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J. Phys. Energy 3 (2021) 031503 N Tapia-Ruiz et al Figure 34. Key dissolution reactions occurring on sodium-ion anodes: attack from reactive species in solution, anodic dissolution, and crack formation caused by structural strain. Heteroatom doping and surface coatings may have a stabilising effect. Figure 35. V-shaped flow cell direct-injection online ICP analysis design for fast-throughput dissolution analysis. The electrolyte flows past an online counter electrode (CE), passes over the working electrode (WE) surface controlled by a potentiostat and the reference electrode (RE). Any dissolution products are efficiently transported to an ICP-type instrument for nebulisation and ionised by the plasma torch. The red-framed insert is a magnified view of the contact between the flow cell and the working electrode. concentrations of dissolved iron from sodium iron hexacyanoferrate electrodes as a function of the surface coating strategy [259]. Energy-dispersive x-ray spectroscopy (EDS) is also commonly used, for example, to analyse the separator in order to identify trapped ions, or to analyse the negative electrode to identify DMD products from Na0.67MnO2 electrodes [260]. The preparation and ex situ handling of such samples increases experimental error and may compromise the reliability of the conclusions. Furthermore, full and half cells prepared in CR2032 coin cells do not isolate a single cause of dissolution, as the effects of electrode arrangement, cell pressure, the counter-electrode material and current collectors must also be considered. Open questions are whether electrode dissolution is electrochemically or chemically induced, i.e., which are the most significant dissolution pathways, and their accurate quantification. Methods of detection must be highly sensitive, as dissolution only affects a small part of the overall electrode mass, and setups must rigorously exclude agents known to accelerate dissolution, such as water, as otherwise, artefacts will arise. An adequate dissolution monitoring system must therefore be carefully designed. Advances in science and technology to meet challenges ICP-based instruments are routinely available, and allow highly sensitive elemental analysis, with detection limits of sub-ppb using optical emission spectroscopy (ICP-OES) or even sub-ppt using mass spectrometry (ICP-MS). Primarily used for aqueous samples, these are, to a certain degree, forgiving towards non-aqueous battery solvents and electrolyte salts (up to 0.1 M (ICP-MS) or 1 M (ICP-OES) without dilution). The observation of dissolution in non-aqueous electrolytes is challenging, due to the need for oxygen and water to be excluded from the electrolyte. Prohibitive factors include instrument corrosion from highly reactive electrolytes and the high cost of many high-quality non-aqueous electrolyte solutions. Recent advances in electrochemical flow cell design have enabled direct observations of the dissolution of candidate electrode surfaces in non-aqueous environments under potential or galvanostatic control. Typically, the electrochemical flow cell outlet is directly connected to the ICP nebuliser by tubing, in the so-called direct-injection analysis. Successful examples include the flow-through scanning flow cell (FT-SFC) introduced by Mayrhofer et al [261], which incorporates a V-shaped channel design for efficient transport of dissolution products, figure 35. This type of cell has also been manufactured by 3D printing and successfully 66PDF Image | 2021 roadmap for sodium-ion batteries
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