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Register a new userInvestigating Degradation Modes in Zn-AgO Aqueous Batteries with $textit{In-Situ}$ X-ray Micro Computed Tomography
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To meet growing energy demands, degradation mechanisms of energy storage devices must be better understood. As a non-destructive tool, X-ray Computed Tomography (CT) has been increasingly used by the battery community to perform $textit{in-situ}$ experiments that can investigate dynamic phenomena. However, few have used X-ray CT to study representative battery systems over long cycle lifetimes (>100 cycles). Here, we report the $textit{in-situ}$ CT study of Zn-Ag batteries and demonstrate the effects of current collector parasitic gassing over long-term storage and cycling. We design performance representative $textit{in-situ}$ CT cells that can achieve >250 cycles at a high areal capacity of $mathrm{12.5;mAh/cm^2}$. Combined with electrochemical experiments, the effects of current collector parasitic gassing are revealed with micro-scale CT (MicroCT). The volume expansion and evolution of ZnO and Zn depletion is quantified with cycling and elevated temperature testing. The experimental insights are then utilized to develop larger form-factor $mathrm{4;cm^2}$ cells with electrochemically compatible current collectors. With this, we demonstrate over 325 cycles at a high capacity of $mathrm{12.5;mAh/cm^2}$ for a $mathrm{4;cm^2}$ form-factor. This work demonstrates that $textit{in-situ}$ X-ray CT used in long cycle-lifetime studies can be applied to examine a multitude of other battery chemistries to improve their performances.
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X-ray Computed Tomography (X-ray CT) is a well-known non-destructive imaging technique where contrast originates from the materials absorption coefficients. Novel battery characterization studies on increasingly challenging samples have been enabled by the rapid development of both synchrotron and laboratory-scale imaging systems as well as innovative analysis techniques. Furthermore, the recent development of laboratory nano-scale CT (NanoCT) systems has pushed the limits of battery material imaging towards voxel sizes previously achievable only using synchrotron facilities. Such systems are now able to reach spatial resolutions down to 50 nm. Given the non-destructive nature of CT, in-situ and operando studies have emerged as powerful methods to quantify morphological parameters, such as tortuosity factor, porosity, surface area, and volume expansion during battery operation or cycling. Combined with powerful Artificial Intelligence (AI)/Machine Learning (ML) analysis techniques, extracted 3D tomograms and battery-specific morphological parameters enable the development of predictive physics-based models that can provide valuable insights for battery engineering. These models can predict the impact of the electrode microstructure on cell performances or analyze the influence of material heterogeneities on electrochemical responses. In this work, we review the increasing role of X-ray CT experimentation in the battery field, discuss the incorporation of AI/ML in analysis, and provide a perspective on how the combination of multi-scale CT imaging techniques can expand the development of predictive multiscale battery behavioral models.
Kinetics parameters for three anion exchange reactions - Zn-LDH-NO3 - Zn-LDH-Cl, Zn-LDH-NO3 - Zn-LDH-SO4 and Zn-LDH-NO3 - Zn-LDH-VOx - were obtained by in situ synchrotron study. The first and the second ones are two-stage reactions; the first stage is characterized by the two-dimensional diffusion-controlled reaction following deceleratory nucleation and the second stage is a one-dimensional diffusion-controlled reaction also with a decelerator nucleation effect. In the case of exchange NO3 - Cl host anions are completely released, while in the case of NO3 - SO42 the reaction ends without complete release of nitrate anions. The exchange of Zn-LDH-NO3 - Zn-LDH-VOx is one-stage reaction and goes much slower than the previous two cases. It is characterized by a one stage two-dimensional reaction and nucleation considered to be instantaneous in this case. As a result, at the end of this process there are two crystalline phases with different polyvanadate species, presumably V4O124 and V2O74, nitrate anions were not completely released. The rate of replacing NO3 anions by guest ones can be represented as Cl > SO42 > VOxy.
Conjugated polymer-based organic electrochemical transistors (OECTs) are being studied for applications ranging from biochemical sensing to neural interfaces. While new conjugated polymers are being developed that can interface digital electronics with the aqueous chemistry of life, the vast majority of high-performance, high-mobility organic transistor materials developed over the past decades are extremely poor at taking up biologically-relevant ions. Here we incorporate an ion exchange gel into an OECT, demonstrating that this structure is capable of taking up biologically-relevant ions from solution and injecting larger, more hydrophobic ions into the underlying polymer semiconductor active layer in multiple hydrophobic conjugated polymers. Using poly[2,5-bis(3-tetradecylthiophen-2-yl) thieno[3,2-b]thiophene] (PBTTT) as a model semiconductor active layer and a blend of the ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (BMIM TFSI) and poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) as the ion exchange gel, we demonstrate more than a four order of magnitude improvement in OECT device transconductance and a one hundred-fold increase in ion injection kinetics. We demonstrate the ability of the ion exchange gel OECT to record biological signals by measuring the action potentials of a Venus flytrap plant. These results show the possibility of using interface engineering to open up a wider palette of organic semiconductor materials as OECTs that can be gated by aqueous solutions.
Amorphous solids, which show characteristic differences from crystals, are common in daily usage. Glasses, gels, and polymers are familiar examples, and polymers are particularly important in terms of their role in construction and crafting. Previous studies have mainly focused on the bulk properties of polymeric products, and the local properties are less discussed. Here, we designed a distinctive protocol using the negatively charged nitrogen vacancy center in nanodiamond to study properties inside polymeric products in situ. Choosing the curing of poly dimethylsiloxane and the polymerization of cyanoacrylate as subjects of investigation, we measured the time dependence of local pressure and strain in the materials during the chemical processes. From the measurements, we were able to probe the local shear stress inside the two polymeric substances in situ. By regarding the surprisingly large shear stress as the internal tension, we attempted to provide a microscopic explanation for the ultimate tensile strength of a bulk solid. Our current methodology is applicable to any kind of transparent amorphous solids with the stress in the order of MPa and to the study of in situ properties in nanoscale. With better apparatus, we expect the limit can be pushed to sub-MPa scale.
Soft X-ray magnetic vector tomography has been used to visualize with unprecedented detail and solely from experimental data the 3D magnetic configuration of a ferrimagnetic Gd12Co88/Nd17Co83/Gd24Co76 multilayer with competing anisotropy, exchange and magnetostatic interactions at different depths. The trilayer displays magnetic stripe domains, arranged in a chevron pattern, which are imprinted from the central Nd17Co83 into the bottom Gd12Co88 layer with a distorted closure domain structure across the thickness. Near the top Gd24Co76 layer, local exchange springs with out-of-plane magnetization reversal, modulated ripple patterns and magnetic vortices and antivortices across the thickness are observed. The detailed analysis of the magnetic tomogram shows that the effective strength of the exchange spring at the NdCo/GdCo interface can be finely tuned by GdxCo1-x composition and anisotropy (determined by sample fabrication) and in-plane stripe orientation (adjustable), demonstrating the capability of 3D magnetic visualization techniques in magnetic engineering research.
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