The electrode drying process is a crucial step in the manufacturing of lithium-ion batteries and can significantly affect the performance of an electrode once stacked in a cell. High drying rates may induce binder migration, which is largely governed by the temperature. Additionally, elevated drying rates will result in a heterogeneous distribution of the soluble and dispersed binder throughout the electrode, potentially accumulating at the surface. The optimized drying rate during the electrode manufacturing process will promote balanced homogeneous binder distribution throughout the electrode film; however, there is a need to develop more informative in situ metrologies to better understand the dynamics of the drying process. Here, ultrasound acoustic-based techniques were developed as an in situ tool to study the electrode drying process using NMC622-based cathodes and graphite-based anodes. The drying dynamic evolution for cathodes dried at 40 and 60 °C and anodes dried at 60 °C were investigated, with the attenuation of the reflective acoustic signals used to indicate the evolution of the physical properties of the electrode-coating film. The drying-induced acoustic signal shifts were discussed critically and correlated to the reported three-stage drying mechanism, offering a new mode for investigating the dynamic drying process. Ultrasound acoustic-based measurements have been successfully shown to be a novel in situ metrology to acquire dynamic drying profiles of lithium-ion battery electrodes. The findings would potentially fulfil the research gaps between acquiring dynamic data continuously for a drying mechanism study and the existing research metrology, as most of the published drying mechanism research studies are based on simulated drying processes. It shows great potential for further development and understanding of the drying process to achieve a more controllable electrode manufacturing process.
Highlights A CFD model is developed to simulate microwave heating in a millifluidic channel. The effect of process parameters on the temperature profile are investigated. Satisfactory agreement between modelling and experiments is obtained.
A highly-reproducible, high-yield flow synthesis of gold nanoparticles is developed based on synthesis kinetics from a high-pH gold precursor solution.
Over the last decade, acoustic methods, including acoustic emission (AE) and ultrasonic testing (UT), have been increasingly deployed for process diagnostics and health monitoring of electrochemical power devices, including batteries, fuel cells, and water electrolysers. These techniques are non-invasive, highly sensitive, and low-cost, providing a high level of spatial and temporal resolution and practicality. Their application in electrochemical devices is based on identifying changes in acoustic signals emitted from or propagated through materials as a result of physical, structural, and electrochemical changes within the material. These changes in acoustic signals are then correlated to critical processes and the health status of these devices. This review summarises progress in the use of acoustic methods for the process and health monitoring of major electrochemical energy conversion and storage devices. First, the fundamental principles of AE and UT are introduced, and then the application of these acoustic techniques to electrochemical power devices are discussed. Conclusions and perspectives on some of the key challenges and potential commercial and academic applications of the devices are highlighted. It is expected that, with further developments, acoustic techniques will form a key part of the suite of diagnostic techniques routinely used to monitor electrochemical devices across various processes, including fabrication, post-mortem examination and recycle decision support to aid the deployment of these devices in increasingly demanding applications.
The controlled formation of microdroplets through temperature variation is an intriguing concept for binary liquid mixtures with a critical solution temperature. Here, we investigate this phenomenon for a blend of...
Artificial metalloenzymes (ArMs) have high potential in biotechnological applications as they combine the versatility of transition-metal catalysis with the substrate selectivity of enzymes. An ideal host protein should allow high-yield recombinant expression, display thermal and solvent stability to withstand harsh reaction conditions, lack nonspecific metal-binding residues, and contain a suitable cavity to accommodate the artificial metal site. Moreover, to allow its rational functionalization, the host should provide an intrinsic reporter for metal binding and structural changes, which should be readily amendable to high-resolution structural characterization. Herein, we present the design, characterization, and de novo functionalization of a fluorescent ArM scaffold, named mTFP*, that achieves these characteristics. Fluorescence measurements allowed direct assessment of the scaffold’s structural integrity. Protein X-ray structures and transition metal Förster resonance energy transfer (tmFRET) studies validated the engineered metal coordination sites and provided insights into metal binding dynamics at the atomic level. The implemented active metal centers resulted in ArMs with efficient Diels–Alderase and Friedel–Crafts alkylase activities.
The quantitative analysis of nanomaterials synthesis kinetics is valuable both for understanding the synthesis and for development of manufacturing processes, and it usually requires the use of synchrotron-based instrumentation, making it challenging to perform experiments in the large parametric space needed to develop quantitative kinetic models. UV−vis spectroscopy represents a convenient technique to circumvent such difficulties, as it is available in most chemistry laboratories and allows fast data acquisition. This technique can in theory be used for the characterization of plasmonic nanomaterials synthesis kinetics. However, linking UV−vis spectra with characteristic features of the produced nanomaterials, such as size and shape, is a challenging task. This work presents a detailed spectroscopic analysis of gold nanoparticles syntheses via in situ time-resolved UV−vis spectroscopy, with emphasis on the role of gold precursor adsorption on the particle surface during nanoparticle growth. We show that the classic Turkevich synthesis and the growth of preformed gold nanoparticles with two different methods exhibit significant commonalities in the spectra evolution, explained in terms of the interaction between gold precursor species and the nanoparticle surface. Such interaction was accounted for in a model based on the Mie theory, describing the growing nanoparticles as core−shell spheres with an outer shell of few Ångstroms characterized by reduced conductivity and increased electron damping rate. The proposed model led to the determination of the nanoparticle size and concentration evolution throughout the synthesis with good quantitative agreement against literature SAXS data. Furthermore, the core−shell model enabled the reproduction of the progressive blue-shift in the SPR peak position observed during the synthesis. Thus, this work reconciles the "seed-mediated growth" mechanism for the Turkevich synthesis with the temporal evolution of the spectra within the framework of the Mie theory, showing that the distinctive purplegreyish hue observed during the synthesis can be related to the interaction of gold precursor with the growing gold nanoparticles.
BACKGROUNDMicrobioreactors have emerged as a new tool for early bioprocess development. The technology has advanced rapidly in the last decade and obtaining real‐time quantitative data of process variables is nowadays state of the art. In addition, control over process variables has also been achieved. The aim of this study was to build a microbioreactor capable of controlling dissolved oxygen (DO) concentrations and to determine oxygen uptake rate in real time.RESULTSAn oscillating jet driven, membrane‐aerated microbioreactor was developed without comprising any moving parts. Mixing times of ∼7 s, and kLa values of ∼170 h−1 were achieved. DO control was achieved by varying the duty cycle of a solenoid microvalve, which changed the gas mixture in the reactor incubator chamber. The microbioreactor supported Saccharomyces cerevisiae growth over 30 h and cell densities of 6.7 gdcw L−1. Oxygen uptake rates of ∼34 mmol L−1 h−1 were achieved.CONCLUSIONThe results highlight the potential of DO‐controlled microbioreactors to obtain real‐time information on oxygen uptake rate, and by extension on cellular metabolism for a variety of cell types over a broad range of processing conditions. © 2015 The Authors. Journal of Chemical Technology & Biotechnology published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.
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