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1.
Ultramicroscopy ; 236: 113475, 2022 06.
Artigo em Inglês | MEDLINE | ID: mdl-35255271

RESUMO

The sensitive coherent interference of electron waves arising from a specimen is useful for revealing subtle structural information in electron micrographs, which can be important for minimising dose and for rapid imaging. In general, dynamical diffraction is expected due to the useful strong interactions of electrons with matter, which can create phase contrast that violates the requisite Radon projection assumption for tomography. It is for these reasons that incoherent imaging modalities such as high angle annular dark field have been favoured to date in electron tomography of crystalline specimens, to access a monotonic relationship between specimen thickness and micrograph intensity. Here we use a geometric approach to track topological features that are robust to perturbation of the imaging conditions, to enable 3D reconstructions from electron microscope tilt series under imaging conditions that violate the Radon projection assumption, with an emphasis on phase contrast. Invoking a sparsity assumption, we demonstrate that topological features can be reliably tracked in 3D using a differential geometric form of stereoscopy, to circumvent departures from the projection approximation and reduce noise by effecting segmentation of interest points from the outset. We demonstrate this approach on a variety of different specimen and data types, from polyhedral nanoparticles, to steel dislocation networks, cryo-EM cellular structures and 3D diffuse diffraction of a relaxor ferroelectric.


Assuntos
Tomografia com Microscopia Eletrônica , Elétrons , Microscopia Crioeletrônica/métodos , Tomografia com Microscopia Eletrônica/métodos
2.
Dalton Trans ; 47(27): 9136-9142, 2018 Jul 10.
Artigo em Inglês | MEDLINE | ID: mdl-29946581

RESUMO

Synthesis of phase pure hopeite pigment through a solvothermal flow method is reported here for the first time. The products show two-step dehydration behaviour from thermogravimetric analysis (TGA), and a higher degree of purity and homogeniety than commercial zinc phosphate pigment. By increasing the reaction temperature stepwise from room temperature to 350 °C it was possible to decrease the size of the individual crystallite sheets and to tune their packing into larger assemblies. The conversion of reactants to product proved to be significantly higher at increased temperature with a measured yield of 98.7% at 250 °C versus 85.4% at room temperature. The synthesis route demonstrated here is environmentally sustainable, increases cost-efficiency through minimization of waste, and is compatible with a scale-up strategy.

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