Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “composition and microstructure”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 829 records · Page 46

Microstructural Assessment of Molybdenum Disulfide Coatings Using Nanoindentation Hardness

MoS 2 coatings are used extensively in aerospace and defense applications due to their ultralow friction and high wear resistance. Burnished and resin-bonded MoS 2 coatings are commonly used in these applications due to simplicity in deposition and history of use, despite issues with consistency in coating properties and performance. Physical vapor deposition (PVD) of MoS 2 thin films has emerged as a process alternative in the past 50 years, promising far greater control over film structure and composition but at a greater cost. Despite PVD’s benefits, hesitance to adoption persists in high-consequence applications, not only due to increased costs but variability in resulting coating properties. These variations in properties and subsequent performance are in part due to the complexity of the PVD process and the sensitive interplay between coating process-structure-property relationships. This work aims to demystify the remaining uncertainties of the process-structure-property relationships in PVD MoS 2 . The microstructure and mechanical and tribological properties of 61 different PVD pure MoS 2 coatings are examined herein. Emphasis has been placed on developing performance-based (i.e., hardness, modulus) metrics that can assess microstructural changes (density, orientation, and crystallinity) and be utilized to accelerate process development and coating optimization. Relationships established within suggest that nanoindentation hardness can be used to infer coating performance (i.e., wear rate) and properties (i.e., density, crystalline texture, and stoichiometry). Furthermore, this work demonstrates that PVD MoS 2 coatings close to the theoretical density of MoS 2 consistently have the best tribological performance and can be reliably identified by their hardness.

MoS2↗

Engineering & Microstructure Scale PIE Report on EBR-II X441A Metallic Fuel Pins for the MORPH Experiment

The objectives of this project are to increase fundamental understanding of irradiation induced metallic U-Pu-Zr fuel behavior and to obtain data needed for the development of irradiation models for metallic fuels in MARMOT. The requested metallic fuel pins are from the X441A experiment irradiated in Experimental Breeder Reactor (EBR)-II and will be provided by the PIs for the duration of the experiment. The purpose of the pins irradiated in the X441A assembly was to vary Zr composition and fuel slug diameter in order to provide data for the metallic fuel performance code “LIFEMETAL” [ANL-IFR-125]. The fuels of interest to this project are metallic fuels with several Zr compositions (in wt.%): U-19Pu-6Zr, U-19Pu-10Zr, and U-19Pu-14Zr, which were irradiated to a peak burnup of approximately 11 at.%. The cladding was the same for all three fuel pins (austenitic stainless steel D9), which allows investigation of fuel-cladding interaction (FCI) phenomena. Varying Zr content in fuel pins enables investigation of the effect of Zr on fuel restructuring and fuel-cladding compatibility. Engineering and microstructure scale PIE activities will be focused on investigation of fundamental aspect of fuel performance such as species diffusion and migration, fission product behavior, and constituent redistribution. Obtained microstructural information will be used as the basis for the development of MARMOT models of U-Pu-Zr fuel performance at the mesoscale. Experimental data obtained through this proposal will be used to provide this fundamental understanding which will serve as the foundation of the development of radiation models for U-Pu-Zr in MARMOT. It will also provide a starting point for the design of new experiments to provide data for the validation of these MARMOT models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructural evolution and phase stability in Nb-containing interstitial Fe-Mn-Co-Cr-C high-entropy alloys: An in-situ synchrotron X-ray diffraction study during laser melting

The influence of Nb on phase stability and microstructural evolution in an interstitial Fe-Mn-Co-Cr-C high-entropy alloy was investigated using in-situ synchrotron X-ray diffraction (SXRD) during laser melting. Scheil-Gulliver simulations predict the formation of σ and γ-f.c.c. phases in all three alloys, along with NbC in Nb-containing compositions. SXRD confirmed the presence of most predicted phases, but the σ phase was absent. Nb promotes crystallite refinement and increases dislocation density, though excessive additions reduce refinement efficiency due to solubility limits and secondary phase formation. Furthermore, Nb addition also enhances ε-h.c.p. phase formation by reducing stacking fault energy through NbC-induced carbon depletion. Analysis of intensity peak evolution reveals that Nb alters preferred grain orientations, reducing {111} γ intensity while enhancing {220} γ , leading to a more isotropic grain distribution. Overall, Nb plays a key role in phase selection, microstructure refinement, and preferred orientation evolution, allowing the tailored microstructure of high-entropy alloys via rapid solidification.

Interstitial high entropy alloys↗

Microstructure-dependent particulate populations in ODS steels revealed by single-particle ICP-TOF-MS

In this work, we evaluated the ability of single-particle inductively coupled plasma time-of-flight mass spectrometry (SP-ICP-TOF-MS) to characterize particulates generated from 300 series stainless steels and oxide dispersion–strengthened (ODS) steels. Particulates were produced using two different rotary tools (cutting disk and grinding bit) to assess the influence of particle generation on effluent particulates. Across all materials and preparation techniques, SP-ICP-TOF-MS detected a substantial population of particles containing the expected constituent elements, with average compositions closely matching the nominal alloy values. A secondary population of Y-bearing particles was evident in ODS steels; their formation is strongly favored in particulates generated using the grinding bit. Specifically, in PM2000, Y-bearing particles were predominantly colocated with Al, whereas in 14YWT, Y-bearing particles were less frequently Fe-free but showed stronger colocation with Ti. These trends are consistent with the known microstructural differences between Y–Al–O oxide particles in PM2000 and finer Y–Ti–O nanoclusters in 14YWT. Together, these results demonstrate that SP-ICP-TOF-MS can resolve distinct particulate populations in complex, multicomponent steels at the femtogram mass scale, enabling particle-resolved insight into microstructure-driven phase separation and preparation-dependent particle generation.

Brubaker, Zach E. [Oak Ridge National Laboratory (↗

Synthesis and Characterization of Enhanced Conductivity Copper Composites [Abstract]

In this project, PNNL will extrude and characterize copper alloy wires embedded with graphene additives using the billets provided by NAECO via the shear assisted processing and extrusion (ShAPE TM ) technology. PNNL will measure the electrical properties of the extruded wires and also perform multimodal imaging to determine the microstructural features as required. These activities will be performed as part of a voucher service provided by PNNL for the CABLE Manufacturing Prize stewarded by DOE Advanced Manufacturing Office. This 6-month effort will be executed at PNNL with a budget of $100,000.00 (USD).

36 MATERIALS SCIENCE↗

XRD and SEM/EDS characterization of two quaternary fuel alloys (U-2.5Mo-2.5Ti-5.0Zr and U-1.5Mo-1.5Ti-7.0Zr in wt. %) for fast reactors

The current study focuses on characterization of two potential fuel alloys for sodium-cooled fast reactors: U-2.5Mo-2.5Ti-5.0Zr (U-MT5Z) and U-1.5Mo-1.5Ti-7.0Zr (U-MT7Z) in wt. %. As-cast alloys and annealed (600°C, 500h) alloys are studied by X-ray powder diffraction (XRD) for their bulk structures, and scanning electron microscopy / energy dispersive X-Ray spectroscopy (SEM/EDS) for their microstructures and phase constituents. For as-cast alloys, the XRD results show that U-MT5Z mainly contains γ, while U-MT7Z alloy contains a. In both alloys, there are three phases indicated by EDS, a U-rich phase, secondary phase, and Zr-rich phase. Further, the elemental compositions varied in different phases and in different alloys. After annealing, both alloys exhibit the structures of α-U and U 2 Ti according to XRD. The EDS results suggest there are five phases found in both alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

New class of tritium breeders for fusion applications: Metal-reinforced composite breeders

Commercial fusion reactors operating on a D-T fuel cycle will require a steady supply of tritium to maintain the burning plasma required for continuous power generation. Since tritium has a short half-life, there is negligible natural abundance which necessitates fusion reactors to produce their own source of tritium. Tritium is most easily produced by surrounding a fusion reactor core with lithium (Li), which reacts under the intense neutron flux leaving the reactor core to form tritium and helium. Due to the hazards and technical challenges associated with surrounding a fusion reactor core with many tons of molten Li, other Li-bearing tritium breeder materials have been pursued. Unfortunately, most of the liquid breeders historically examined are exceedingly corrosive to reactor structural materials while many solid breeders in the form of ceramics are forced to make tradeoffs between Li content and mechanical integrity. In this work, to break the historic limit between Li-density and mechanical integrity of traditional solid breeders, a new class of solid tritium breeders is developed: metal-reinforced composite (MERC) breeders. Specifically, the high Li-density of lithium oxide (Li 2 O) is exploited through the addition of a metal reinforcing phase, producing a composite breeder material exhibiting high splitting tensile strength and quasi-ductility with a Li-density greater than other leading solid breeder candidates, including lithium orthosilicate (Li 4 SiO 4 ) and lithium metatitanate (Li 2 TiO 3 ). Mechanical testing, microstructural characterization, and neutronic simulation results are presented and discussed in light of fusion reactor design considerations.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

The Efficacy of Replacing Metallic Cerium in Aluminum–Cerium Alloys with LREE Mischmetal

The ongoing development of aluminum–cerium alloys has produced materials exhibiting elevated temperature mechanical property retention, long term microstructural stability, and flexible processability compared to traditional aluminum alloys, accommodating the growing demand for high temperature aluminum alloys not requiring the use of high-cost elements like scandium. To date, reported Al–Ce alloy compositions contain large amounts of elemental cerium. Mischmetal (MM), a mixture of lanthanum, cerium, and other light rare earth elements (LREE) is less expensive and more available than pure cerium. The chemical similarity of the LREEs means there is possibility to use MM as the primary alloy addition, lowering alloy cost. This talk will report the effect of using MM instead of cerium in a 12 wt% binary alloy on mechanical properties, phase constituency, thermal stability, and load sharing. Results will show that MM can be substituted completely for cerium with a mostly positive impact on alloy performance.

Sims, Zachary↗

EDS-PhaSe: Phase Segmentation and Analysis from EDS Elemental Map Images Using Markers of Elemental Segregation

Scanning electron microscopy (SEM), combined with energy-dispersive spectroscopy (EDS), is an extensively used technique for in-depth microstructural analysis. Here, we present the EDS-Phase Segmentation (EDS-PhaSe) tool that enables phase segmentation and phase analysis using the EDS elemental map images. Importantly, it converts the EDS map images into estimated composition maps for calculating markers of selective elemental redistribution in the scanned area and creates a phase-segmented micrograph while providing approximate fraction and composition of each identified phase. EDS-PhaSe offers two unique advantages. Firstly, it enables the direct processing of EDS elemental map images without requiring any raw or proprietary data/software, thereby allowing the analysis of EDS results available in the published literature as images. Secondly, it enables segmentation and analysis of phases even when the phase contrast is missing in backscattered micrographs, assisting in correlating the XRD and SEM-EDS data as shown in this work for a AlCoCrFeNi high-entropy alloy.

36 MATERIALS SCIENCE↗

Internal Microstructure Dictates Interactions of Polymer-grafted Nanoparticles in Solution

Understanding the effects of polymer brush architecture on particle interactions in solution is requisite to enable the development of functional materials based on self-assembled polymer-grafted nanoparticles (GNPs). Static and dynamic light scattering of polystyrene-grafted silica particle solutions in toluene reveals that the pair interaction potential, inferred from the second virial coefficient, A 2 , is strongly affected by the grafting density, σ, and degree of polymerization, N, of tethered chains. In the limit of intermediate σ (~0.3 to 0.6 nm -2 ) and high N, A 2 is positive and increases with N. This confirms the good solvent conditions and can be qualitatively rationalized on the basis of a pair interaction potential derived for grafted (brush) particles. In contrast, for high σ > 0.6 nm -2 and low N, A 2 displays an unexpected reversal to negative values, thus indicating poor solvent conditions. These findings are rationalized by means of a simple analysis based on a coarse-grained brush potential, which balances the attractive core-core interactions and the excluded volume interactions imparted by the polymer grafts. The results suggest that the steric crowding of polymer ligands in dense GNP systems may fundamentally alter the interactions between brush particles in solution and highlight the crucial role of architecture (internal microstructure) on the behavior of hybrid materials. The effect of grafting density also illustrates the opportunity to tailor the physical properties of hybrid materials by altering geometry (or architecture) rather than a variation of the chemical composition.

36 MATERIALS SCIENCE↗

Phase evolution and amorphous stability upon solid-state reaction in superlattice like Ge–Sb–Te combinatorial thin-film

In this paper, the superlattice-like (SLL) Ge–Sb–Te combinatorial thin films were prepared by using a high-throughput ion beam sputtering system. The phase evolution and amorphous stability of such films undergoing heat treatment as a function of the coating sequence and modulation period were systematically studied. The composition structure diagram was constructed via an automated process of data obtained by high-throughput synchrotron micro-X-ray diffraction and lab-based micro-X-ray fluorescence. Furthermore, the element distribution and microstructure in the depth direction of the SLL thin films were characterized with time-of-flight secondary ion mass spectrometry and transmission electron microscopy, respectively. These studies demonstrated that the coating sequence has a significant effect on the element distribution in the as-deposited SLL thin films and the structure of the final product upon solid-state reaction. Reducing the modulation period of the SLL thin film improves the stability of the amorphous Ge–Sb–Te phase. This work lays a solid foundation for the rational design of SLL Ge–Sb–Te thin films to improve their performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Optimization of La 2 NiO 4+δ Electrolysis Cell Oxygen Electrode through Surfactant-Enabled LaCoO 3±δ Nanocatalyst Deposition

Lanthanum nickelate (LNO) has shown promise as a Cr-resistant air electrode material for SOECs but has suboptimal surface oxygen exchange properties. Nanocoating of the LNO surface with lanthanum cobaltite (LCO) was chosen to improve cell performance as a surface oxygen conductor. The work focused on the implementation of a two-step nano-LCO film deposition utilizing catechol molecules in a porous LNO electrode. The subgoals of the work were to maintain nanosized LCO particles/ grains to increase active surface area and to control the regularity/ homogeneity of the coating across the microstructure. To achieve these goals, a novel surfactant-enhanced liquid infiltration method was utilized, where nucleation sites were spread across the electrode structure to control the location and size of LCO particles. Various catechol surfactant compositions were evaluated for their ability to control the kinetics of nanoparticle deposition and the homogeneity of the coating. Chelated LCO was characterized by X-ray diffraction (XRD), which found a substantial improvement in LCO formation with surfactant addition and determined polymerized norepinephrine to be the best-performing surfactant, with 88.4% pure LCO formed at low temperature. X-ray photoelectron spectroscopy (XPS) confirmed LCO nanostructures formed by the two-step infiltration process, showing no impurities and a stable perovskite structure. Deposition kinetics were analyzed using atomic force microscopy (AFM), correlating infiltration times and solution molarity to nanoparticle size and distribution, the results of which were confirmed in symmetrical cell samples by scanning electron microscopy (SEM). Electrochemical impedance spectroscopy (EIS) testing demonstrated substantial improvements in polarization resistance, where the nanocoating reduced the resistance by ∼55% to 0.152 Ω·cm 2 at 700 °C and 0.039 Ω·cm 2 at 800 °C. Electrical conductivity relaxation (ECR) at this temperature confirmed an improved surface oxygen exchange coefficient of the LCO + LNO heterostructure predicted by the Bode data from EIS, alongside a reduction in activation energy by about 30%.

Deposition↗

Machine learning approaches for intentional materials engineering

In this article, the development of nanoporous metals and metallic composites through dealloying processes presents significant opportunities in materials engineering. However, designing multicomponent precursor alloys and establishing corresponding processing methods that yield predictable compositions and nanostructures remain a complex challenge. This article explores how machine learning (ML)-augmented computational and experimental methodologies can tackle these challenges by predicting precursor alloy compositions, final nanoporous structures, and mechanical properties, while integrating ML-enabled autonomous experimentation for material design and quantification. We highlight recent advancements in applying ML to nanostructured materials design via dealloying and discuss how techniques from other nanomaterial designs can be adapted for improved control over morphological and compositional outcomes in nanoporous and nanocomposite materials. Furthermore, we explore the role of ML in autonomous synchrotron x-ray experimentation, enabling real-time feedback between modeling and experimental setups. ML-driven approaches to microstructure characterization and mechanical property prediction are also examined, with a focus on modeling and advanced imaging techniques such as three-dimensional nanotomography. Finally, this article outlines future directions for ML-enhanced materials science, emphasizing the exploration of high-dimensional parameter spaces and the incorporation of materials kinetics into processing and property evaluation, ultimately advancing the design of nanoporous structures and materials science.

36 MATERIALS SCIENCE↗

Rapidly solidifying Pb-free Sn-Ag-Cu-Al or Sn-Cu-Al solder

A solder alloy includes Sn, optional Ag, Cu, and Al wherein the solder alloy composition together with the solder alloy superheat temperature and rapid cooling rate from the superheat temperature are controlled to provide a dispersion of fine hard Cu—Al intermetallic particles in an as-solidified solder alloy microstructure wherein the particles are retained even after multiple solder reflow cycles often used in modern electronic assembly procedures to provide a particle strengthening to the solder joint microstructure as well as exert a grain refining effect on the solder joint microstructure, providing a strong, impact- and thermal aging-resistant solder joint that has beneficial microstructural features and is substantially devoid of Ag3Sn blades.

36 MATERIALS SCIENCE↗

Development of Stable Solid Oxide Electrolysis Cells for Low-Cost Hydrogen Production

The project objective was to demonstrate a solid oxide cell-based steam electrolysis stack that exhibits robustness, reliability, endurance, hydrogen purity, and produces hydrogen at elevated pressure of 2 to 3 bar. Innovative materials and processing methods were evaluated to improve degradation characteristics. Performance improvement focused on nearly all layers involved in the cell and stack assembly. Primary attention was paid to zirconia-ceria interface resistance control via sintering optimization and decrease in degradation from the oxygen electrode by evaluating low strontium (Sr) or Sr-free composition for both the oxygen electrode and current collection layer. Stack robustness was addressed by validating redox tolerance of fuel electrode, confirming capability of cells to survive repeated thermal cycles, studying the effect of pressure on performance and degradation, evaluating the effect of contamination on fuel and oxygen electrode performance and degradation, and identifying mitigation strategies to improve performance. The characterization included evaluation of electrochemical performance and stability followed by microstructural analysis. At the cell level, performance and stability improvements were achieved by incorporating a Sr-free oxygen electrode and a denser oxygen electrode barrier layer. At the stack level, pressurized operation reduces demand on first stage compression, the redox tolerant fuel electrode mitigates risk from service interruptions, and improvements to interconnect coating alleviate chromium (Cr) contamination effects. The denser barrier layer was achieved by adding a sintering aid to the samaria-doped ceria (SDC) composition that reduced sintering temperature by 150 °C. The resulting density was on par with the baseline SDC barrier layer density and the lower sintering temperature resulted in less resistive phase formation during sintering. Button cell tests did not demonstrate a change in performance when exposed to silicon (Si) or manganese (Mn) impurities to the fuel electrode and Cr impurity to the oxygen electrode. More detailed study however is warranted. The project addressed SOEC performance and stability at the cell and stack levels through a systematic approach to known sources of degradation that were combined and tested in three stack tests using an electrolyte supported cell design to allow for evaluation of a variety of fuel and oxygen electrode compositions. STK-82 and STK-83 had identical compositions. STK-100 incorporated the best materials and processing variables developed under this and concurrent projects, and was tested at elevated pressure in steam electrolysis. • STK-82 recovered performance after redox and thermal cycling, demonstrating the robustness of the stack and seals. It exhibited stable performance in testing for 500 hours in SOEC mode, followed by 300 hours of cycling between SOEC and SOFC tests. Degradation during SOEC operation was 1.8 %/ 1,000 hours. • STK-83 generated hydrogen at >80% steam conversion, and oxygen above 98.5 % purity during pressurized operation. Both hydrogen and oxygen were generated at 3 barg pressure without the use of a pressure vessel. In addition to balanced pressure, electrolysis operation at 1 bar differential pressure across anode and cathode was also demonstrated to substantial the robustness of the cell and seal. • STK-100 measured at initial ambient pressure conditions showed an area specific resistance of 1.1 ohm-cm 2 , and STK-83 had 1.3 ohm-cm 2 .

08 HYDROGEN↗

Materials Challenges and Opportunities for Energy Generation, Conversion, Delivery, and Storage (Applied Energy Tri-Laboratory Consortium Workshop Report)

This report documents the outcomes of the Tri-Laboratory Materials Workshop that was held July 31 and August 1, 2019 to begin addressing the needs, opportunities, and challenges associated with the development, fabrication, and testing of the needed materials and components for integrated hybrid energy systems (i.e., incorporating nuclear, fossil, and renewables for electric and thermal applications). This was accomplished by assembling the research program leads and principal investigators at Idaho National Laboratory (INL), National Energy Technology Laboratory (NETL), and National Renewable Energy Laboratory (NREL), who support the research and development of new technology and system integration. The team then identified and prioritized key materials development needs. This effort was intended to enhance communications and synergy among the Tri-Lab partners. Advanced functional and structural materials are central to transformative energy technologies for energy generation, conversion, delivery, and storage. With that in mind, the workshop focused on identifying and assessing the foundational materials research needs at both the basic and applied levels. Materials challenges include the ability to withstand harsh environments, such as high temperatures and pressures, corrosion, oxidation, or irradiation while maintaining flexible mission profiles and long service lifespans. Advanced energy system material challenges and needs range from materials for the capture, upgrading/concentration, storage, and delivery of low-grade heat to materials for high temperature environments that involve liquid metals, molten salt, and very high temperature gas heat delivery and storage systems. Material improvements are needed for hybrid energy systems due to accelerated corrosion and stress-fatigue failure of materials and equipment, which results from increased frequency and amplitude of thermal, mechanical, and electrical cycling of systems components. Multifunctional materials are needed for high temperature solid-oxide fuel cells, advanced electrochemical reactors, and in-process separation. Relative to materials manufacturing, application of advanced additive and subtractive methods need to be understood to develop both thin-layer homogenous materials and materials of graded composition. Materials modeling and machine learning will be critical to accelerate the design and production of power electronics, and nuclear reactor materials and fuel, as well as to gain an understanding of beneficial materials phenomena or deleterious microstructure evolution. There is also a need for standardized models, computational structures, data reporting protocols and modeling tools across the three laboratories. This would allow consistent results, analysis, and data sharing. Combining computational capabilities between the three laboratories (e.g., hardware, software) would greatly increase computational capabilities and throughput. The workshop identified the need for laboratories to anticipate and address problems that will occur during scale-up. Laboratory work must connect with industry to ensure that research focuses on processes that are scalable and marketable. Industry input and perspective are essential to guide laboratory research to meet these requirements and deploy new technology in industrial demonstrations. Another aspect of scale-up is the integration of multiple systems since new challenges often arise at the subsystem interfaces. Establishing a scale-up manufacturing demonstration/pilot plant, potentially as an industrial user facility, would be beneficial to the laboratories and industry. That modular scale-up manufacturing demonstration/pilot plant would allow researchers to find and resolve interface problems that cannot be identified by focusing only on individual parts. Communication exchanges among the organizers, attendees, and workshop survey responses indicate that the workshop was successful in achieving its goal to identify key technology gaps and research needs. Strong positive feedback was received on the sharing of ideas, capabilities, talent, and passion to move forward on the materials-related action items.

36 MATERIALS SCIENCE↗

Phase-inversion polymer composite material, fabricating methods and applications of same

A composite film usable as a separator of an electrochemical device includes hBN nanosheets and at least one polymer. The hBN nanosheets are uniformly dispersed within a matrix of said least one polymer to achieve a highly porous microstructure. Said at least one polymer comprises one or more electrically insulating and electrochemically inert polymers.

Hersam, Mark C.↗

The effect of ink ball milling time on interparticle interactions and ink microstructure and their influence on crack formation in rod-coated catalyst layers

This work investigates the influence of ballmilling (sometimes also referred to as jar roller milling) time on cathode catalyst layer (CL) inks and electrode properties using formulations and coating methods relevant for industrial manufacturing. Four CL inks with the same composition were milled for 24, 48, 72, or 96 h. Rheological investigation of these inks showed a reduction of elastic moduli and steady-shear viscosity with continuous ink milling, which is correlated to a decrease in particle-particle interactions as well as formation of smaller agglomerates. Optical microscopy (OM) analysis of the fabricated electrodes revealed a trend in surface crack formation; formulations milled for 24 h contained the lowest average surface crack area percentages of 0.370% at heavy-duty loadings of ~0.300 mg Pt cm -2 , compared to 2.418% for the ink milled for 96 h. Further characterization of the CL through transmission electron microscopy (TEM) imaging showed a decrease in the mean agglomerate and pore size with milling time. Furthermore, these smaller electrode features were consistent with reduced fracture resistance and, hence, development of larger stresses during drying. Our results highlight the need to consider ink processing as an important component in defect-free CL manufacturing.

30 DIRECT ENERGY CONVERSION↗