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Reversible magnetism switching of iron oxide nanoparticle dispersions by controlled agglomeration
The controlled agglomeration of superparamagnetic iron oxide nanoparticles (SPIONs) was used to rapidly switch their magnetic properties. Small-angle X-ray scattering (SAXS) and dynamic light scattering showed that tailored iron oxide nanoparticles with phase-changing organic ligand shells agglomerate at temperatures between 5 °C and 20 °C. We observed the concurrent change in magnetic properties using magnetic particle spectroscopy (MPS) with a temporal resolution on the order of seconds and found reversible switching of magnetic properties of SPIONs by changing their agglomeration state. The non-linear correlation between magnetization amplitude from MPS and agglomeration degree from SAXS data indicated that the agglomerates' size distribution affected magnetic properties.
Surfactant stabilization of vanadium iron oxide derived from Prussian blue analog for lithium-ion battery electrodes
Due to their high energy density, Li-ion batteries have become indispensable for energy storage in many technical devices. Prussian blue and its analogs are a versatile family of materials. Apart from their direct use as an alkali-ion battery electrode, they are a promising source for templating other compounds due to the presence of carbon, nitrogen, and metallic elements in their structure, ease of synthesis, and high tunability. In this study, homogeneous iron vanadate derivatization from iron vanadium Prussian blue was successfully carried out using an energy efficient infrared furnace utilizing CO2 gas. Iron-vanadate is an inherently unstable electrode material if cycled at low potentials vs. Li/Li+. Several parameters were optimized to achieve a stable electrochemical performance of this derivative, and the effect of surfactants, such as tannic acid, sodium dodecylbenzene sulfonate, and polyvinylpyrrolidone were shown with their role in the morphology and electrochemical performance. While stabilizing the performance, we demonstrate that the type and order of addition of these surfactants are fundamental for a successful coating formation, otherwise they can hinder the formation of PBA, which has not been reported previously. Step-by-step, we illustrate how to prepare self-standing electrodes for Li-ion battery cells without using an organic solvent or a fluorine-containing binder while stabilizing the electrochemical performance. A 400 mA h g−1 capacity at the specific current of 250 mA g−1 was achieved after 150 cycles while maintaining a Coulombic efficiency of 99.2% over an extended potential range of 0.01–3.50 V vs. Li/Li+.
Hydraulic characterisation of iron-oxide-coated sand and gravel based on nuclear magnetic resonance relaxation mode analyses
The capability of nuclear magnetic resonance (NMR) relaxometry to characterise hydraulic properties of iron-oxide-coated sand and gravel was evaluated in a laboratory study. Past studies have shown that the presence of paramagnetic iron oxides and large pores in coarse sand and gravel disturbs the otherwise linear relationship between relaxation time and pore size. Consequently, the commonly applied empirical approaches fail when deriving hydraulic quantities from NMR parameters. Recent research demonstrates that higher relaxation modes must be taken into account to relate the size of a large pore to its NMR relaxation behaviour in the presence of significant paramagnetic impurities at its pore wall. We performed NMR relaxation experiments with water-saturated natural and reworked sands and gravels, coated with natural and synthetic ferric oxides (goethite, ferrihydrite), and show that the impact of the higher relaxation modes increases significantly with increasing iron content. Since the investigated materials exhibit narrow pore size distributions, and can thus be described by a virtual bundle of capillaries with identical apparent pore radius, recently presented inversion approaches allow for estimation of a unique solution yielding the apparent capillary radius from the NMR data. We found the NMR-based apparent radii to correspond well to the effective hydraulic radii estimated from the grain size distributions of the samples for the entire range of observed iron contents. Consequently, they can be used to estimate the hydraulic conductivity using the well-known Kozeny–Carman equation without any calibration that is otherwise necessary when predicting hydraulic conductivities from NMR data. Our future research will focus on the development of relaxation time models that consider pore size distributions. Furthermore, we plan to establish a measurement system based on borehole NMR for localising iron clogging and controlling its remediation in the gravel pack of groundwater wells.
Benchmark study using a multi-scale, multi-methodological approach for the petrophysical characterization of reservoir sandstones
This paper presents a detailed description and evaluation of a multi-methodological petrophysical approach for the comprehensive multi-scale characterization of reservoir sandstones. The suggested methodology enables the identification of links between Darcy-scale permeability and an extensive set of geometrical, textural and topological rock descriptors quantified at the pore scale. This approach is applied to the study of samples from three consecutive sandstone layers of Lower Cretaceous age in northern Israel. These layers differ in features observed at the outcrop, hand specimen, petrographic microscope and micro-CT scales. Specifically, laboratory porosity and permeability measurements of several centimetre-sized samples show low variability in the quartz arenite (top and bottom) layers but high variability in the quartz wacke (middle) layer. The magnitudes of this variability are also confirmed by representative volume sizes and by anisotropy evaluations conducted on micro-CT-imaged 3-D pore geometries. Two scales of directional porosity variability are revealed in quartz arenite sandstone of the top layer: the pore size scale of ∼0.1 mm in all directions and ∼3.5 mm scale related to the occurrence of high- and low-porosity horizontal bands occluded by Fe oxide cementation. This millimetre-scale variability controls the laboratory-measured macroscopic rock permeability. More heterogeneous pore structures were revealed in the quartz wacke sandstone of the intermediate layer, which shows high inverse correlation between porosity and clay matrix in the vertical direction attributed to depositional processes and comprises an internal spatial irregularity. Quartz arenite sandstone of the bottom layer is homogenous and isotropic in the investigated domain, revealing porosity variability at a ∼0.1 mm scale, which is associated with the average pore size. Good agreement between the permeability upscaled from the pore-scale modelling and the estimates based on laboratory measurements is shown for the quartz arenite layers. The proposed multi-methodological approach leads to an accurate petrophysical characterization of reservoir sandstones with broad ranges of textural, topological and mineralogical characteristics and is particularly applicable for describing anisotropy and heterogeneity of sandstones on various rock scales. The results of this study also contribute to the geological interpretation of the studied stratigraphic units.
Ultrathin structures derived from interfacially modified polymeric nanocomposites to curb electromagnetic pollution
The use of electronic devices and wireless networks is increasing rapidly, and electromagnetic (EM) pollution remediation remains a challenge. We employed a unique approach to fabricate two ultrathin (approx. 53 μm) multilayered assemblies to address this. By sequentially stacking thin films of polyvinylidene difluoride (PVDF) and polycarbonate (PC) nanocomposites and interfacially locking them with a mutually miscible polymer (PMMA, polymethyl methacrylate), materials with enhanced structural properties and electromagnetic interference (EMI) shielding performance can be designed. Utilizing reduced graphene oxide (rGO) and molybdenum disulfide (MoS2) as a template, ferrite was grown on the surface to design two different nanohybrid structures (rGO–Fe3O4 and MoS2–Fe3O4). PVDF was composited with either rGO–Fe3O4 or MoS2–Fe3O4, and multiwall carbon nanotubes (CNTs) were dispersed in the PC component. As PC and PVDF are immiscible, their poor interface would result in inferior structural properties, which can be challenging in designing EMI shielding materials due to cyclic thermal fatigue. Hence, PMMA is sandwiched to interfacially stitch the components (PC and PVDF) and improve interfacial adhesion. This was confirmed using SEM/EDS and Raman mapping/imaging. The mechanical stability of the multilayered assemblies was characterized using a dynamic mechanical analyzer (DMA), and the storage modulus was found to be as high as 2767 MPa at 40 °C (@constant frequency and strain amplitude), for the multilayered film with rGO–Fe3O4 in PVDF, PMMA as a sandwich layer and CNTs in PC. A typical assembly of 9 multilayers (∼480 μm) with rGO–Fe3O4 in PVDF, and CNTs in PC, and interfacially stitched with PMMA gave rise to a high EMI shield effectiveness (SET) of −26.3 dB @ 26.5 GHz. This unique arrangement of a multilayered assembly suppressed EMI primarily by absorption.