Magnetic resonance imaging of the rheology of ionic liquid colloidal suspensions

The rheology, and underpinning colloidal interactions, of ionic liquid (IL) dispersions of colloidal silica have been investigated using bulk rheological measurements with magnetic resonance (MR) velocity and relaxation measurements. Two ionic liquids were investigated: tetradecyl(trihexyl)phosphonium bistriflamide ([P6,6,6,14][NTf2]) and 1-butyl-methylimidizolium tetrafluoroborate ([C4mim][BF4]), in the absence and presence of hydrophilic silica nanoparticles (Aerosil 200). Bulk rheology was probed using measurements of shear stress and viscosity as a function of shear rate in a cone-and-plate rheometer. Local rheology was probed using MR velocity imaging of flow in Couette and cone-and-plate cells. Velocity profiles were extracted from the Couette measurements and fitted using a power-law model. Newtonian rheology was observed for both ILs in the absence of dispersed silica. For the dispersion of 15% silica in [C4mim][BF4], bulk rheology and MR velocity imaging measurements showed Newtonian behaviour at low shear rates (10 s−1). For the dispersion of 5% silica in [P6,6,6,14][NTf2], more complex rheology was observed in the flow curve, which was suggestive of shear-banding. This was investigated further using the MR velocity profiles in a Couette cell and velocity images in a cone-and-plate cell, which both showed the coexistence of regions of sheared and unsheared fluid. The sheared fluid was found to be highly shear-thinning and close inspection of the flow profile at the interface between sheared and unsheared fluid suggested that the behaviour was shear-banding rather than shear-localisation. This was further confirmed by the velocity images in the cone-and-plate rheometer, which showed sheared and unsheared fluid in a uniform shear stress environment

Quantitative, InSitu Visualization of Metal-Ion Dissolution and Transport Using ¹H Magnetic Resonance Imaging

Quantitative mapping of metal ions freely diffusing in solution is important across a diverse range of disciplines and is particularly significant for dissolution processes in batteries, metal corrosion, and electroplating/polishing of manufactured components. However, most current techniques are invasive, requiring sample extraction, insertion of an electrode, application of an electric potential or the inclusion of a molecular sensor. Thus, there is a need for techniques to visualize the distribution of metal ions non‐invasively, in situ, quantitatively, in three dimensions (3D) and in real time. Here we have used (1)H magnetic resonance imaging (MRI) to make quantitative 3D maps showing evolution of the distribution of Cu(2+) ions, not directly visible by MRI, during the electrodissolution of copper, with high sensitivity and spatial resolution. The images are sensitive to the speciation of copper, the depletion of dissolved O(2) in the electrolyte and show the dissolution of Cu(2+) ions is not uniform across the anode

Characterization of Open-Cell Sponges via Magnetic Resonance and X-ray Tomography

The applications of polymeric sponges are varied, ranging from cleaning and filtration to medical applications. The specific properties of polymeric foams, such as pore size and connectivity, are dependent on their constituent materials and production methods. Nuclear magnetic resonance imaging (MRI) and X-ray micro-computed tomography (mu CT) offer complementary information about the structure and properties of porous media. In this study, we employed MRI, in combination with mu CT, to characterize the structure of polymeric open-cell foam, and to determine how it changes upon compression, mu CT was used to identify the morphology of the pores within sponge plugs, extracted from polyurethane open-cell sponges. MRI T-2 relaxation maps and bulk T-2 relaxation times measurements were performed for 7 degrees dH water contained within the same polyurethane foams used for mu CT. Magnetic resonance and mu CT measurements were conducted on both uncompressed and 60% compressed sponge plugs. Compression was achieved using a graduated sample holder with plunger. A relationship between the average T-2 relaxation time and maximum opening was observed, where smaller maximum openings were found to have a shorter T-2 relaxation times. It was also found that upon compression, the average maximum opening of pores decreased. Average pore size ranges of 375-632 +/- 1 mu m, for uncompressed plugs, and 301-473 +/- 1 mu m, for compressed plugs, were observed. By determining maximum opening values and T-2 relaxation times, it was observed that the pore structure varies between sponges within the same production batch, as well as even with a single sponge

Tuning coordination chemistry through the second sphere in designed metallocoiled coils

The metal hydration state within a designed coiled coil can be progressively tuned across the full integer range (3 → 0 aqua ligands), by careful choice of a second sphere terminal residue, including the lesser used Trp. Potential implications include a four-fold change in MRI relaxivity when applied to lanthanide coiled coils.</p

Operando visualisation of battery chemistry in a sodium-ion battery by 23Na magnetic resonance imaging

© 2020, The Author(s). Sodium-ion batteries are a promising battery technology for their cost and sustainability. This has led to increasing interest in the development of new sodium-ion batteries and new analytical methods to non-invasively, directly visualise battery chemistry. Here we report operando 1H and 23Na nuclear magnetic resonance spectroscopy and imaging experiments to observe the speciation and distribution of sodium in the electrode and electrolyte during sodiation and desodiation of hard carbon in a sodium metal cell and a sodium-ion full-cell configuration. The evolution of the hard carbon sodiation and subsequent formation and evolution of sodium dendrites, upon over-sodiation of the hard carbon, are observed and mapped by 23Na nuclear magnetic resonance spectroscopy and imaging, and their three-dimensional microstructure visualised by 1H magnetic resonance imaging. We also observe, for the first time, the formation of metallic sodium species on hard carbon upon first charge (formation) in a full-cell configuration

In situ, real-time visualization of electrochemistry using magnetic resonance imaging

The drive to develop better electrochemical energy storage devices requires the development of not only new materials, but also better understanding of the underpinning chemical and dynamical processes within such devices during operation, for which new analytical techniques are required. Currently, there are few techniques that can probe local composition and transport in the electrolyte during battery operation. In this paper, we report a novel application of magnetic resonance imaging (MRI) for probing electrochemical processes in a model electrochemical cell. Using MRI, the transport and zinc and oxygen electrochemistry in an alkaline electrolyte, typical of that found in zinc-air batteries, are investigated. Magnetic resonance relaxation maps of the electrolyte are used to visualize the chemical composition and electrochemical processes occurring during discharge in this model metal-air battery. Such experiments will be useful in the development of new energy storage/conversion devices, as well as other electrochemical technologies

Centre selection for clinical trials and the generalisability of results: a mixed methods study.

BACKGROUND: The rationale for centre selection in randomised controlled trials (RCTs) is often unclear but may have important implications for the generalisability of trial results. The aims of this study were to evaluate the factors which currently influence centre selection in RCTs and consider how generalisability considerations inform current and optimal practice. METHODS AND FINDINGS: Mixed methods approach consisting of a systematic review and meta-summary of centre selection criteria reported in RCT protocols funded by the UK National Institute of Health Research (NIHR) initiated between January 2005-January 2012; and an online survey on the topic of current and optimal centre selection, distributed to professionals in the 48 UK Clinical Trials Units and 10 NIHR Research Design Services. The survey design was informed by the systematic review and by two focus groups conducted with trialists at the Birmingham Centre for Clinical Trials. 129 trial protocols were included in the systematic review, with a total target sample size in excess of 317,000 participants. The meta-summary identified 53 unique centre selection criteria. 78 protocols (60%) provided at least one criterion for centre selection, but only 31 (24%) protocols explicitly acknowledged generalisability. This is consistent with the survey findings (n = 70), where less than a third of participants reported generalisability as a key driver of centre selection in current practice. This contrasts with trialists' views on optimal practice, where generalisability in terms of clinical practice, population characteristics and economic results were prime considerations for 60% (n = 42), 57% (n = 40) and 46% (n = 32) of respondents, respectively. CONCLUSIONS: Centres are rarely enrolled in RCTs with an explicit view to external validity, although trialists acknowledge that incorporating generalisability in centre selection should ideally be more prominent. There is a need to operationalize 'generalisability' and incorporate it at the design stage of RCTs so that results are readily transferable to 'real world' practice

The aggregation of an alkyl-C₆₀ derivative as a function of concentration, temperature and solvent type

Contrast-variation SANS, SAXS, NMR and ITC measurements show that molecule1associates into micelles with tunable size based on the solution parameters.</p