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Optimizing Porous Transport Layer Porosity for Proton Exchange Membrane Water Electrolysis

An empirical model is presented that describes anode-side losses related to porous transport layer (PTL) morphology in proton exchange membrane water electrolysis (PEMWE). The model is based on an advanced voltage breakdown analysis that links various overpotentials to PTL morphology. Custom Ti PTLs, spanning uncommonly low porosities (22 - 31%), were fabricated and analyzed with X-ray CT to obtain pore and particle size distributions. Particle size distributions were consistent across samples with an average particle diameter of 12.0?..mu..m, whereas average pore diameters ranged from 6.0 to 7.0?..mu..m. The PTLs were tested in standard PEMWE cell assemblies with anode catalyst loadings of 0.1 mgIr cm-2 to obtain polarization curves, electrochemical impedance spectra, and augmented Tafel analysis. The PTL-dependent anode side losses were deconvoluted and assigned to excess utilization, concentration, ion transport resistance, and electrical contact resistance overpotentials. The data and model reveal an optimal 20 - 28% PTL porosity region where utilization and contact resistance overpotentials are minimized without triggering concentration and ion transport losses related to water deprivation. The optimal PTL porosity depends on the operating current density and is demonstrated at realistic PEMWE water flow rates to establish PTL design guidance for operation at scale.

08 HYDROGEN

Vapor-phase pillarization of MXenes for engineering hierarchical interlayer porosity

MXenes, a family of two-dimensional (2D) multilamellar materials, possess excellent thermal and electronic properties for a range of applications. Their use in heterogeneous catalysis, however, is limited by the low surface area resulting from stacked layers. Pillarization with inorganic oxides can create more open, mesoporous MXene structures, improving accessibility for guest species to diffuse, reside or react in the space between 2D layers. A previous liquid-phase pillarization method, however, involves excessive use of solvent-based precursors and multiple processing steps. Here, we report a vapor-phase pillarization (VPP) strategy to introduce pillars, exemplified by silica pillars, with high pillar precursor usage efficiency and a simplified processing workflow. The resulting silica-pillared mesoporous MXene exhibits significantly increased surface area and porosity. These textural properties can be easily tuned by the VPP synthesis conditions. When applied as a ruthenium (Ru) catalyst support for the hydrogenolysis of low-density polyethylene (LDPE), the silica-pillared MXene enabled high Ru dispersion and catalytic activity. This study highlights the potential of the VPP method for engineering mesoporous, 2D MXene materials and demonstrates the effectiveness of mesoporous MXene as a catalyst support in overcoming mass transport and active-site accessibility challenges in heterogeneous catalysis involving bulky substances, such as plastics upcycling.

Luo, Song [University of Delaware, Newark, DE (Uni

A General Solution Route to Nanoporous Metal Oxide Films

Metal oxide semiconductors are of interest as efficient, stable, and low-cost photoanode materials for photoelectrochemical water splitting, but their characteristically poor charge transport properties remain a fundamental challenge to practical use. Nanoporous metal oxide films that feature open bicontinuous networks of nanocrystals and nanopores can overcome such inefficient charge transport to enable high-performance photoanodes. Here, this paper describes a general method to make high-quality nanoporous films of metal oxides by spin coating and calcining molecular inks that contain a porosity-generating block copolymer. Phase-pure nanoporous films of BiFeO 3 , FeWO 4 , WO 3 , Fe 2 O 3 , and TiO 2 serve to demonstrate the versatility of the approach. It is demonstrated that the crystallite size, film porosity, and film thickness can be independently tuned by adjusting the ink composition and film processing conditions. The method is extended to fabricate core–shell nanoporous films consisting of a nanoporous film coated in a thin shell of a second metal oxide, using WO 3 –BiVO 4 and BiFeO 3 –BiVO 4 as examples. Given its simplicity and flexibility, this solution-phase route should prove useful for making nanoporous films of many different materials for a variety of applications, including energy conversion and storage, catalysis, and chemical sensing.

coating materials

Thermal Inspection for the Assessment of Adhesively Bonded Metal Adherents

Certification of adhesively bonded structures is currently a challenge for aircraft manufacturers. The ability to certify bonds in primary structure can reduce dependence on fasteners and this will enable more efficient manufacturing. For example, drilling holes and installing fasteners in bonded joints can be a potentially significant bottleneck in airframe manufacturing. In addition, fasteners increase the airframe weight and can add stress concentration areas. Reducing fastener count can accelerate manufacturing and improve aircraft performance. NASA is currently investigating nondestructive evaluation (NDE) techniques to assess bond integrity. For example, bond thickness influences bond strength and therefore NDE techniques are being investigated to determine bond thickness. For bonded metal structures, there is a large difference in the thermal diffusivity between the 7075 aluminum alloy metal adherends and aircraft grade adhesive. Multi-layered thermal models show a large variation in the thermal response for bondline adhesive thicknesses that vary from 100 to 300 microns for adherend thicknesses of 0.163 cm. Experimental through-transmission thermal measurements reveal promise to quantitatively characterize the bondline thickness. Results were validated with X-ray computed tomography and optical microscopy measurements, and influence of porosity on the thermal model and measurements are investigated.

bondline thickness

Thermal Inspection for the Assessment of Adhesively Bonded Metal Adherends

Certification of adhesively bonded structures is currently a challenge for aircraft manufacturers. The ability to certify bonds in primary structure can reduce dependence on fasteners and this will enable more efficient manufacturing. For example, drilling holes and installing fasteners in bonded joints can be a potentially significant bottleneck in airframe manufacturing. In addition, fasteners increase the airframe weight and can add stress concentration areas. Reducing fastener count can accelerate manufacturing and improve aircraft performance. NASA is currently investigating nondestructive evaluation (NDE) techniques to assess bond integrity. For example, bond thickness influences bond strength and therefore NDE techniques are being investigated to determine bond thickness. For bonded metal structures, there is a large difference in the thermal diffusivity between the 7075 aluminum alloy metal adherends and aircraft grade adhesive. Multi-layered thermal models show a large variation in the thermal response for bondline adhesive thicknesses that vary from 100 to 300 microns for adherend thicknesses of 0.163 cm. Experimental through-transmission thermal measurements reveal promise to quantitatively characterize the bondline thickness. Results were validated with X-ray computed tomography and optical microscopy measurements, and influence of porosity on the thermal model and measurements are investigated.

X-ray computed tomography

Effect of directed energy deposition process parameter on build quality of tantalum

Tantalum is a refractory metal used in a variety of harsh environment applications. Additive manufacturing of tantalum is limited based on its high melting point and affinity for oxygen. Directed Energy Deposition is an additive manufacturing technique with rapid deposition time and compositional flexibility within builds. Additively manufactured tantalum is susceptible to a variety of material and process-based defects. Various lack-of-fusion defects were identified resulting from excessive powder feed rates or insufficient laser power. Oxygen impurities in some samples caused cracking and increased material hardness. Precipitates were identified in the highly oxidized samples which were printed immediately after the build chamber was opened. High-density, low-defect parts were successfully produced. The effects of scan speed, laser power, and powder feed rate on density and defects were analyzed. A processing window was identified for producing high-quality parts which requires adequately high laser power and lower powder feed rate.

DED

Graphitization of banana peel – synergistic effect of Ca and other elements of the biomass on carbon structure transformation

Recently, growing interest has been observed in using calcium as an effective catalyst for graphitizing disordered carbon materials derived from biomass and bioprecursors, such as cellulose and lignin, at relatively low tem peratures (<2000 °C). Herein, it is demonstrated that in the presence of elements such as calcium, silicon, sulfur, and potassium, which are abundant in banana peel composed of cellulose and lignin base, graphitization occurs much more effectively. The addition of external calcium source, in the form of calcium carbonate, to the banana peel-derived carbon and heat-treatment of the mixture under protective atmosphere up to 1750 °C results in a significant increase in the degree of the graphitization order and local formation of graphite crystals, whereas the same preparation and heat-treatment procedure applied to carbon material derived from pristine cellulose does not lead to such effective graphitization. It is indicated that the graphitization of banana peel carbon occurs due to the synergistic effect of the external Ca-based catalyst and the internal elements present in the raw biomass, supporting the transformation of the disordered graphene-like layers into graphitic structures. These findings are important for the future production of green graphite from biomass

09 BIOMASS FUELS

Expanding the Horizons of Polymer Aerogels

As the Space Community endeavors to reach new heights of human exploration, materials for extreme environments are at the forefront of research. One class of materials of particular focus are polymer aerogels; lightweight solids with nanoscale pore size, high internal surface area, and extremely high porosities. These interesting properties allow aerogels to act as superior thermal insulators, IR scattering filters, sensor platforms, and vibro-acoustic mitigating materials. Polymer aerogels also have the potential to combat issues found in lunar environments such as dust and radiation mitigation. Herein, past and present research, synthesis, and applications of polymer aerogels will be discussed.

Stephanie L Vivod

Glancing Angle Deposition in Gas Sensing: Bridging Morphological Innovations and Sensor Performances

Glancing Angle Deposition (GLAD) has emerged as a versatile and powerful nanofabrication technique for developing next-generation gas sensors by enabling precise control over nanostructure geometry, porosity, and material composition. Through dynamic substrate tilting and rotation, GLAD facilitates the fabrication of highly porous, anisotropic nanostructures, such as aligned, tilted, zigzag, helical, and multilayered nanorods, with tunable surface area and diffusion pathways optimized for gas detection. This review provides a comprehensive synthesis of recent advances in GLAD-based gas sensor design, focusing on how structural engineering and material integration converge to enhance sensor performance. Key materials strategies include the construction of heterojunctions and core–shell architectures, controlled doping, and nanoparticle decoration using noble metals or metal oxides to amplify charge transfer, catalytic activity, and redox responsiveness. GLAD-fabricated nanostructures have been effectively deployed across multiple gas sensing modalities, including resistive, capacitive, piezoelectric, and optical platforms, where their high aspect ratios, tailored porosity, and defect-rich surfaces facilitate enhanced gas adsorption kinetics and efficient signal transduction. These devices exhibit high sensitivity and selectivity toward a range of analytes, including NO2, CO, H2S, and volatile organic compounds (VOCs), with detection limits often reaching the parts-per-billion level. Emerging innovations, such as photo-assisted sensing and integration with artificial intelligence for data analysis and pattern recognition, further extend the capabilities of GLAD-based systems for multifunctional, real-time, and adaptive sensing. Finally, current challenges and future research directions are discussed, emphasizing the promise of GLAD as a scalable platform for next-generation gas sensing technologies.

Chemistry

Investigation of Lunar-Inspired Geopolymer Concrete Formulations Mixed and Cured in Microgravity on the International Space Station (ISS)

The research outlined in this presentation investigates the use of various lunar regolith simulants in geopolymer lunar concrete mixes mixed and cured on the International Space Station (ISS). The motivation for this work is to study the effects of gravity on the microstructure of alkali-activated materials cured with heat, and to develop materials for the construction of long-term infrastructure on the lunar surface with in-situ resource utilization (ISRU). ISRU for construction materials reduces the cost and mass of payloads related to lunar construction. The advantage of geopolymer concrete as opposed to traditional portland cement concrete is that water acts as a medium for the polymerization reaction and leaves the system throughout the process, reducing its demand. Twelve samples of lunar regolith simulant and a solution composed of sodium hydroxide and sodium silicate were sent to the ISS. The three simulants were OPRH2N, OPRL2N, and JSC-1AF, using only particles less than 53 µm in diameter to increase reactivity of the simulant. Simulant to solution ratios were determined by workability while mixing. The simulant and solution were sealed Burst Pouches® along with 2 other sealed bags to prevent material from leaking. Crew member F-14 conducted testing on the ISS by introducing the solution to the simulant in the Burst Pouch®, mixing the sample with a spatula, and then clamping the specimen in the fresh state to prevent flow inside the Burst Pouch®. These specimens were then put in a thermos heated to 80C via sealed drinking water bags to cure for 24 hours with a temperature logger. The cured specimens remained in microgravity for at least 28 days and were returned from the ISS in February 2025. The specimens were then brought to the NASA Marshall Space Flight Center (MSFC) to analyze. Material characterization consisted of conducting Micro-CT tests of entire samples in their sealed apparatus to a resolution of 25µm. 2D image slices were saved in each orthogonal direction of each specimen at a 0.03 mm step size from the 3D model to conduct analytical porosity calculations. Representative samples from each specimen were sampled to perform helium gas pycnometery and were then mounted in resin for SEM imaging, EDS, and nanoindentation. Porosity was analyzed analytically using micromechanics modelling with the assistance of the NASA Multiscale Analysis Tool (NASMAT), as well as the NASA Advanced Supercomputing (NAS) servers (V. Saseendran & N. Yamamoto, 2024). Density was measured using helium gas pycnometery and was then compared to the theoretical density for experimental porosity calculation. Due to the samples’ non-uniform shape being cured in a pouch, traditional compression and tensile strength testing could not be performed. Nanoindentation was conducted at Clarkson University to determine the microhardness and reduced modulus of elasticity. Results from flight samples can be compared to ground samples currently in DLR’s possession to determine the effect on microstructure from being mixed and cured in microgravity. This study gives further insight and understanding of geopolymer lunar concrete and its viability as a lunar construction material with ISRU.

Adam Johnson

Highly Porous Polyimide Gel for Use as Battery Separator with Room Temperature Ionic Liquid Electrolytes

Advanced aerospace vehicular concepts require advances in many existing technologies, including space power and energy storage systems. Batteries represent one of the major areas in need of improvement, both in terms of energy density and safety, with growing concerns over the fire safety of commercial lithium-ion batteries. This has prompted efforts to develop nonflammable battery components, namely the electrolyte and separator. Existing commercial lithium-ion batteries utilize polyolefin microporous membranes as separators with an electrolyte consisting of a lithium salt dissolved in a mixture of cyclic carbonate solvents. This separator/electrolyte combination has ionic conductivities in the range of 10 −2 to 10 −3 S/cm. However, the cyclic carbonate solvents are inherently flammable. Room-temperature ionic liquids (RTILs) appear to be a safer alternative. They offer good ionic conductivities and are inherently nonvolatile and nonflammable, giving them a safety advantage. However, many promising RTILs for battery electrolytes are not compatible with commercial polyolefin separator materials. Alternative separator materials, such as polyimides, are non-flammable and are capable of accepting RTILs into their structure. Polyimide gels, with a composition of 4,4′-oxydianiline, 3,3′,4,4′-tetracarboxylic dianhydride and cross-linked with Desmodur N3300A, possess an open-porous, fibrillar network architecture which offers a high degree of porosity (typically greater than 85% porosity) for lithium-ion transport and conduction, as well as good mechanical properties. Furthermore, these polyimide gels are compatible with selected imidazolium-based RTILs. Nonflammable separator/electrolyte systems with room-temperature conductivities in the range of 10 −3 S/cm have been evaluated. It has been demonstrated that 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide was the most promising among six RTILs screened, in terms of both ionic conductivity and constant current cycling.

Polyimide

In Situ Synchrotron Micro-CT of Microballoon-Filled RTV Silicone During Thermal Decomposition

This work investigates the thermal decomposition of microballoon-filled room-temperature-vulcanizing (RTV) silicone using time-resolved synchrotron micro-CT at the Advanced Light Source. In situ imaging of constrained and unconstrained samples captures the evolution of the internal microstructure during heating, including material expansion, microballoon and void growth, tearing, pyrolysis, shrinkage, and increasing porosity. The measurements provide new insight into the mechanisms governing RTV degradation and generate three-dimensional data for future quantitative analysis and material-response model development.

TPS

The Effects of Gravity on Combustion and Structure Formation During Combustion Synthesis in Gasless Systems

There have been relatively few publications examining the role of gravity during combustion synthesis (CS), mostly involving thermite systems. The main goal of this research was to study the influence of gravity on the combustion characteristics of heterogeneous gasless systems. In addition, some aspects of microstructure formation processes which occur during gasless CS were also studied. Four directions for experimental investigation have been explored: (1) the influence of gravity force on the characteristic features of heterogeneous combustion wave propagation (average velocity, instantaneous velocities, shape of combustion front); (2) the combustion of highly porous mixtures (with porosity greater than that for loose powders), which cannot be obtained in normal gravity; (3) the effect of gravity on sample expansion during combustion, in order to produce highly porous materials under microgravity conditions; and (4) the effect of gravity on the structure formation mechanism during the combustion synthesis of poreless composite materials.

Arvind Varma

X-ray tomography of damage dynamics in advanced materials using a laser wakefield accelerator

Additively manufactured (AM) metals offer the potential for customizable, cost-effective components, but qualification and certification are crucial. Key to this process is understanding pore dynamics under stress, typically analyzed using micro-computed tomography. This study introduces laboratory-scale “betatron” x-rays from laser wakefield acceleration as a high-throughput alternative for x-ray tomography of advanced materials, such as AM AlSi10Mg alloys. Coupled with 3D finite element modeling, this method provides detailed insights into stress-porosity interactions. The approach delivers high-resolution scans, revealing that pore shape and local triaxiality significantly influence fracture dynamics, supporting advanced material characterization. This work also demonstrates the potential and versatility of laser-betatron x-ray μCT for generating large datasets to accelerate our understanding of the stochastic, process-specific nature of pore formation in AM alloys.

Senthilkumaran, Vigneshvar

Thermo-Poro-Mechanical Modeling of RTV Intumescence

Room temperature vulcanizing (RTV) silicone is a high-temperature adhesive used as a gap-filler between heatshield tiles in numerous entry missions. Its propensity to intumesce, or swell upon exposure to heat, is a well-known effect that needs to be carefully quantified during design. At tile interfaces of charring ablators, intumescence, combined with differential recession, could cause the gap filler to protrude past the ablator outer mold line, forming a “fence”. Fencing can in turn cause transition to turbulence of the flow wetting the heat shield, leading to augmented surface heating. Recent experiments conducted at the Plasmatron X facility, the high enthalpy wind tunnel of the Center for Hypersonics and Entry Systems Studies, have shown prominent fencing of RTV gap fillers in PICA, under both nitrogen and air plasmas. Similar observations are well known in the arcjet literature. Further experiments under controlled environment, performed using in situ X-ray micro-computed tomography (micro-CT) at the Advanced Light Source (ALS), have shown heating rate-dependent swelling and shrinkage of RTV during pyrolysis. To simulate RTV intumescence, a novel model was introduced in the Porous Materials Analysis Toolbox based on OpenFOAM, PATO, to account for pore-pressure buildup within both closed- and open-pores. The governing equation for the thermo-poro-mechanical response were developed, assuming linear elasticity for the charring silicone. A new multi-pyrolysis model that tracks non-monotonic advancement of material properties with pyrolysis was proposed. This model addresses the limitations of state-of-the-art ablator models to capture the different stages of thermal degradation and coupled thermomechanics. Swelling of RTV was simulated using the new thermo-poro-mechanical model and compared against in situ micro-CT data. Results showed good agreement in intumescence height and temperature profiles at all heating rates, indicating that the key factor contributing to RTV swelling is the internal pressure build-up within closed- and open-pores. As RTV is cured into a soft (rubbery) compound with low-porosity and permeability, initial temperature increase and pyrolysis gas production cause a significant increase of internal pressure, causing a pronounced volume growth. As thermal degradation progresses, rigidization of the silicone occurs due to char hardening which counteract volume shrinkage after gas pressure relief. Overall, our model shows that accounting for changes in properties such porosity, permeability and key thermomechanical coefficients is crucial for capturing the RTV volume change during ablation and enable a predictive capability for heatshield tile interface response. A plan for future calibration of thermomechanical properties evolution during degradation is discussed, as a key next step to close the new model.

RTV

Thermo-Poro-Mechanical Modeling of RTV Intumescence

Room temperature vulcanizing (RTV) silicone is a high-temperature adhesive used as a gap-filler between heatshield tiles in numerous entry missions. Its propensity to intumesce, or swell upon exposure to heat, is a well-known effect that needs to be carefully quantified during design. At tile interfaces of charring ablators, intumescence, combined with differential recession, could cause the gap filler to protrude past the ablator outer mold line, forming a “fence”. Fencing can in turn cause transition to turbulence of the flow wetting the heat shield, leading to augmented surface heating. Recent experiments conducted at the Plasmatron X facility, the high enthalpy wind tunnel of the Center for Hypersonics and Entry Systems Studies, have shown prominent fencing of RTV gap fillers in PICA, under both nitrogen and air plasmas. Similar observations are well known in the arcjet literature. Further experiments under controlled environment, performed using in situ X-ray micro-computed tomography (micro-CT) at the Advanced Light Source (ALS), have shown heating rate-dependent swelling and shrinkage of RTV during pyrolysis. To simulate RTV intumescence, a novel model was introduced in the Porous Materials Analysis Toolbox based on OpenFOAM, PATO, to account for pore-pressure buildup within both closed- and open-pores. The governing equation for the thermo-poro-mechanical response were developed, assuming linear elasticity for the charring silicone. A new multi-pyrolysis model that tracks non-monotonic advancement of material properties with pyrolysis was proposed. This model addresses the limitations of state-of-the-art ablator models to capture the different stages of thermal degradation and coupled thermomechanics. Swelling of RTV was simulated using the new thermo-poro-mechanical model and compared against in situ micro-CT data. Results showed good agreement in intumescence height and temperature profiles at all heating rates, indicating that the key factor contributing to RTV swelling is the internal pressure build-up within closed- and open-pores. As RTV is cured into a soft (rubbery) compound with low-porosity and permeability, initial temperature increase and pyrolysis gas production cause a significant increase of internal pressure, causing a pronounced volume growth. As thermal degradation progresses, rigidization of the silicone occurs due to char hardening which counteract volume shrinkage after gas pressure relief. Overall, our model shows that accounting for changes in properties such porosity, permeability and key thermomechanical coefficients is crucial for capturing the RTV volume change during ablation and enable a predictive capability for heatshield tile interface response. A plan for future calibration of thermomechanical properties evolution during degradation is discussed, as a key next step to close the new model.

silicone intumescence

Solvent-Free Preparation of High Energy, Binder-Free Electrodes Enabled by Dry Compressible Holey Graphene

Graphene is an atomically thick sheet consisting of a graphitic carbon network with excellent mechanical strength, electrical and thermal conductivity, and chemical stability. Holey graphene, a structural derivative of graphene, has an array of through-the-thickness holes across the lateral surface of the nanosheet. The presence of these holes has minimal detrimental effect on the graphene properties and leads to enhanced performance in applications such as electronics, sensors, and energy storage. For example, these holes allow more facile cross-plane ion and gas transport than intact graphene, making holey graphene an ideal electrode material for electrochemical energy storage. This presentation will focus on the ability of holey graphene to be compression molded into robust articles or architectures under solvent-free conditions without the need for potentially parasitic binders. The unique dry compressibility of holey graphene has enabled facile fabrication of high mass loading electrodes with both high density and high porosity, which have found use in supercapacitors and various high-energy battery systems such as lithium-oxygen, lithium-sulfur, and lithium-selenium batteries.

Yi Lin