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At least 1,531 records · Page 85

A two-dimensional analytical unit cell model for redox flow battery evaluation and optimization

Cell performance optimization is important for improving the overall system efficiency of a redox flow battery. To gain better insights into key controlling factors of system efficiency, this work first proposed a theoretical model for a unit flow battery cell by extending a two-dimensional analytic model to a full battery cell. Such a model is then used for cell performance optimization after validating it with experimental and numerical modeling data. With the model results, the activation, equilibrium, and pump energy losses are identified as the dominant sources of battery energy losses. Further, a guideline for reducing these sources is also proposed. Following the guideline, the mass transport coefficient is shown as a key control factor of the equilibrium energy loss and Coulombic efficiency (CE). Approaches are then proposed to improve CE and the overall system efficiency. The mass transport is also revealed as the mechanism of pump rate optimization where an optimal pump rate significantly reduces the equilibrium energy loss. With both low equilibrium and pump energy losses, an optimal electrode porosity or specific area design can further improve a battery's system efficiency based on an optimal porosity predicted by the present model. The model also demonstrates distinct behaviors and overestimation in the system efficiency when reduced to a zero-dimensional model with neglected mass transport resistance. With the new model, the guideline, and new insights, this work provides a reliable and efficient tool for the evaluation and optimization of redox flow battery design in practical applications.

25 ENERGY STORAGE↗

Developing cathode infiltration processes for all-solid-state bilayer LLZO cells

To realize the bilayer architecture of lithium lanthanum zirconate (LLZO) for application in solid-state batteries (SSBs), the scaffold structure must be optimized, and effective cathode infiltration strategies must be established. In this study, we fabricate a modified bilayer LLZO using a sacrificial layer to enhance surface porosity, and systematically investigate various cathode infiltration techniques to fill the scaffold with oxide cathode active materials (CAM). Structural characterizations showed that the sacrificial layer significantly increased open surface porosity, enabling the surface of the scaffold to be filled with CAM. To further increase infiltration depth, applying vacuum or vibration was compared, with the full-depth infiltration achieved using a sonicator-based vibration. Full cells prepared using the modified bilayer LLZO and vibration-assisted technique demonstrated successful operation. This work demonstrates a practical and scalable approach for engineering bilayer LLZO structures and integrating oxide cathodes into porous scaffolds, offering a promising pathway toward high-performance solid-state batteries.

Bilayer↗

Carbon nanosheet-titania nanocrystal composites from reassembling of exfoliated graphene oxide layers with colloidal titania nanoparticles

Nanoporous composites of carbon nanosheets (CNS) and titania nanoparticles (NPs) were synthesized by reassembling of delaminated graphite oxide (GO) layers with titania clear sol (TCS), and their structural and porous properties were examined by various physico-chemical methods such as XRD, TG/DTA, FT-IR, Raman, FE-SEM/TEM, and low temperature N{sub 2} adsorption. It was found that the facile approach, which utilizes the electrostatic attraction between the negatively charged GO layers and the positively charged TCS particles, leads to a well composed CNS and ultrafine TiO{sub 2} NPs material whose titania amount reaches up to 71 wt%. The titania phase in these composite materials is mainly anatase, which is resistible against high temperature calcination, but also contains a little amount of rutile and brookite depending on synthesis condition. The porosity of the composite is improved and partially affected by the size distributions of TiO{sub 2} NPs. The unique structure, better porosity, and compatible surface affinity of these composites bring about an adsorption concentration-promoted photocatalytic effects toward organic dyes by successfully combining both properties of CNS and titania NPs. - Graphical Abstract: Carbon nanosheet-titania nanocrystal composites can be synthesized by a facile delamination-reassembling method from graphene oxide and colloidal titania. Highlights: Black-Right-Pointing-Pointer A facile delamination-reassembling method for graphene oxide-titania nanocomposite. Black-Right-Pointing-Pointer A nanoporous composite containing mixed phase titania nanocrystals. Black-Right-Pointing-Pointer Partition effect of carbon nanosheets preventing TiO{sub 2} nanoparticles from aggregating. Black-Right-Pointing-Pointer Adsorption concentration-promoted photocatalysis.

36 MATERIALS SCIENCE↗

Synthesis of sulfonated porous carbon nanospheres solid acid by a facile chemical activation route

Generally, porous carbon nanospheres materials are usually prepared via a template method, which is a multi-steps and high-cost strategy. Here, we reported a porous carbon nanosphere solid acid with high surface area and superior porosity, as well as uniform nanospheical morphology, which prepared by a facile chemical activation with ZnCl{sub 2} using resorcinol-formaldehyde (RF) resins spheres as precursor. The activation of RF resins spheres by ZnCl{sub 2} at 400 °C brought high surface area and large volume, and simultaneously retained numerous oxygen-containing and hydrogen-containing groups due to the relatively low processing temperature. The presence of these functional groups is favorable for the modification of –SO{sub 3}H groups by a followed sulfonation treating with sulphuric acid and organic sulfonic acid. The results of N{sub 2} adsorption–desorption and electron microscopy clearly showed the preservation of porous structure and nanospherical morphology. Infrared spectra certified the variation of surface functional groups after activation and the successful modification of –SO{sub 3}H groups after sulfonation. The acidities of catalysts were estimated by an indirect titration method and the modified amount of –SO{sub 3}H groups were examined by energy dispersive spectra. The results suggested sulfonated porous carbon nanospheres catalysts possessed high acidities and –SO{sub 3}H densities, which endowed their significantly catalytic activities for biodiesel production. Furthermore, their excellent stability and recycling property were also demonstrated by five consecutive cycles. - Graphical abstract: Sulfonated porous carbon nanospheres with high surface area and superior catalytic performance were prepared by a facile chemical activation route. - Highlights: • Porous carbon spheres solid acid prepared by a facile chemical activation. • It owns high surface area, superior porosity and uniform spherical morphology. • It possesses high acidity and high –SO{sub 3}H density. • It exhibits excellently catalytic performance for esterification of oleic acid.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ultrasound-assisted facile synthesis of a new tantalum(V) metal-organic framework nanostructure: Design, characterization, systematic study, and CO{sub 2} adsorption performance

This work presents a fast route for the preparation of a new Ta(V) metal-organic framework nanostructure with high surface area, significant porosity, and small size distribution. X-ray diffraction (XRD), scanning electron microscopy (SEM), Transition electron microscopy (TEM), energy dispersive spectrometer (EDS), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), CHNS/O elemental analyser, and Brunauer-Emmett-Teller (BET) surface area analysis were applied to characterize the synthesized product. Moreover, the influences of ultrasonic irradiation including temperature, time, and power on different features of the final products were systematically studied using 2{sup k-1} factorial design experiments, and the response surface optimization was used for determining the best welding parameter combination. The results obtained from analyses of variances showed that ultrasonic parameters affected the size distribution, thermal behaviour, and surface area of Ta-MOF samples. Based on response surface methodology, Ta-MOF could be obtained with mean diameter of 55 nm, thermal stability of 228 °C, and high surface area of 2100 m{sup 2}/g. The results revealed that the synthesized products could be utilized in various applications such as a novel candidate for CO{sub 2} adsorption. - Graphical abstract: A facile route was used for fabrication of a new metal -organic framework based on tantalum nanostructures that have high surface area, considerable porosity, homogenous morphology, and small size distribution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Assessing the geomechanical stability of interbedded hydrate-bearing sediments under gas production by depressurization at NGHP-02 Site 16

Establishing the geomechanical stability of marine sediments in the vicinity of a production well is one of the key design considerations in planning offshore gas production from marine hydrate reservoirs. This work presents an assessment of the sediment stability at India's National Gas Hydrate Program, Expedition 2 (NGHP-02) Site 16 Area B offshore eastern India, for which gas production is to be carried out by depressurization. One important feature of the study is that extensive calibration of constitutive model parameters has been conducted based on laboratory test data from pressured core samples. From analysis perspective, the site is challenging because the hydrate reservoir consists of thin layers of hydrate-bearing sands interbedded with mud. Moreover, depressurization at the depth of a reservoir more than 2750 m below sea surface will lead to a pore pressure drop, and accordingly an effective confining stress increase as high as 25 MPa. In dealing with thin interbedded hydrate-bearing strata, meshing requirements for flow and geomechanical analysis are quite different from those for reservoirs with thicker massive layers, An axisymmetric model and one-way coupling simulations were thus adopted for this study, in which the geomechanical study utilizes pore pressure and hydrate saturation output from the flow study, but the flow study does not takes the porosity changes from the geomechanical analysis. Instead, the reduction of porosity due to sediment deformation in the flow study is based on a pressure-dependent pore compressibility relationship derived from geomechanical modeling. The rationality is validated through back computing the pore compressibility from the geomechanical deformation results. Finally, the study shows that large compression in the reservoir will result in movement of the sediments from above and below, as well as laterally in smaller magnitudes; and the sediment is deemed stable during the gas production period.

58 GEOSCIENCES↗

Physical property characteristics of gas hydrate-bearing reservoir and associated seal sediments collected during NGHP-02 in the Krishna-Godavari Basin, in the offshore of India

India’s National Gas Hydrate Program Expedition 02 (NGHP-02) was conducted to better understand geologic controls on gas hydrate occurrence and morphology, targeting coarse-grained sediments along the lower continental slope offshore eastern India. This study combines seismic, logging-while-drilling data, and a petroleum system approach to provide a regional geologic and lithologic context for: 1) gas hydrate morphology and distribution, and 2) effects of fine-grained sediments (clays and other grains smaller than 63µm) on gas production in NGHP-02 Area B in the Krishna-Godavari Basin. Area B seismic data show a buried anticline/syncline structure with strong reflectors, R1 and R2, that delineate two of the five lithologic units: Unit I (shallowest), II (R1), III, IV (R2) and V (below the bas of gas hydrate stability). Throughout Area B, gas hydrate morphology depends on its placement within these units. Specifically, core- and grain-scale measurements indicate fines content exerts a primary control on the gas hydrate distribution and morphology. Units I, II and III are generally fine-grained. On the anticline crest, these units host primarily grain-displacing gas hydrate veins linked to pore-occupying gas hydrate in thin, localized, coarser-grained deposits. Diatoms in Unit III increase porosity with depth, reaching ~70% where it contacts Unit IV, the gas hydrate reservoir associated with reflector R2. The Unit III lithology and porosity allow fluid and dissolved-phase methane to escape Unit IV and form gas hydrate in the fine-grained overburden. Within Unit IV, fine-grained layers are interbedded with coarser-grained gas hydrate reservoir sands, and the fines content even in the sands is high enough to impact hydraulic and mechanical properties during gas production. Fluid motion during gas production can mobilize fines, which can then clog pore throats, limiting production rates. In conclusion, pore-water freshening during gas hydrate dissociation can increase fines mobilization, particularly given the smectite identified in the fine-grained interbeds.

03 NATURAL GAS↗

Properties of the thermally stable Al{sub 95}Cr{sub 3.1}Fe{sub 1.1}Ti{sub 0.8} alloy prepared by cold-compression at ultra-high pressure and by hot-extrusion

An Al{sub 95}Cr{sub 3.1}Fe{sub 1.1}Ti{sub 0.8} (in at.%) alloy was made into rapidly solidified powder by melt atomization. The powder was compacted by two processes: 1) uni-axial cold compression at an ultra-high pressure of 6 GPa and 2) hot extrusion at 480 Degree-Sign C. The structures, mechanical properties and thermal stability of both materials were compared with the commercial AlSi{sub 12}Cu{sub 1}Mg{sub 1}Ni{sub 1} (in wt.%) casting alloy, which is generally considered to be thermally stable. It was found that cold compression at ultra-high pressure created a compact and porosity-free material, which was similar to the material that was prepared with the commonly used hot extrusion method. The Vickers hardness, compressive strength and compressive yield strength of the cold-compressed alloy were 161 HV, 680 MPa and 547 MPa, respectively, which were higher than the values obtained for the hot-extruded and casting alloys. The thermal stability of the hot-extruded Al{sub 95}Cr{sub 3.1}Fe{sub 1.1}Ti{sub 0.8} alloy was excellent because its mechanical properties did not change significantly, even after 100 h of annealing at 500 Degree-Sign C. The mechanical properties and thermal stability of the investigated materials were discussed in relation to their structures and diffusivities of the alloying elements. - Highlights: Black-Right-Pointing-Pointer The Al{sub 95}Cr{sub 3.1}Fe{sub 1.1}Ti{sub 0.8} alloy was prepared by compression at an ultra-high pressure of 6 GPa. Black-Right-Pointing-Pointer The resulting material was dense and porosity-free. Black-Right-Pointing-Pointer The material had high hardness of 161 HV and a compressive strength of 680 MPa. Black-Right-Pointing-Pointer The material had excellent thermal stability at 500 Degree-Sign C.

36 MATERIALS SCIENCE↗

Replication of engine block cylinder bridge microstructure and mechanical properties with lab scale 319 Al alloy billet castings

In recent years, aluminum alloy gasoline engine blocks have in large part successfully replaced nodular cast iron engine blocks, resulting in improved vehicle fuel efficiency. However, because of the inadequate wear resistance properties of hypoeutectic Al–Si alloys, gray iron cylinder liners are required. These liners cause the development of large tensile residual stress along the cylinder bores and necessitate the maximization of mechanical properties in this region to prevent premature engine failure. The aim of this study was to replicate the engine cylinder bridge microstructure and mechanical properties following TSR treatment (which removes the sand binder to enable easy casting retrieval) using lab scale billet castings of the same alloy composition with varying cooling rates. Comparisons in microstructure between the engine block and the billet castings were carried out using optical and scanning electron microscopy, while mechanical properties were assessed using tensile testing. The results suggest that the microstructure at the top and middle of the engine block cylinder bridge was successfully replicated by the billet castings. However, the microstructure at the bottom of the cylinder was not completely replicated due to variations in secondary phase morphology and distribution. The successful replication of engine block microstructure will enable the future optimization of heat treatment parameters. - Highlights: • A method to replicate engine block microstructure was developed. • Billet castings will allow cost effective optimization of heat treatment process. • The replication of microstructure in the cylinder region was mostly successful. • Porosity was more clustered in the billet castings compared to the engine block. • Mechanical properties were lower in billet castings due to porosity and inclusions.

36 MATERIALS SCIENCE↗

Pore- and micro-structural characterization of a novel structural binder based on iron carbonation

The pore- and micro-structural features of a novel binding material based on the carbonation of waste metallic iron powder are reported in this paper. The binder contains metallic iron powder as the major ingredient, followed by additives containing silica and alumina to facilitate favorable reaction product formation. Compressive strengths sufficient for a majority of concrete applications are attained. The material pore structure is investigated primarily through mercury intrusion porosimetry whereas electron microscopy is used for microstructural characterization. Reduction in the overall porosity and the average pore size with an increase in carbonation duration from 1 day to 4 days is noticed. The pore structure features are used in predictive models for gas and moisture transport (water vapor diffusivity and moisture permeability) through the porous medium which dictates its long-term durability when used in structural applications. Comparisons of the pore structure with those of a Portland cement paste are also provided. The morphology of the reaction products in the iron-based binder, and the distribution of constituent elements in the microstructure are also reported. - Highlights: • Carbonation of iron produces a dense microstructure. • Pore volume in iron carbonate lower, critical size higher than those in OPC pastes • Reaction product contains iron, carbon, silicon, aluminum and calcium. • Power-law for porosity-moisture permeability relationship was established.

36 MATERIALS SCIENCE↗

Fractographical characterization of hot pressed and pressureless sintered AlN-doped ZrB{sub 2}–SiC composites

In this paper, ZrB{sub 2}–SiC composites doped with 0–5 wt.% AlN were prepared by a low pressure hot pressing as well as a pressureless sintering methods at 1900 °C for 2 h. The influence of aluminum nitride addition on the sinterability and microstructure development of such ceramic composites was studied by a fractographical approach. The results revealed that only 1 wt.% AlN can aid the densification process of the hot pressed ceramic composite via the liquid phase sintering mechanism due to the formation of nano-scale metakaolinite spinel layers. In the pressureless sintering method, adding more AlN can increase the formation of gaseous products which raised the amount of porosities in the final microstructure. The formation of nano-graphite phase in the hot pressing process, the formation of Al{sub 2}OC in the pressureless sintering process, and the formation of BN in the both processes were disclosed by X-ray diffraction, SEM and TEM analyses. - Highlights: • The effect of AlN addition on densification of ZrB{sub 2}–SiC composites was studied. • AlN promotes the densification in hot pressed samples by liquid phase formation. • A fully dense composite was obtained by adding 1 wt.% AlN in hot pressing process. • In pressureless sintering, more AlN content intensifies the formation of porosities.

36 MATERIALS SCIENCE↗

Fission gas bubble identification using MATLAB's image processing toolbox

Automated image processing routines have the potential to aid in the fuel performance evaluation process by eliminating bias in human judgment that may vary from person-to-person or sample-to-sample. This study presents several MATLAB based image analysis routines designed for fission gas void identification in post-irradiation examination of uranium molybdenum (U–Mo) monolithic-type plate fuels. Frequency domain filtration, enlisted as a pre-processing technique, can eliminate artifacts from the image without compromising the critical features of interest. This process is coupled with a bilateral filter, an edge-preserving noise removal technique aimed at preparing the image for optimal segmentation. Adaptive thresholding proved to be the most consistent gray-level feature segmentation technique for U–Mo fuel microstructures. The Sauvola adaptive threshold technique segments the image based on histogram weighting factors in stable contrast regions and local statistics in variable contrast regions. Once all processing is complete, the algorithm outputs the total fission gas void count, the mean void size, and the average porosity. The final results demonstrate an ability to extract fission gas void morphological data faster, more consistently, and at least as accurately as manual segmentation methods. - Highlights: •Automated image processing can aid in the fuel qualification process. •Routines are developed to characterize fission gas bubbles in irradiated U–Mo fuel. •Frequency domain filtration effectively eliminates FIB curtaining artifacts. •Adaptive thresholding proved to be the most accurate segmentation method. •The techniques established are ready to be applied to large scale data extraction testing.

36 MATERIALS SCIENCE↗

Preparation of amine-impregnated silica foams using agar as the gelling agent

In this work we successfully prepared amine-impregnated gel-cast silica foams using agar and atmospheric air as the gelling agent and heat treatment atmosphere, respectively. The concentration of 3,6-anhydrogalactose in agar was evaluated by ultraviolet–visible spectroscopy (UV–Vis). The obtained foams were examined by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TG) coupled to mass spectrometry (TG-MS), scanning electron microscopy (SEM), X-ray microtomography (micro-CT), and Archimedes method. The cold crushing strength of the materials prepared in this work was assessed using a mechanical testing stage available in the micro-CT system. The obtained foams exhibited a highly interconnected pore network, with an expressive presence of open pores. Samples heat-treated at 1300 °C for 2 h showed both an expressive porosity (≈ 77%) and a significant cold crushing strength (≈ 1.4 MPa). It was observed that the calcination of the prepared materials at 1200 °C for times as long as 16 h may lead to the rupture of pore walls. FTIR and TG-MS revealed that amine groups were properly incorporated into the foams structure. - Highlights: •Successful preparation of amine-impregnated gel-cast silica foams •Agar used as the gelling agent •Samples with expressive porosity and cold crushing strength •Sintering times as long as 16 h led to the rupture of the pore network.

36 MATERIALS SCIENCE↗

Microstructural Progression of Shear-Induced Mixing in a CuNi Alloy

Shear deformation has been highlighted in multiple research efforts for its ability to impart mechanical properties improvements and unique microstructures. When used to process and densify powdered material, these shear-based consolidation techniques are commonly referred to as friction consolidation (FC). In this paper, we have examined the microstructural evolution from compacted Cu and Ni powders to a consolidated Cu0.5Ni0.5 alloy. We have shown various stages of porosity reduction and preferential deformation being accommodated by the more ductile material early in the process, leading to formation of a tortuous microstructural zone. Porosity reduction was extensive, decreasing from ~65% in the unprocessed powder to ~1% in the fully consolidated alloy. The final consolidated alloy showed roughly a 2X hardness improvement over the unalloyed, compacted material. Unique aspects of this work include demonstration of the ability to use FC processing to produce a submicron and equiaxed grain size in samples within a 0.5 to 2 minute processing time.

Overman, Nicole R.↗

Establishing a process-structure-property-performance framework for SLS additive manufacturing through integrated multiscale modeling

This study presents a comprehensive suite of high-fidelity computational models that integrate multiscale and multiphysics simulations to capture the full Selective Laser Sintering (SLS) additive manufacturing process—from initial melting and solidification to mechanical response under external loads. Process simulations are linked with mechanical analysis through Representative Volume Elements (RVEs), establishing a process-structure–property-performance framework. The interaction between laser light and polyamide 12 (PA12) powder is modeled, accounting for laser characteristics and the optical, thermal, and geometrical properties of the powder. The heat source is incorporated into a heat transfer model, coupled with crystallization kinetics and densification models to predict material density and crystallinity. The porosity distribution from the densification model and crystallinity interpolated from experimental data are used to construct the RVEs. A multi-mechanism constitutive model is then calibrated using mechanical tests to predict the stress–strain response. Simulation results show good agreement with experimental data in terms of porosity, crystallinity, and mechanical performance when sufficient laser power (62 W or higher) is used. This research supports the inverse design of 3D-printed structures by introducing a high-fidelity framework that combines multiscale and multiphysics modeling with experimental calibration for predictive and performance-driven additive manufacturing.

SLS↗

The effect of fuel to nitrates ratio on the properties of FeCr{sub 2}O{sub 4} nanopowders

Highlights: • Single phase spinel FeCr{sub 2}O{sub 4} nanopowders were formed without further heat treatment based on powder X-ray diffraction, FTIR and EDS studies. • The probable combustion mechanism with thermodynamic concepts involved in the formation of FeCr{sub 2}O{sub 4} nanopowders were discussed. • The effect of different amount of fuel to metal nitrates ratio (F/N) on the self-combusted FeCr{sub 2}O{sub 4} nanopowders was investigated. • It greatly affects the morphologies, different nanocrystallite sizes, and magnetic properties by using different combinations of F/N ratios. - Abstract: The solution combustion of spinel type FeCr{sub 2}O{sub 4} nanopowders via different ratios of fuel to stating metal nitrates was investigated. The synthesized FeCr{sub 2}O{sub 4} nanopowders were deemed to be single phase spinel type material based on powder X-ray diffraction, FTIR and EDS studies. The properties of synthesized FeCr{sub 2}O{sub 4} nanopowders such as morphology, porosity, elemental composition, crystallite size, strain and lattice deformations, magnetic moment, and coercivity were influenced by the amount of the fuel used in the combustion process. FeCr{sub 2}O{sub 4} nanopowders with different morphologies, porosities, structural, and magnetic properties could be prepared in a single procedure on a hotplate magnetic stirrer without the need for high temperature furnaces.

36 MATERIALS SCIENCE↗

In Situ Investigation of Chemomechanical Effects in Thiophosphate Solid Electrolytes

Solid-state batteries can suffer from catastrophic failure at high current densities due to solid electrolyte fracture, interface decomposition, or lithium filament growth. Failure is linked to chemomechanical material transformations that can manifest during electrochemical cycling. We systematically investigate how solid electrolyte microstructure and interfacial decomposition (e.g., interphase) affect failure mechanisms in lithium thiophosphates (Li3PS4, LPS) electrolytes. Kinetically metastable interphases are engineered with iodine doping, and microstructural control is achieved using milling and annealing processing techniques. In situ transmission electron microscopy reveals iodine diffusion to the interphase, and upon electrochemical cycling, pores are formed in the interphase region. In situ synchrotron tomography reveals that interphase pore formation drives edge fracture events, which are the origin of through-plane fracture failure. Fractures in thiophosphate electrolytes actively grow toward regions of higher porosity and are affected by heterogeneity in microstructure (e.g., porosity factor). This report provides fundamental design guidelines for high-performance solid-state batteries.

25 ENERGY STORAGE↗