In this work, we demonstrate the power of a simple top-down electrochemical erosion approach to obtain Pt nanoparticle with controlled shapes and sizes (in the range from ∼ 2 to ∼ 10 nm). Carbon supported nanoparticles with narrow size distributions have been synthesized by applying an alternating voltage to macroscopic bulk platinum structures, such as disks or wires. Without using any surfactants, the size and shape of the particles can be changed by adjusting simple parameters such as the applied potential, frequency and electrolyte composition. For instance, application of a sinusoidal AC voltage with lower frequencies results in cubic nanoparticles; whereas higher frequencies lead to predominantly spherical nanoparticles. On the other hand, the amplitude of the sinusoidal signal was found to affect the particle size; the lower the amplitude of the applied AC signal, the smaller the resulting particle size. Pt/C catalysts prepared by this approach showed 0.76 A/mg mass activity towards the oxygen reduction reaction which is ∼ 2 times higher than the state-of-the-art commercial Pt/C catalyst (0.42 A/mg) from Tanaka. In addition to this, we discussed the mechanistic insights about the nanoparticle formation pathways.
The two‐dimensional lithium distribution in the graphite anode was non‐destructively probed by spatially resolved neutron diffraction for a batch consisting of 34 different cylinder‐type (18650) Li‐ion batteries in fully charged state. The uniformity of the lithium distribution was quantified and correlated to the cell specifications/electrochemistry and to intrinsic cell parameters like electrode thickness, position of current collectors, etc. which were obtained by X‐ray micro‐computed tomography. Non‐uniformities in the lithiation state of the anode from a constant plateau have been observed for the majority of the studied cells. Their location corresponds to the positions of current tabs connecting the electrode stripes and areas of incomplete electrode coating at the beginning and the end of the electrode stripes. Four commonly used schemes of current lid connection were identified. Each of them displays its own effect on the uniformity of the lithiation at the anode and, therefore, variation of the intrinsic state‐of‐charge distribution and, most probably, the ageing behavior of the electrodes.
LiNi0.5Mn1.5O4 (LNMO) is a promising cathode in lithium‐ion batteries (LIBs) due to its high operating voltage and open Li+ diffusion framework. However, the instability of the electrode–electrolyte interface and the negative environmental impact of electrode fabrication processes limit its practical application. Therefore, switching electrode processing conditions to aqueous and understanding the accompanying surface structural evolution are imperative. Here, water‐treated, poly(acrylic acid) (PAA)‐treated, and H3PO4‐treated LNMO, labeled as W‐LNMO, A‐LNMO, and H‐LNMO, are studied systematically. W‐LNMO shows a high concentration of Mn3+ induced by Li loss while a conformal PAA layer formed on A‐LNMO reduces this phenomenon. H‐LNMO displays a second MnPO4∙H2O phase. Upon cycling, a fast capacity decay is observed in W‐LNMO while an extra plateau at ≈2.7 V appears in the initial charging, corresponding to a two‐phase transition. A surface reconstruction layer from a spinel to a rock‐salt phase with a reductive Mn2+ segregation is observed in W‐LNMO after 105 cycles. The PAA layer persists on A‐LNMO and alleviates the capacity decay. H‐LNMO delivers a relatively low capacity due to the formation of a MnPO4∙H2O phase. This study provides new insights into manipulating the surface chemistry of LNMO cathodes to enable aqueous, large‐scale processingin LIBs.
Increased formability of aluminium alloys has been demonstrated via cryogenic deformation. In previous studies, the microstructures of samples deformed at low temperatures were analysed after reheating to room temperature (RT) and storage. However, after heating the dislocation structure and density of the deformed material do not reflect the cryogenic situation. In this work, we investigate the evolution of flow stress during recovery in Al-Mg and Al-Mg-Si alloys. We examine the RT recovery behaviour of samples pre-strained at 77 K to different strain levels, and evaluate the structural stability upon subsequent deformation. We also study microstructural evolution via in-situ synchrotron X-ray diffraction, starting from initial conditions at cryogenic temperatures to long-term RT-recovery. Recovery of cryogenically deformed samples at RT results in reduction of the flow stress, in dependence on RT storage. The recovery process can be divided into three distinct sections, each based on a different mechanism characterized by either the arranging or the annihilation of dislocations. Subsequent further straining at room temperature after cryogenic forming also generates plastic instabilities and premature fracture due to unfavourable hardening and recovery assisted softening interplay.
Rare‐earth based luminescent materials are key functional components for the rational design of light‐conversion smart devices. Stable Eu3+‐doped strontium fluoride (SrF2) nanoparticles were prepared at room temperature in ethylene glycol. Their luminescence depends on the Eu content and changes after heat treatment. The crystallinity of heat‐treated material increases in comparison with as‐synthesized samples. Particles were investigated in solution using X‐ray diffraction, small‐angle X‐ray scattering, and X‐ray spectroscopy. After heat treatment, the size of the disordered nanoparticles increases together with a change of their local structure. Interstitial fluoride ions can be localized near Eu3+ ions. Therefore, non‐radiative relaxation from other mechanisms is decreased. Knowledge about the cation distribution is key information for understanding the luminescence properties of any material.
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