optical spatial resolution better than 10 nm was achieved, which corresponds to a sensitivity of just several thousand C--H groups facilitated by the local-field enhancement at the sharp metallic probe tips. The results demonstrate that infrared spectroscopy with access to intramolecular dimensions is within reach.

An adequate buffer layer architecture is of great importance for YBa2Cu3O7−δ (YBCO)-coated conductor fabrication. We present a transmission electron microscopy (TEM) analysis of La2Zr2O7 (LZO) buffer layers on biaxially textured Ni–5 at.%W substrates for YBCO-coated conductors prepared by chemical solution deposition (CSD). The LZO thin films were heat-treated at 900 and 1050 °C respectively. Electron diffraction patterns, and bright and dark-field images were used to determine the microstructure, texture and the nanoporosity of the films. By x-ray diffraction the films were found to be [100] oriented and strongly biaxially textured. Although x-ray diffraction suggests an epitaxial growth of LZO on Ni it was shown by TEM that this was not the case. The grain size of the films is between 100 and 300 nm and therefore much smaller than the Ni grain size of 40 µm. Appropriate acquisition conditions for scanning electron microscopy (SEM) and TEM imaging are given to identify the nanogranularity of the films. For the film annealed at 1050 °C high-resolution SEM images clearly show a polycrystalline LZO microstructure and the grain size can readily be determined. Electron diffraction rings are more pronounced than for the film annealed at 900 °C, indicating a higher level of polycrystallinity in the film. SEM images of the film annealed at 900 °C yield no evidence of a polycrystalline microstructure; only single misoriented LZO grains separated by 500 nm are observed. Nanovoids 10–40 nm in size were found in the LZO buffer layers with a high density. The voids had approximately cuboid shape, indicating an anisotropy of the surface energy in LZO. The surface planes of the voids were identified as {111} lattice planes. Despite the nanoporosity, which is a typical feature of CSD-grown buffer layers, the LZO buffer layers act as efficient Ni diffusion barriers. Energy dispersive x-ray microanalysis (EDX) in the transmission electron microscope yielded the composition of the films. In the LZO films no Ni-rich secondary phases were detected and significant C contamination occurred during spectrum acquisition.

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Lanthanum-cerium oxide (LCO) films were deposited on Ni-5%W substrates by chemical solution deposition (CSD) from water-based precursors. LCO films containing different ratios of lanthanum and cerium ions (from CeO 2 to La 2 Ce 2 O 7 ) were prepared. The composition of the layers was optimized towards the formation of LCO buffer layers, lattice-matched with the superconducting YBa 2 Cu 3 O y layer, useful for the development of coated conductors. Single, crack-free LCO layers with a thickness of up to 140 nm could be obtained in a single deposition step. The crystallinity and microstructure of these lattice-matched LCO layers were studied by X-ray diffraction techniques, RHEED and SEM. We find that only layers with thickness below 100 nm show a crystalline top surface although both thick and thin layers show good biaxial texture in XRD. On the most promising layers, AFM and (S)TEM were performed to further evaluate their morphology. The overall surface roughness varies between 3.9 and 7.5 nm, while the layers appear much more dense than the frequently used La 2 Zr 2 O 7 (LZO) systems, showing much smaller nanovoids (1-2 nm) than the latter system. Their effective buffer layer action was studied using XPS. The thin LCO layers supported the growth of superconducting YBCO deposited using PLD methods.