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At least 91 records · Page 5

Hardness Measurements and Interface Behavior of SiC-B 4 C-Si Multiple Phase Particulate Composites Made with Melt Infiltration and Additive Manufacturing

Reaction-bonded SiC-B 4 C-Si ceramic composites were binder jet 3D-printed and subsequently pressureless-melt-infiltrated with molten Si. The addition of B 4 C aided the Si infiltration to produce a highly dense composite. The microstructures and phases of these composites were examined. The measured hardness values of each constituent with Vickers and nanoindentation matched the bulk values, and the macro-hardness values with Knoop and spherical indentation represented the bulk, composite hardness values of all three phases together, which was close to a rule of mixtures value. For particulate-based composites, this is a significant finding. The interfacial bonds of SiC and Si were imaged using scanning transmission electron microscopy to view intimacy, whereas the crack propagation was examined with carefully placed indents. This work demonstrated that pressureless melt infiltration with a reactive particle provides a method to shape non-wetting reaction-bonded ceramic composites with limited shrinkage and high density and provides insights into the mechanical behavior with numerous indentation techniques.

36 MATERIALS SCIENCE↗

Simple processing via thermal treatment and catalyst infiltration to enhance nickel electrode performance for liquid alkaline water electrolyzers

Two simple processes for enhancing liquid alkaline water electrolyzer performance are demonstrated. Both enhance 3D Ni electrodes by introducing a micron-scale rough structure throughout the bulk of the electrode. Oxidation/reduction relies on a simple thermal treatment cycle to create surface roughening through the volumetric expansion during NiO formation and volume contraction during reduction back to Ni metal. Catalyst infiltration introduces a washcoat of additional metal particles throughout the electrode, by flooding the electrode with catalyst precursor and converting it to micron-scale particles via a reducing thermal treatment. Further, the largest improvement in performance (211mV at 1.8Acm -2 ) is observed for infiltrated NiFe-3x catalyst. For Fe-free Ni-only electrodes, oxidation/reduction provides a larger improvement (157 mV at 1.8Acm -2 ) than infiltrated Ni-3X (106mV at 1.8Acm -2 ). For both processes, the observed electrode surface structure and performance is quite sensitive to the thermal treatment temperature.

08 HYDROGEN↗

A hydrogeophysical framework to assess infiltration during a simulated ecosystem-scale flooding experiment

This study presents a framework to quantify changes in soil saturation in response to flooding caused by extreme hydrologic perturbation on coastal ecosystems at the interfaces and transition between terrestrial and aquatic systems. Subsurface heterogeneity limits the use of in situ measurements to quantify subsurface flow during flooding due to the spatial discontinuity in the measured data. While geophysical methods, including time-lapse electrical resistivity imaging (ERI), are increasingly used to monitor soil hydrological processes, their abilities to parameterize flow models have been underutilized. This study combines background ERI, ground penetrating radar (GPR), time-lapse ERI, soil characterization, and a numerical flow model developed using an Advanced Terrestrial Simulator (ATS) code to quantify the infiltration pathway and describe the hydrological dynamics during a simulated flooding experiment. We assessed the use of two conceptual models developed using [1] ERI and GPR data that described the stratigraphic distribution, and time-lapse ERI that mapped permeability contrast, and [2] information from a national soil database for capturing changes in saturation. Combining the ERI and GPR results with soil core data revealed the stratigraphic heterogeneity at the site with a silty clay layer from 1 to 2 m between an overlying loamy topsoil and an underlying saturated silty sand. This silty clay layer could restrict deep infiltration. The time-lapse ERI showed up to a 35% decrease in resistivity, which correlated with soil moisture data (R 2 value > 0.53) and revealed preferential infiltration zones used to inform the flow model. Numerical simulation results from both the geophysics- and soil database-informed models quantified changes in soil saturation with calculated soil moistures that agreed with field data. The geophysics-informed model captured more of the system’s variability, reflective of shallow subsurface heterogeneities. The framework presented will serve as a precursor for a robust ecohydrological model that can describe the impacts of extreme events induced by climate change on coastal ecosystems.

54 ENVIRONMENTAL SCIENCES↗

Carbon dioxide reduction in solid oxide electrolyzer cells using transition metals infiltrated into Gd 0.1 Ce 0.9 O 1.95 (GDC10) scaffolds

Here, this study reports the catalytic activity of transition metal electrocatalysts (Co, Ni, and Cu) incorporated into Gd 0.1 Ce 0.9 O 1.95 (GDC10) cathodes for the electroreduction of CO 2 in solid oxide electrolyzer cells (SOECs). CO 2 electroreduction performance of cells having porous and non-infiltrated GDC10 cathodes was compared with the performance of cells containing transition metal electrocatalysts infiltrated into porous GDC10 cathodes at 750, 800, and 850°C. Results showed that cells with Co infiltrated cathodes had the best catalytic activity towards CO 2 electroreduction. Furthermore, these cells displayed good stability towards CO electroreduction, having a faradaic efficiency value close to 100% with insignificant voltage increase when tested for 48h at 750 and 850°C under the current densities of 0.2, and 0.4Acm -2 , respectively.

25 ENERGY STORAGE↗

Resolving Triblock Terpolymer Morphologies by Vapor-Phase Infiltration

The spontaneous formation of well-organized three-dimensional (3D) nanostructures from self-assembled block copolymers (BCPs) holds promise for nanofabrication and lithography. The addition of a third block to BCPs provides access to a plethora of 3D geometries, but it remains difficult to resolve the geometry of such “three-color” structures when there is low contrast between the polymeric components at length scales of a few nm. Here, we apply vapor-phase infiltration synthesis to a silicon-containing triblock terpolymer, poly(1,1- dimethyl silacyclobutane-b-styrene-b-lactide) (PDMSB-b-PS-b-PLA or DSL) to distinguish the 3D microdomain morphologies of the two organic blocks, PLA and PS. Selective infiltration of ZnO within the PLA microdomains reveals morphologies consisting of three-color lamellae or lamellae combined with vertically aligned core-shell cylinders, depending on the volume fractions of each block. The infiltration produces ZnO nanoparticles throughout the 260 nm thickness of the DSL film, generating 3D nanocomposites containing ZnO and SiO x . These results provide a strategy for synthesizing multicomponent 3D nanostructures as well as visualizing the phase behavior of multi-block copolymers.

36 MATERIALS SCIENCE↗

Improving the performance for direct electrolysis of CO 2 in solid oxide electrolysis cells with a Sr 1.9 Fe 1.5 Mo 0.5 O 6– δ electrode via infiltration of Pr 6 O 11 nanoparticles

Direct CO 2 electrolysis using solid oxide electrolysis cells (CO 2 -SOECs) holds promise to efficiently convert carbon dioxide to carbon monoxide and oxygen. Cathodes with desirable catalytic activity and chemical stability play a critical role in the development of direct CO 2 -SOECs. Although Sr 2 Fe 1.5 Mo 0.5 O 6–δ (SFM) has exhibited promise for direct CO 2 -SOECs due to its redox stability, it suffers from insufficient activity for the CO 2 reduction reaction (CO 2 RR). Here we report interface engineering of nanosized Pr 6 O 11 on the SFM cathode obtained through infiltration to promote the CO 2 RR performance for direct CO 2 -SOECs. The effect of Pr 6 O 11 loading on the performance of the CO 2 RR is systematically investigated. At 800 °C, the current density of the Pr 6 O 11 infiltrated SFM cathode with an optimum Pr 6 O 11 loading of 14.8 wt% reaches 1.61 A cm –2 at 1.5 V, more than double that of the SFM cathode (0.76 A cm –2 ) under the same operating conditions. X-ray photoelectron spectroscopy (XPS) characterization and in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) analysis indicate that the adsorption ability of CO 2 on the SFM cathode has been significantly improved by the formation of Pr 6 O 11 . Temperature-programmed desorption (TPD) of CO 2 measurements further manifest that a 14.8 wt% Pr 6 O 11 -SFM cathode has better CO desorption capacity. In addition, polarization resistance of the SFM cathode has significantly decreased with the addition of Pr 6 O 11 . Three-electrode measurement was used to analyze the improved electrode kinetics. Finally, these results demonstrate that the formation of Pr 6 O 11 in the SFM cathode through infiltration is a promising approach for increasing CO 2 RR activity for CO 2 -SOECs.

03 NATURAL GAS↗

Modeling Microwave-Enhanced Chemical Vapor Infiltration Process for Preventing Premature Pore Closure

The chemical vapor infiltration (CVI) process involves infiltrating a porous preform with reacting gases that undergo chemical transformation at high temperatures to deposit the ceramic phase within the pores, ultimately leading to a dense composite. The conventional CVI process in composite manufacturing needs to follow an isothermal approach to minimize temperature differences between the external and internal surfaces of the preform, ensuring that reactive gases infiltrate internal pores before external surfaces seal. Here, this study addresses the challenge of premature pore closure in CVI processes through microwave heating. A frequency-domain microwave solver is developed in OpenFOAM to investigate volumetric heating mechanisms within the preform. Through numerical studies, we demonstrate the capability of microwave heating of creating an inside-out temperature inversion. This inversion accelerates reactions proximal to the preform center, effectively mitigating the risk of premature external pore closure and ensuring uniform densification. The results reveal a significant enhancement in temperature inversion when high-permittivity reflectors are incorporated to generate resonant waves. This microwave heating strategy is then coupled with high-fidelity direct numerical simulation (DNS) of reacting flow, enabling the analysis of resulting densification processes. The DNS includes detailed chemistry and realistic diffusion coefficients. The numerical results can be used to estimate the impact of microwave-induced temperature inversion on densification in productions.

42 ENGINEERING↗

Modeling Microwave-Enhanced Chemical Vapor Infiltration Process for Preventing Premature Pore Closure

The chemical vapor infiltration (CVI) process involves infiltrating a porous preform with reacting gases that undergo chemical transformation at high temperatures to deposit the ceramic phase within the pores, ultimately leading to a dense composite. The conventional CVI process in composite manufacturing needs to follow an isothermal approach to minimize temperature differences between the external and internal surfaces of the preform, ensuring that reactive gases infiltrate internal pores before external surfaces seal. This study addresses the challenge of premature pore closure in CVI processes through microwave heating. A frequency-domain microwave solver is developed in Open-FOAM to investigate volumetric heating mechanisms within the preform. Through numerical studies, we demonstrate the capability of microwave heating of creating an inside-out temperature inversion. This inversion accelerates reactions proximal to the preform center, effectively mitigating the risk of premature external pore closure and ensuring uniform densification. The results reveal a significant enhancement in temperature inversion when high-permittivity reflectors are incorporated to generate resonant waves. This microwave heating strategy is then coupled with high-fidelity direct numerical simulation (DNS) of reacting flow, enabling the analysis of resulting densification processes. The DNS simulation includes detailed chemistry and realistic diffusion coefficients. The numerical results can be used to estimate the impact of microwave-induced temperature inversion on densification in productions.

Ge, Wenjun↗

Data and scripts associated with the manuscript "A Hydrogeophysical Framework to Assess Infiltration During a Simulated Ecosystem-Scale Flooding Experiment”

This package contains the data and scripts used in "A hydrogeophysical framework to assess infiltration during a simulated ecosystem-scale flooding experiment" (Adebayo et al., 2023). The Geophysics folder contains two subfolders containing Ground Penetrating Radar (GPR) and Electrical Resistivity Imaging (ERI) datasets acquired between August 23 and August 26, 2021. The GPR subfolder contains raw data (Tempest_Project.GPZ) and processed results using the Sensors and Software EKKO Project software. The ERI subfolder contains two additional subfolders named Static and Timelapse. The Static subfolder contains background resistivity datasets acquired before infiltration, both raw and inverted results using the ResIpy code. The Timelapse subfolder contains repeated resistivity datasets acquired during infiltration on two profiles, along with raw and inverted results using the ResIpy code. The Flow model folder contains ATS model simulation files. The Geophysics-informed subfolder contains simulation datasets for two profiles generated using information from the geophysics data. The National_database-informed subfolder contains simulation datasets for two profiles generated using information from a national soil database. Each subfolder contains initial simulation results, multiple ensembles, and final simulation files. The Sensitivity_analysis folder contains the observation files exported from the flow model, notebooks used in running the code, and sensitivity analysis results showing the sensitivity of different parameters over a 48-hour period. We used mutual information-based global sensitivity analysis for the sensitivity analysis, following Jiang et al., 2022. This study shows a novel approach that integrates geophysical data with hydrological modeling to understand subsurface flow during coastal flooding.

54 ENVIRONMENTAL SCIENCES↗

Polymer-Infiltrated Metal–Organic Frameworks for Thin-Film Composite Mixed-Matrix Membranes with High Gas Separation Properties

Thin-film composite mixed-matrix membranes (TFC-MMMs) have potential applications in practical gas separation processes because of their high permeance (gas flux) and gas selectivity. In this study, we fabricated a high-performance TFC-MMM based on a rubbery comb copolymer, i.e., poly(2-[3-(2H-benzotriazol-2-yl)-4-hydroxyphenyl] ethyl methacrylate)-co-poly(oxyethylene methacrylate) (PBE), and metal–organic framework MOF-808 nanoparticles. The rubbery copolymer penetrates through the pores of MOF-808, thereby tuning the pore size. In addition, the rubbery copolymer forms a defect-free interfacial morphology with polymer-infiltrated MOF-808 nanoparticles. Consequently, TFC-MMMs (thickness = 350 nm) can be successfully prepared even with a high loading of MOF-808. As polymer-infiltrated MOF is incorporated into the polymer matrix, the PBE/MOF-808 membrane exhibits a significantly higher CO 2 permeance (1069 GPU) and CO 2 /N 2 selectivity (52.7) than that of the pristine PBE membrane (CO 2 permeance = 431 GPU and CO 2 /N 2 selectivity = 36.2). Therefore, the approach considered in this study is suitable for fabricating high-performance thin-film composite membranes via polymer infiltration into MOF pores.

59 BASIC BIOLOGICAL SCIENCES↗

Accessibility and Mechanical Stability of Nanoporous Zinc Oxide and Aluminum Oxide Coatings Synthesized via Infiltration of Polymer Templates

The conformal nanoporous inorganic coatings with accessible pores that are stable under applied thermal and mechanical stresses represent an important class of materials used in the design of sensors, optical coatings, and biomedical systems. Here, we synthesize porous AlO x and ZnO coatings by the sequential infiltration synthesis (SIS) of two types of polymers that enable the design of porous conformal coatings—polymers of intrinsic microporosity (PIM) and block co-polymer (BCP) templates. Using quartz crystal microbalance (QCM), we show that alumina precursors infiltrate both polymer templates four times more efficiently than zinc oxide precursors. Using the quartz crystal microbalance (QCM) technique, we provide a comprehensive study on the room temperature accessibility to water and ethanol of pores in block copolymers (BCPs) and porous polymer templates using polystyrene-block-poly-4-vinyl pyridine (PS75-b-P4VP25) and polymers of intrinsic microporosity (PIM-1), polymer templates modified by swelling, and porous inorganic coatings such as AlO x and ZnO synthesized by SIS using such templates. Importantly, we demonstrate that no structural damage occurs in inorganic nanoporous AlO x and ZnO coatings synthesized via infiltration of the polymer templates during the water freezing/melting cycling tests, suggesting excellent mechanical stability of the coatings, even though the hardness of the inorganic nanoporous coating is affected by the polymer and precursor selections. We show that the hardness of the coatings is further improved by their annealing at 900 °C for 1 h, though for all the cases except ZnO obtained using the BCP template, this annealing has a negligible effect on the porosity of the material, as is confirmed by the consistency in the optical characteristics. These findings unravel new potential for the materials being used across various environment and temperature conditions.

36 MATERIALS SCIENCE↗

Self-Cleaning Highly Porous TiO 2 Coating Designed by Swelling-Assisted Sequential Infiltration Synthesis (SIS) of a Block Copolymer Template

Photocatalytic self-cleaning coatings with a high surface area are important for a wide range of applications, including optical coatings, solar panels, mirrors, etc. Here, we designed a highly porous TiO 2 coating with photoinduced self-cleaning characteristics and very high hydrophilicity. This was achieved using the swelling-assisted sequential infiltration synthesis (SIS) of a block copolymer (BCP) template, which was followed by polymer removal via oxidative thermal annealing. The quartz crystal microbalance (QCM) was employed to optimize the infiltration process by estimating the mass of material infiltrated into the polymer template as a function of the number of SIS cycles. This adopted swelling-assisted SIS approach resulted in a smooth uniform TiO 2 film with an interconnected network of pores. The synthesized film exhibited good crystallinity in the anatase phase. The resulting nanoporous TiO 2 coatings were tested for their functional characteristics. Exposure to UV irradiation for 1 h induced an improvement in the hydrophilicity of coatings with wetting angle reducing to unmeasurable values upon contact with water droplets. Furthermore, their self-cleaning characteristics were tested by measuring the photocatalytic degradation of methylene blue (MB). The synthesized porous TiO 2 nanostructures displayed promising photocatalytic activity, demonstrating the degradation of approximately 92% of MB after 180 min under ultraviolet (UV) light irradiation. Thus, the level of performance was comparable to the photoactivity of commercial anatase TiO 2 nanoparticles of the same quantity. Our results highlight a new robust approach for designing hydrophilic self-cleaning coatings with controlled porosity and composition.

36 MATERIALS SCIENCE↗

Development of lightweight aluminum compression panels reinforced by boron-epoxy infiltrated extrusions

Analytical and experimental studies were performed to evaluate the structural efficiencies afforded by the selective reinforcement of conventional aluminum compression panels with unidirectional boron epoxy composite materials. A unique approach for selective reinforcement was utilized called boron/epoxy infiltration. This technique uses extruded metal sections with preformed hollow voids into which unidirectional boron filaments are drawn and subsequently infiltrated with resin to form an integral part. Simplified analytical models were developed to investigate the behavior of stiffener webs with reinforced flanges. Theoretical results are presented demonstrating the effects of transverse shear, of the reinforcement, flange eccentricity and torsional stiffness in such construction. A series of 55 tests were conducted on boron-infiltrated rods and extruded structural sections.

Roy, P. A.↗

A model for estimating time-variant rainfall infiltration as a function of antecedent surface moisture and hydrologic soil type

Recent research indicates that the use of remote sensing techniques for the measurement of near surface soil moisture could be practical in the not too distant future. Other research shows that infiltration rates, especially for average or frequent rainfall events, are extremely sensitive to the proper definition and consideration of the role of the soil moisture at the beginning of the rainfall. Thus, it is important that an easy to use, but theoretically sound, rainfall infiltration model be available if the anticipated remotely sensed soil moisture data is to be optimally utilized for hydrologic simulation. A series of numerical experiments with the Richards' equation for an array of conditions anticipated in watershed hydrology were used to develop functional relationships that describe temporal infiltration rates as a function of soil type and initial moisture conditions.

Wilkening, H. A.↗

Melt-Infiltration Process For SiC Ceramics And Composites

Reactive melt infiltration produces silicon carbide-based ceramics and composites faster and more economically than do such processes as chemical vapor infiltration (CVI), reaction sintering, pressureless sintering, hot pressing, and hot isostatic pressing. Process yields dense, strong materials at relatively low cost. Silicon carbide ceramics and composites made by reactive melt infiltration used in combustor liners of jet engines and in nose cones and leading edges of high-speed aircraft and returning spacecraft. In energy industry, materials used in radiant-heater tubes, heat exchangers, heat recuperators, and turbine parts. Materials also well suited to demands of advanced automobile engines.

Behrendt, Donald R.↗

Reactive Melt Infiltration Of Silicon Into Porous Carbon

Report describes study of synthesis of silicon carbide and related ceramics by reactive melt infiltration of silicon and silicon/molybdenum alloys into porous carbon preforms. Reactive melt infiltration has potential for making components in nearly net shape, performed in less time and at lower temperature. Object of study to determine effect of initial pore volume fraction, pore size, and infiltration material on quality of resultant product.

Behrendt, Donald R.↗

Theoretical considerations for Reaction-Formed Silicon Carbide (RFSC) formation by molten silicon infiltration into slurry-derived preforms

For reaction-formed silicon carbide (RFSC) ceramics produced by silicon melt infiltration of porous carbon preforms, equations are developed to relate the amount of residual silicon to the initial carbon density. Also, for a slurry derived preform containing both carbon and silicon powder, equations are derived which relate the amount of residual silicon in the RFSC to the relative density of the carbon in the preform and to the amount of silicon powder added to the slurry. For a porous carbon preform that does not have enough porosity to prevent choking-off of the silicon infiltration, these results show that complete silicon infiltration can occur by adding silicon powder to the slurry mixture used to produce these preforms.

Behrendt, D. R.↗

A study of metal-ceramic wettability in SiC-Al using dynamic melt infiltration of SiC

Pressure-assisted infiltration with a 2014 Al alloy of plain and Cu-coated single crystal platelets of alpha silicon carbide was used to study particulate wettability under dynamic conditions relevant to pressure casting of metal-matrix composites. The total penetration length of infiltrant metal in porous compacts was measured at the conclusion of solidification as a function of pressure, infiltration time, and SiC size for both plain and Cu-coated SiC. The experimental data were analyzed to obtain a threshold pressure for the effect of melt intrusion through SiC compacts. The threshold pressure was taken either directly as a measure of wettability or converted to an effective wetting angle using the Young-Laplace capillary equation. Cu coating resulted in partial but beneficial improvements in wettability as a result of its dissolution in the melt, compared to uncoated SiC.

Asthana, R.↗