469 research outputs found

    Refining structures against reflection rank: an alternative metric for electron crystallography.

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    A new metric is proposed to improve the fidelity of structures refined against precession electron diffraction data. The inherent dynamical nature of electron diffraction ensures that direct refinement of recorded intensities against structure-factor amplitudes can be prone to systematic errors. Here it is shown that the relative intensity of precessed reflections, their rank, can be used as an alternative metric for refinement. Experimental data from erbium pyrogermanate show that applying precession reduces the dynamical transfer of intensity between reflections and hence stabilizes their rank, enabling accurate and reliable structural refinements. This approach is then applied successfully to an unknown structure of an oxygen-deficient bismuth manganite resulting in a refined structural model that is similar to a calcium analogue.The authors thank the EPSRC for financial support through grant number HO1771

    Scanning precession electron tomography for three-dimensional nanoscale orientation imaging and crystallographic analysis.

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    Three-dimensional (3D) reconstructions from electron tomography provide important morphological, compositional, optical and electro-magnetic information across a wide range of materials and devices. Precession electron diffraction, in combination with scanning transmission electron microscopy, can be used to elucidate the local orientation of crystalline materials. Here we show, using the example of a Ni-base superalloy, that combining these techniques and extending them to three dimensions, to produce scanning precession electron tomography, enables the 3D orientation of nanoscale sub-volumes to be determined and provides a one-to-one correspondence between 3D real space and 3D reciprocal space for almost any polycrystalline or multi-phase material.A.S.E. and P.A.M acknowledge financial support from the European Research Council under the European Union's Seventh Framework Programme (FP7/2007-2013)/ERC grant agreement 291522-3DIMAGE, the Seventh Framework Programme of the European Commission: ESTEEM2, contract number 312483, EPSRC grant number EP/H017712/1 and the Royal Society. R.K. acknowledges financial support from Rolls-Royce, EPSRC and the BMWi under EP/H022309/1, EP/H500375/1 and grant number 20T0813. We are grateful to Professor Edgar Rauch for valuable discussion on the use of the Astar system, to Dr Cathie Rae and Dr Mark Hardy of Rolls-Royce for supply of the superalloy samples and valuable discussion about their microstructure, Dr Zineb Saghi for help with the tomographic reconstructions and Dr Francisco de la Peña for help with the NMF decompositions.This is the final version. It was first published by NPG at http://www.nature.com/ncomms/2015/150601/ncomms8267/full/ncomms8267.html

    Denoising time-resolved microscopy image sequences with singular value thresholding.

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    Time-resolved imaging in microscopy is important for the direct observation of a range of dynamic processes in both the physical and life sciences. However, the image sequences are often corrupted by noise, either as a result of high frame rates or a need to limit the radiation dose received by the sample. Here we exploit both spatial and temporal correlations using low-rank matrix recovery methods to denoise microscopy image sequences. We also make use of an unbiased risk estimator to address the issue of how much thresholding to apply in a robust and automated manner. The performance of the technique is demonstrated using simulated image sequences, as well as experimental scanning transmission electron microscopy data, where surface adatom motion and nanoparticle structural dynamics are recovered at rates of up to 32 frames per second.Junior Research Fellowship from Clare CollegeThis is the final version of the article. It first appeared from Elsevier via http://dx.doi.org/10.1016/j.ultramic.2016.05.00

    Very weak electron-phonon coupling and strong strain coupling in manganites

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    The coupling of the manganite stripe phase to the lattice and to strain has been investigated via transmission electron microscopy studies of polycrystalline and thin film manganites. In polycrystalline \PCMOfiftwo a lockin to q/a=0.5q/a^*=0.5 in a sample with x>0.5x>0.5 has been observed for the first time. Such a lockin has been predicted as a key part of the Landau CDW theory of the stripe phase. Thus it is possible to constrain the size of the electron-phonon coupling in the CDW Landau theory to between 0.04% and 0.05% of the electron-electron coupling term. In the thin film samples, films of the same thickness grown on two different substrates exhibited different wavevectors. The different strains present in the films on the two substrates can be related to the wavevector observed via Landau theory. It is demonstrated that the the elastic term which favours an incommensurate modulation has a similar size to the coupling between the strain and the wavevector, meaning that the coupling of strain to the superlattice is unexpectedly strong.Comment: 6 pages, 7 figure

    Electron tomography provides a direct link between the Payne effect and the inter-particle spacing of rubber composites.

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    Rubber-filler composites are a key component in the manufacture of tyres. The filler provides mechanical reinforcement and additional wear resistance to the rubber, but it in turn introduces non-linear mechanical behaviour to the material which most likely arises from interactions between the filler particles, mediated by the rubber matrix. While various studies have been made on the bulk mechanical properties and of the filler network structure (both imaging and by simulations), there presently does not exist any work directly linking filler particle spacing and mechanical properties. Here we show that using STEM tomography, aided by a machine learning image analysis procedure, to measure silica particle spacings provides a direct link between the inter-particle spacing and the reduction in shear modulus as a function of strain (the Payne effect), measured using dynamic mechanical analysis. Simulations of filler network formation using attractive, repulsive and non-interacting potentials were processed using the same method and compared with the experimental data, with the net result being that an attractive inter-particle potential is the most accurate way of modelling styrene-butadiene rubber-silica composite formation.L.S. and P.A.M thank Michelin for funding. The research leading to these results has received funding from the European Research Council under the European Union's Seventh Framework Programme (FP7/2007-2013)/ERC grant agreement 291522-3DIMAGE.This is the final published version. It first appeared at http://www.nature.com/srep/2014/141209/srep07389/full/srep07389.html

    Superhydrophobic supported Ag-NPs@ZnO-nanorods with photoactivity in the visible range

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    In this article we present a new type of 1D nanostructures consisting of supported hollow ZnO nanorods (NRs) decorated with Ag nanoparticles (NPs). The 3D reconstruction by high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM) electron tomography reveals that the Ag NPs are distributed along the hollow interior of the ZnO NRs. Supported and vertically aligned Ag-NPs@ZnO-NRs grow at low temperature (135 °C) by plasma enhanced chemical vapour deposition on heterostructured substrates fabricated by sputtered deposition of silver on flat surfaces of Si wafers, quartz slides or ITO. The growth mechanisms of these structures and their wetting behavior before and after visible light irradiation are critically discussed. The as prepared surfaces are superhydrophobic with water contact angles higher than 150°. These surfaces turn into superhydrophilic with water contact angles lower than 10° after prolonged irradiation under both visible and UV light. The evolution rate of the wetting angle and its dependence on the light characteristics are related to the nanostructure and the presence of silver embedded within the ZnO NRs. ÂEuropean Union NMP3-CT-2006- 032583Ministerio de Ciencia e Innovación MAT2010-21228, MAT2010-18447, CSD2008-00023Junta de Andalucía P09-TEP-5283, CTS-518

    Competition for the in vitro binding of radioiodinated human follicle-stimulating hormone in reptilian, avian, and mammalian gonads by nonmammalian gonadotropins

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    Radioiodinated human FSH (125I-hFSH) was used to study the specificity of the gonadotropin binding sites of various reptilian, avian, and mammalian gonadal tissues by examining competitive interactions with several nonmammalian gonadotropins. All preparations of nonmammalian gonadotropins showed some activity in these radioligand assays, but wide variations in activities were evident depending on the source of the tissue and source of the hormone. Several cases of marked species specificity in binding were apparent: Nonmammalian hormones were relatively inactive with porcine granulosa cells; frog and snake hormones were relatively inactive in turtle tissues; and frog hormones were essentially inactive in avian tissues. FSH-LH specificity of binding determined with hormones of nonmammalian origin differed significantly from that previously described with the aid of mammalian gonadotropins. In particular, when tested with some tissues, three preparations of LH, from the turkey, sea turtle, and frog, were in some cases more active in competing for 125I-hFSH binding than preparations of FSH from the same species; this activity could not be readily accounted for by FSH contamination. These comparative data demonstrate the existence of considerable overlap in the binding characteristics of some species of FSH and LH; the observed differences probably reflect evolutionary changes in both gonadotropin binding sites and in the structure of the gonadotropins.Peer Reviewedhttp://deepblue.lib.umich.edu/bitstream/2027.42/21644/1/0000028.pd
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