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Abstract: The addition of nano-fillers has been widely proposed as a method to enhance the dielectric properties of high voltage polymeric insulation, though there are mixed reports in the literature. Here the potential of silica nano-particles to extend the time to failure specifically through resistance to electrical tree growth in epoxy resin is determined. The benefit of silane treating the nano-particles before compounding is clearly established with regard to slowing tree growth and subsequent time to failure. The growth of trees in needle-plane samples is measured in the laboratory with loadings of 1, 3 and 5 wt% nano-filler. In all cases the average times to failure are extended, but silane treatment of the nano-particles prior to compounding yields much superior results. The emergence of a pronounced inception time before tree growth is also noted for the higher-filled, silane-treated cases. The average time to failure of silane-treated 5 wt% filled material was 28 times that of the unfilled resin. The improvement in performance between the nanocomposites with untreated and treated fillers is attributed to fewer agglomerations and improved dispersion of the filler in the treated cases. Measurements of Partial Discharge (PD) indicated significant differences in PD patterns during the growth of trees in the treated and untreated cases. This distinction may provide a quality control method for monitoring materials. In particular, long periods in which PDs were not measured were observed in the silane-treated cases. Visual imaging of tree growth in the unfilled material allowed the changing nature of the tree from fine to tree to dark tree to be observed as it grew. Corresponding PD measurements suggest the dark tree is gradually becoming conductive, and that growth of maximum PD measured is dependent on the relative rates of the growth of the tree and its carbonization. X-ray computer tomography identified significant differences in average tree channel diameters (a reduction from 2.8 µm to 2.0 µm for 1 wt% and 3 wt% cases). This implies that in addition to tree length changes, evaporated tree volumes also change and may explain the change in partial discharge characteristics observed.

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Abstract: Magnesium potassium phosphate cements (MKPC) were investigated to determine their efficacy towards retardation of reactive uranium metal corrosion. Optimised low-water content, fly ash (FA) and blast furnace slag (BFS) blended MKPC formulations were developed and their fluidity, hydration behaviour, strength and phase assemblage investigated. In-situ time resolved synchrotron powder X-ray diffraction was used to detail the early age (~60 h) phase assemblage development and hydration kinetics, where the inclusion of BFS was observed to delay the formation of struvite-K by ~14 h compared to FA addition (~2 h). All samples set within this period, suggesting the possible formation of a poorly crystalline binding phase prior to struvite-K crystallisation. Long-term corrosion trials using metallic uranium indicated that MKPC systems are capable of limiting uranium corrosion rates (reduced by half), when compared to a UK nuclear industry grout, which highlights their potential application radioactive waste immobilisation.

Open Access

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Abstract: The nature and evolution of FeNxCy moieties in Fe/C/N catalysts has been studied by analysing Fe and N environments. TEM and Fe-XAS reveal the presence of FeNx moieties and Fe3C particles in the fresh catalyst. NEXAFS reveals the presence of two groups of (Fe)NxCy ensembles, namely (Fe)Nx-pyridinic and (Fe)Nx-pyrrolic. The architecture of the FeNxCy ensembles and their evolution during the ORR has been analysed by XAS, NEXAFS, and identical locations TEM. NxCy, FeNxCy and Fe3C species are partially removed during the ORR, resulting in the formation of Fe2O3 and Fe3O4 particles with different morphologies. The process is more severe in acid electrolyte than in alkaline one. (Fe)Nx-pyrrolic moieties are the main ones in the fresh catalysts, but (Fe)Nx-pyridinic groups are more stable after the ORR. The correlation between the evolution of the ORR activity and that of the FeNxCy ensembles indicates that FeNx-pyridinic ensembles are responsible for the ORR activity.

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Abstract: Solid state batteries have attracted extensive attention, but the lithium penetration through the solid electrolyte remains a critical barrier to commercialisation and is not yet fully understood. In this study, the 3D morphological evolution of cracks with deposited lithium were tracked as they penetrated through the solid electrolyte during repetitive plating. This is achieved by utilising in-situ synchrotron X-ray computed tomography with high spatial and temporal resolutions. Thin-sheet cracks were observed to penetrate the solid electrolyte without immediate short-circuiting of the cell. Changes in their width and volume were quantified. By calculating the volume of deposited lithium, it was found that the lithium was only partially filled in cracks, and its filling ratio quickly dropped from 94.95% after the 1st plating to ca. 20% after the 4th plating. The filling process was revealed through tracking the line profile of grayscale along cracks. It was found that lithium grew much more slowly than cracks, so that the cracks near the cathode side were largely hollow and the cell could continue to operate. The deposited lithium after short circuit was segmented and its distribution was visualised. DVC analysis was applied to map local high stress and strain, which aggregated along cracks and significantly increased at areas where new cracks formed.

Open Access

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Abstract: The production of diffraction-quality protein crystals is challenging and often requires bespoke, time-consuming and expensive strategies. A system has been developed in which the BCL6 BTB domain acts as a crystallization chaperone and promiscuous assembly block that may form the basis for affinity-capture crystallography. The protein of interest is expressed with a C-terminal tag that interacts with the BTB domain, and co-crystallization leads to its incorporation within a BTB-domain lattice. This strategy was used to solve the structure of the SH3 domain of human nebulin, a structure previously solved by NMR, at 1.56 Å resolution. This approach is simple and effective, requiring only routine protein complexation and crystallization screening, and should be applicable to a range of proteins.