Chemists of all fields currently publish about 50 000 crystal structures per year, the vast majority of which are X‐ray structures. We determined two molecular structures by employing electron rather than X‐ray diffraction. For this purpose, an EIGER hybrid pixel detector was fitted to a transmission electron microscope, yielding an electron diffractometer. The structure of a new methylene blue derivative was determined at 0.9 Å resolution from a crystal smaller than 1×2 μm 2 . Several thousand active pharmaceutical ingredients (APIs) are only available as submicrocrystalline powders. To illustrate the potential of electron crystallography for the pharmaceutical industry, we also determined the structure of an API from its pill. We demonstrate that electron crystallography complements X‐ray crystallography and is the technique of choice for all unsolved cases in which submicrometer‐sized crystals were the limiting factor.
Single crystals of Mg 1-x Al x B 2 have been grown at a pressure of 30 kbar using the cubic anvil technique. Precipitation free crystals with x < 0.1 were obtained as a result of optimization of already developed MgB 2 crystal growth procedure. Systematic decrease of the c-axis lattice constant with increasing Al content, when the a-axis lattice constant is practically unchanged, was observed. Variation of the critical temperature on Al content in Mg 1-x Al x B 2 crystals was found to be slightly different than that one observed for polycrystalline samples since, even a very small substitution of 1-2% of Al leads to the decrease of T c by about 2-3 K. X-ray and high resolution transmission electron microscopy investigations indicate on the appearance of second precipitation phase in the crystals with x > 0.1. This is in a form of non-superconducting MgAlB 4 domains in the structure of superconducting Mg 1-x Al x B 2 matrix. Resistivity and magnetic investigations show the slight increase of the upper critical field, H c2 , for H//c for the samples with small x, significant reduction of the H c2 anisotropy at lower temperatures, and decrease of the residual resistance ratio value for Al substituted samples as compared to those of unsubstituted crystals. Superconducting gaps variation as a function of Al content, investigated with point contact spectroscopy for the series of the crystals with T c in the range from 20 to 37 K, does not indicate on the merging of the gaps with decreasing T c down to 20 K. It may be related to an appearance of the precipitation phase in the Mg 1-x Al x B 2 structure. 74.70.Ad, 74.62.Dh, 81.10.-h, 74.25.Ha
Abstract:Highly active and durable oxygen reduction catalysts are needed to reduce the costs and enhance the service life of polymer electrolyte fuel cells (PEFCs). This can be accomplished by alloying Pt with a transition metal (e.g. Ni) and by eliminating the corrodible, carbon based catalyst support -however, materials combining both approaches have seldom been implemented in PEFC cathodes. In this work, an unsupported Pt-Ni alloy nanochain ensemble (aerogel) demonstrates high current PEFC performance commensurate with that of a carbon supported benchmark (Pt/C) following optimization of the aerogel's catalyst layer (CL) structure. The latter is accomplished using a soluble filler to shift the CL's pore size distribution towards larger pores which improves reactant and product transport. Chiefly, the optimized PEFC aerogel cathodes display ≈ 2.5-fold larger surface-specific ORR activity than Pt/C and maintain 90% of the initial activity after an accelerated stress test (vs. 40% for Pt/C). Unsupported Pt-Ni Aerogels with Enhanced High Current Performance and Durability in Fuel Cell CathodesSebastian Henning [a] , Hiroshi Ishikawa [b] , Laura Kühn [c] , Juan Herranz [a] *, Elisabeth Müller [d] , Alexander Eychmüller [c] and Thomas J. Schmidt [a,e] Abstract: Highly active and durable oxygen reduction catalysts are needed to reduce the costs and enhance the service life of polymer
Highly active and durable oxygen reduction catalysts are needed to reduce the costs and enhance the service life of polymer electrolyte fuel cells (PEFCs). This can be accomplished by alloying Pt with a transition metal (for example Ni) and by eliminating the corrodible, carbon-based catalyst support. However, materials combining both approaches have seldom been implemented in PEFC cathodes. In this work, an unsupported Pt-Ni alloy nanochain ensemble (aerogel) demonstrates high current PEFC performance commensurate with that of a carbon-supported benchmark (Pt/C) following optimization of the aerogel's catalyst layer (CL) structure. The latter is accomplished using a soluble filler to shift the CL's pore size distribution towards larger pores which improves reactant and product transport. Chiefly, the optimized PEFC aerogel cathodes display a circa 2.5-fold larger surface-specific ORR activity than Pt/C and maintain 90 % of the initial activity after an accelerated stress test (vs. 40 % for Pt/C).
An innovative strategy in dislocation analysis, based on comparison between continuous and tessellated film, demonstrates that vertical dislocations, extending straight up to the surface, easily dominate in thick Ge layers on Si(001) substrates. The complete elimination of dislocations is achieved by growing self-aligned and self-limited Ge microcrystals with fully faceted growth fronts, as demonstrated by AFM extensive etch-pit counts.
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