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Wong-Sam, Andres↗
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Mechanical and chemical properties of PVD and cold spray Cr-coatings on Zircaloy-4
In this paper, accident-tolerant fuel (ATF) cladding materials aim to improve fuel reliability and safety during accident scenarios in water-cooled reactors. These ATF cladding should also perform comparable or better than the current zirconium alloy cladding under reactor normal operating conditions. Surface-modified Zircaloy-4 was produced by depositing a protective coating of chromium by two different coating techniques, Physical Vapor Deposition (PVD) and Cold Spray (CS). The coating thickness, structure, composition, and mechanical properties of the coated Zircaloy were assessed with advanced materials characterization techniques. Results showed a strengthening effect of the Cr-coating, along with ~83% higher hardness compared to that of the Zircaloy-4 substrate. Surface topography and surface chemistry of the Cr-coated Zircaloy-4 were assessed with contact profilometry, atomic force microscopy, contact angle goniometry, and X-ray photoelectron spectroscopy. Deposited Cr-coating significantly improved surface wettability compared to the substrate Zircaloy-4. The formation of surface oxides on the coatings by prolonged exposure to ambient air showed a further increase in the hydrophobic behavior. Surface parameters and surface chemistry after flow boiling critical heat flux tests, conducted at atmospheric pressure, evidenced a slight increase in surface roughness with notable changes in wettability associated with the formation of surface oxides.
36 MATERIALS SCIENCE↗
Supramolecular design principles in pseudohalides for high-performance perovskite solar mini modules
In this work, we reveal the role of non-covalent interactions, which are known to play important roles in supramolecular phenomena, in achieving efficient perovskite surface and grain boundary passivation. By using a series of pseudohalides, we find that trifluoroacetate (TFA - ) provides the strongest binding to iodide vacancies by means of non-covalent hydrogen bonding and dispersion interactions. By exploiting additional non-covalent dispersion and hydrophobic interactions in aromatic 3,3-diphenylpropylammonium (DPA + ), we present a dual-ion passivation strategy that not only minimizes the non-radiative recombination center and local chemical inhomogeneities but also induces preferentially oriented growth of α-FAPbI 3 lattice. Further, this leads to an outstanding power conversion efficiency (PCE) of 25.63% with an exceptional open-circuit voltage of 1.191 V in a perovskite solar cell with a small area, while perovskite solar mini modules with aperture areas of 25 and 64cm 2 achieved PCE of 22.47% (quasi-steady-state [QSS]-certified 20.50%) and 20.88%, respectively, with outstanding stability under high-humidity conditions.
14 SOLAR ENERGY↗
Copper(I) photosensitizer-silica nanoparticle assembly towards enhanced aqueous photoluminescence
Harnessing the luminescence potential of Cu(I) complexes in aqueous media is typically hindered by their poor photostability and altered properties. Here, we report the synthesis, engineering and morphological characterization of a hydrophobic homoleptic copper(I) complex entrapped into silica nanoparticles, Cu-I@SiO 2 (where “Cu-I” designates [Cu(2,9-diiodo-1,10-phenanthroline) 2 ] + ), as a promising stabilisation strategy towards water-compatible, Cu(I) complex-based luminescence. The polyether chain-decorated nano-objects are spherical with an average diameter of ca. 10.8 ± 1.9 nm. Upon dispersion in water, clear solution-like suspensions were obtained. Significantly, the aqueous suspensions photo-luminesce (Φ em = 5×10 -4 ) upon excitation through the Metal-to-Ligand Charge-Transfer transition (MLCT) of the embedded copper(I) complexes. In contrast, the corresponding silica-free molecular complex dissolved in an aqueous environment revealed fully quenched emission. Finally, the use of Cu-I@SiO 2 suspensions as luminescent probes is reported, first by assessing their potential use as electrochemiluminescent probes, and second by monitoring the photoluminescence from Cu-I@SiO 2 in the presence of whole blood.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Non-planar platinum group metal-free fuel cell cathodes for enhanced oxygen transport and water rejection
Proton exchange membrane fuel cells (PEMFC) with cathodes using platinum group metal-free (PGM-free) catalysts could significantly reduce costs, but the lower volumetric oxygen reduction reaction (ORR) activity requires thick electrodes that suffer from liquid water flooding and increased oxygen transport resistance. To address these challenges, we developed a 3D gas diffusion electrode (GDE) architecture to enhance liquid water removal through the diffusion media and reduce cathode saturation. The cathode features a uniform catalyst layer adjacent to the membrane for high ORR activity and then pillars of the hydrophilic catalyst layer that pass through the microporous layer (MPL), providing a low capillary pressure barrier pathway to the carbon fiber paper layer and channel. The non-planar cathode also increases the interfacial area between the catalyst layer and hydrophobic MPL for a greater fraction of the cathode with high O 2 concentration. Our studies included parametric experimental study of the pillar density to identify the optimum pitch between pillars. Our measurements show significant improvements in the mass transport region of the polarization curve with 3D structured electrodes leading to an 8% increase in maximum current density, 19% increase in maximum power density, and 16% increase in current density at 0.67 V with air.
25 ENERGY STORAGE↗
Design and operating principles for high-performing anion exchange membrane water electrolyzers
Anion-exchange-membrane water electrolyzers (AEMWEs) provide a promising pathway to utilize low-carbon renewable electricity to produce clean hydrogen at high efficiency and purity, while maintaining low system costs compared to incumbent technologies. Though significant progress has been made in developing membranes and catalysts, AEMWEs still require better performance and durability to realize widespread deployment. Here, we overcome these challenges by decoupling anode and cathode polarization behavior via integration of a reference electrode in the membrane-electrode assembly. This measurement identified that the mass-transport losses dominate the cathode overpotential if feeding with electrolytes, while kinetic losses dominate the anode overpotential. These losses are mitigated by varying electrode properties and operating strategies, where a more hydrophobic, optimal loaded cathode, a high porosity anode, and operating with the cathode dry exhibited the best performance. These findings eventually enabled achieving a high-performing and durable complete PGM-free AEMWE operating at 1.5 Acm –2 for over 500h with negligible degradation, demonstrating significant progress for AEMWEs.
25 ENERGY STORAGE↗
Highly durable platinum group metal-free catalyst fiber cathode MEAs for proton exchange membrane fuel cells
For this work, Fe-based platinum group metal (PGM)-free catalysts were incorporated into electrospun fiber mat or powder cathode membrane-electrode-assemblies (MEAs) with a Nafion 211 membrane and a Pt/C powder anode. Fabrication and characterization tests were performed on MEAs with: (1) a conventional powder cathode with a neat Nafion binder, (2) a fiber mat cathode with a Nafion/polyethylene oxide (PEO) binder, where PEO was extracted before MEA testing, (3) a powder cathode with a blended binder of Nafion and polyvinylidene fluoride (PVDF), and (4) a series of fiber mat cathodes with different Nafion/PVDF binder weight ratios. Cathode degradation occurred, with a loss in power output, in MEAs with a neat Nafion powder cathode or with a Nafion fiber cathode. In contrast, little or no power loss was observed for powder or fiber cathodes when the binder was a blend of Nafion and PVDF. The presence of hydrophobic PVDF drove water and electrogenerated peroxide out of the cathode, away from catalyst particles, which improved cathode durability, but PVDF also decreased the binder conductivity and slowed oxygen reduction kinetics, resulting in lower power densities. A 75:25 w:w Nafion:PVDF fiber cathode MEA was the best compromise for maximizing power and minimizing catalyst degradation. For such a cathode, with a PGM-free cathode catalyst loading of 3.0 mg cm –2 , a power density of 88 mW cm –2 at 0.5 V, 80 °C, and 200 kPa abs pressure was maintained for 80 h of continuous operation.
25 ENERGY STORAGE↗
Influence of solvents on electrochemical stability window of ionic liquid solutions
The electrochemical stability window (ESW) defines the voltage range within which an electrolyte remains stable against oxidation and reduction, serving as a key descriptor for ionic liquid (IL)-based systems. The ESWs of 15 ILs with diverse cation-anion combinations were systematically investigated, both in their neat forms and as binary mixtures with three representative solvents, i.e., propylene carbonate (PC), ethylene glycol (EG), and tetrahydrofuran (THF). Cyclic voltammetry on a glassy carbon electrode determined anodic and cathodic stability limits, revealing that ESW protection in IL-solvent mixtures strongly depends on solvent polarity, proticity, and IL compatibility. PC, with a high dielectric constant and aprotic character, broadened anodic limits and moderately stabilized cathodic limits. THF maintained compact interfacial structure, offering additional cathodic protection, whereas EG, being protic, reduced ESWs via proton-coupled electron transfer and hydrogen evolution. The solvent protection trend followed by PC > THF > EG, with bulky, hydrophobic cations ([HMIM] + , [BMPYRR] + ) and weakly coordinating anions ([NTF 2 ] - , [DCA] - , [DEP] - ) showing the highest ESW protection for 50 mol% IL in these solvents. Among the neat ILs, [EMIM][DEP], [HMIM][PF 6 ], and [BMPYRR][DCA] showed wide ESWs of ∼5.5 V. These results provide valuable insight into solvent-modulated electrochemical stability, enabling rational design of IL-based electrolytes for energy storage and electrosynthesis.
25 ENERGY STORAGE↗
CoRE MOF DB: A curated experimental metal-organic framework database with machine-learned properties for integrated material-process screening
Here, we present an updated version of the Computation-Ready, Experimental (CoRE) Metal-Organic Framework (MOF) database, which includes a curated set of computation-ready MOF crystal structures designed for high-throughput computational materials discovery. Data collection and curation procedures were improved from the previous version to enable more frequent updates in the future. Machine-learning-predicted properties, such as stability metrics and heat capacities, are included in the dataset to streamline screening activities. An updated version of MOFid was developed to provide detailed information on metal nodes, organic linkers, and topologies of an MOF structure. DDEC6 partial atomic charges of MOFs were assigned based on a machine-learning model. Gibbs ensemble Monte Carlo simulations were used to classify the hydrophobicity of MOFs. The finalized dataset was subsequently used to perform integrated material-process screening for various carbon-capture conditions using high-fidelity temperature-swing adsorption (TSA) simulations. Our workflow identified multiple MOF candidates that are predicted to outperform CALF-20 for these applications.
CoRE MOF database↗
Surface engineering of polymeric membranes with metal oxides for improved fouling resistance and superior oil-water separation
Rapid industrial growth has increased the need for efficient membranes to separate oil-water emulsions. Polyvinylidene fluoride (PVDF) membranes, although widely used due to their chemical inertness and favorable mechanical properties, suffer from fouling due to their intrinsic hydrophobicity. Modifying these membranes after fabrication offers a practical solution as it easily fits into existing large-scale manufacturing processes. Atomic layer deposition (ALD), an atomically-precise vapor phase surface modification technique, can create ultrathin metal oxide layers that greatly improve membrane hydrophilicity without significantly affecting the original pore size. However, PVDF's lack of reactive chemical moieties makes ALD challenging. Here, in this study, we present a simple alkali treatment that greatly enhances ALD nucleation and growth on PVDF membranes. This treatment imparts exceptional oil-water emulsion separation capabilities and antifouling behavior in PVDF membranes after just a few ALD cycles, surpassing the performance of PVDF membranes coated with hundreds of ALD cycles. This dramatic reduction in the number of ALD cycles required could enable cost-effective modification of commercial PVDF membranes at scale using spatial, roll-to-roll ALD. These modified membranes outperform reported modified PVDF membranes, with >99 % permeance recovery and <1 % irreversible loss of permeance and >98 % oil rejection from oil-water emulsions over 100 h continuous operation, making them promising for advanced water purification technologies.
Atomic layer deposition↗
Synthesis and characterization of magnetic ionic liquids containing multiple paramagnetic lanthanide and transition metal centers and functionalized diglycolamide ligands
Magnetic ionic liquids (MILs) containing paramagnetic centers have gained widespread recognition as sustainable solvents due to their ability to respond to an external magnetic field. The physico-chemical properties of MILs are dependent on the choice of anion/cation ligands and metal centers; the search for highly tunable ligands and precursors that can confer favorable characteristics, such as low viscosity, is ongoing. Diglycolamides employed as cationic ligands have been previously shown to form hydrophobic MILs that can simultaneously incorporate multiple lanthanide metal centers in both the anion/cation. Despite their enhanced magnetic susceptibility, the effect of diglycolamide chemical structure modifications on the physico-chemical properties of MILs has not been thoroughly studied. Additionally, the possibility of forming diglycolamide-based MILs with popularly employed transition metals has not been investigated and combinations that can simultaneously embed two different types of metal centers in both the anion/cation have not been explored. In this study, thirty (30) MILs comprised of lanthanide and transition metals were synthesized by examining their chelation to both straight-chained and branched diglycolamides. Here, transition metal-based MILs were found to possess high thermal stabilities up to 235 °C compared to 192 °C for those comprised of lanthanides. While MILs comprised of rare-earth metal centers exhibited the lowest viscosities, substituting lanthanides with transition metals in just the anion or cation resulted in enhanced thermal stability and reduced viscosity. The effective magnetic moment for these MILs varied between 4.71 and 21.08 µ B and was much higher compared to all previous classes of MILs prepared using the same metals. Results from this study explore all possible modifications that can be made to these MILs in an effort to demonstrate their structural tunability, which is often highly desirable in various applications, including organic synthesis and chemical separations.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
CO 2 adsorption mechanisms at the ZIF-8 interface in a Type 3 porous liquid
Porous liquids (PLs) are an attractive material for gas separation and carbon sequestration due to their permanent internal porosity and high adsorption capacity. PLs that contain zeolitic imidazole frameworks (ZIFs), such as ZIF-8, form PLs through exclusion of aqueous solvents from the framework pore due to its hydrophobicity. The gas adsorption sites in ZIF-8 based PLs are historically unknown; gas molecules could be captured in the ZIF-8 pore or adsorb at the ZIF-8 interface. To address this question, ab initio molecular dynamics was used to predict CO 2 binding sites in a PL composed of a ZIF-8 particle solvated in a water, ethylene glycol, and 2-methylimidazole solvent system. Further, the results show that CO 2 energetically prefers to reside inside the ZIF-8 pore aperture due to strong van der Waals interactions with the terminal imidazoles. However, the CO 2 binding site can be blocked by larger solvent molecules that have greater adsorption interactions. CO 2 molecules were unable to diffuse into the ZIF-8 pore, with CO 2 adsorption occurring due to binding with the ZIF-8 surface. Therefore, future design of ZIF-based PLs for enhanced CO 2 adsorption should be based on the strength of gas binding at the solvated particle surface.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Chemometric modeling of power conversion efficiency of organic dyes in dye sensitized solar cells for the future renewable energy
The present study reports chemometric modeling of power conversion efficiency (PCE) of dye sensitized solar cells (DSSCs) using the biggest available data set till date which comprises around 1200 dyes covering 7 chemical classes. To extract the best structural features required for higher PCE, we have developed multiple partial least squares (PLS) quantitative structure-property relationship (QSPR) models for the Triphenylamine, Phenothiazine, Indoline, Porphyrin, Coumarin, Carbazole and Diphenylamine chemical classes using descriptors derived from the best subset selection method followed by selection of best five models in each dataset based on the Mean Absolute Error (MAE) values. The models were validated both internally and externally followed by the consensus predictions employing “Intelligent Consensus Predictor” tool to examine whether the quality of predictions can be improved with the “intelligent” selection of multiple PLS models. The quality of predictions for the respective external sets showed that the consensus models (CM) are better than the individual models (IM) in most of the cases. From the insights of the developed models, we concluded that attributes like a packed structure toward higher conductivity of electrons, auxiliary donor fragment of aromatic tertiary amines, number of thiophenes inducing the bathochromic shift and augmenting the absorption, presence of additional electron donors, enhancement of electron-donating abilities, number of non-aromatic conjugated C(sp 2 ) which helps as conjugation extension units to broaden the absorption and highly conjugated $π$-systems exert positive contributions to the PCE. On the contrary, features negatively contributing to PCE are the followings: fragments which lower the tendency of localized $π–π*$ transition, fragments related to larger volume and surface area of dyes along with hydrophobicity resulting in poor adhesion, fragment RC = N causing dye hydrolysis, steric hindrance for π electronic mobility, fragments enhancing polarity, etc. Finally, the identified features from the best QSPR model of the coumarin dataset was employed in designing of ten more efficient coumarin dyes (predicted %PCE ranging from 8.93 to 10.62) than the existing ones.
14 SOLAR ENERGY↗
Versatile coating with multifunctional performance for solar steam generation
In this work, a new kind of material, composite complex coating (CCC), with multifunctional performance has been developed for solar steam generation. The CCC has many advantages: (a) Scalability. The fabrication process is facile and mild; it can be realized in aqueous solution at room temperature, without high pressure, toxic organic solvents, or complex equipment. (b) Cost-effectiveness. The reagents used for preparation of CCC are low-cost and readily available. (c) Universality and stability. CCC firmly adheres on surfaces of various substrates with diverse shapes (cotton, filter paper, wood, polyurethane sponge, and even chemically inert and highly hydrophobic polyvinylidene fluoride membranes), and can withstand rinsing treatment (3000 r/min for 96 h), cyclic frost-thaw test (-18 °C ⇌ 30 °C, 90 times), and both high and low pH environments. In addition, many other reported coatings, such as carbon black, fail under similar process strain. (d) Anti-crude oil-fouling property. The CCC possesses stable superhydrophilicity and underwater superoleophobicity, which collectively endow substrates with the ability to resist fouling by oils. (e) Broad and strong light absorption. CCC can transform various substrates with diverse shapes into black materials with broadband light absorption due to its d-d transitions and rough surface. Together, these properties of CCC enable substrates with nearly any structural design to be easily transformed into photothermal materials for efficient solar steam generation. Furthermore, as a proof of concept, poplar wood is treated with CCC, achieving a water evaporation rate of ~1.8 kg m-2 h-1 (one sun), which is a record among wood-based photothermal materials.
14 SOLAR ENERGY↗
Multicolored microwave absorbers with dynamic frequency modulation
Microwave-absorbing materials are extensively used in intelligent electronic devices and stealth technologies where the ability to dynamically adjust microwave-absorbing capacity in response to specific requirements is vitally important. Herein, we report a new approach for constructing dynamically tunable microwave absorbers with ultrawide tunable frequency ranges that are simultaneously endowed with vibrant structural colors. Here, the methodology produces structural colors and adjusts absorption properties by constructing ZnO coatings with precisely adjustable thicknesses on a polypyrrole/melamine foam (PPy/MF) surface by atomic layer deposition (ALD) in conjunction with a pressure-driven strategy that regulates the compression ratio. The electrical conductivity, electromagnetic parameters, thickness, and pore size of the ZnO-coated PPy/MF (ZnO/PPy/MF) are effectively adjusted, and simply applying external pressure widens the tunable frequency range and the effective absorption bandwidth. As a result, the effective absorption frequency of ZnO/PPy/MF is dynamically adjustable from the S band to the Ku band, thereby covering 94.3% of the entire microwave spectrum. Moreover, the brilliant and uniform structural colors of ZnO/PPy/MF, which span various color categories, are precisely regulated by tuning the thickness of the ZnO coating by adjusting the number of ALD cycles. ZnO/PPy/MF is strongly hydrophobic, which endows it with remarkable self-cleaning properties. Therefore, ZnO/PPy/MF provides a conceptually novel platform for the development of next-generation smart microwave-absorbing materials due to its integrated dynamic frequency-regulating ability, brilliant structural coloration, and self-cleaning features.
36 MATERIALS SCIENCE↗
Pool boiling critical heat flux studies of accident tolerant fuel cladding materials
Pool boiling experiments have been performed at atmospheric pressure on potential accident tolerant fuel (ATF) cladding materials (Zirlo®, Cr coated Zirlo®, FeCrAl coated Zirlo®, and monolithic SiC) to evaluate the Critical Heat Flux (CHF) points. Corrosion resistant coatings of Cr and FeCrAl alloy were deposited on flat Zirlo® samples using cold spray technology. The as-prepared samples after uniform surface polishing were subjected to autoclave tests at 360 °C water and 18.6 MPa for 360 h to simulate prototypic corrosion of the ATF cladding materials in LWR normal operation. Surface characteristics potentially influencing CHF such as surface morphology, roughness, static contact angle, and surface chemistry were characterized using a suite of characterization methods including scanning electron microscopy, 3D optical profilometry, optical contact angle measurements, and x-ray photoelectron spectroscopy (XPS). Thermo-physical properties of the samples such as density, thermal conductivity, and heat capacity were measured by differential scanning calorimetry and laser flash thermal diffusivity measurement. FeCrAl coatings showed CHF values comparable to bare Zirlo® samples, while slightly lower CHF values were observed for Cr coated samples and bulk SiC flats (produced by chemical vapor deposition, CVD). As-deposited Cr coatings showed 67% higher CHF than the as-polished Cr coatings due to its higher surface roughness level. The autoclave testing for the prepared samples generally increased the CHF except for the surface polished Cr coatings. Similar CHF values of bare Zirlo®, FeCrAl coating, and CVD SiC samples were observed after autoclave test but there were negligible change CHF of Cr coatings. XPS studies indicated that the formation or deposition of a few monolayers of hydrophobic carbonaceous species on surface can affect CHF values. The trends in CHF data are discussed in terms of evolution of the surface characteristics of the ATF materials.
73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
Experimental investigations of Critical Heat Flux re-occurrence on post-CHF surfaces
Under the extreme environments of light water reactors, the cladding materials demonstrate evolutionary transformations in terms of material compositions, surface morphologies, and thermal-physical properties. This study investigates how the temperature overshooting of Critical Heat Flux (CHF) affects the re-occurrence of CHF on the post-CHF surfaces. Experimental results reveal that the CHF difference between as-received and post-CHF surfaces can be significant, which depends on materials. CHF is enhanced on post-CHF Stainless Steel (SS 316) specimens while it deteriorates on post-CHF Inconel-600 specimens. In comparison with the as-received surfaces, the post-CHF surface of SS 316 is more hydrophobic, while Inconel 600 is more hydrophilic. The scanning electron microscope micrographs of post-CHF surfaces show that surface morphologies that are structured by oxide crystals are formed on SS 316 samples but not on Inconel 600 samples. The physical rationale behind the CHF difference could be boiling heat transfer conjugated with thermal-physical proprieties of investigated surface materials and surface morphologies features. In conclusion, the results imply that it is indispensable to bookkeep the evolutionary changes of cladding surface materials, especially for cladding candidates of Accident Tolerant Fuel since operation histories can leave footprints on cladding surfaces, thus resulting in CHF re-occurrence differences.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Hairy nanoparticles by atom transfer radical polymerization in miniemulsion
Polymer nanoparticles with various architectures and functionalities are promising materials in numerous fields. Miniemulsion polymerization is one of the suitable pathways to prepare polymer nanoparticles since each droplet could act as a “nanoreactor”. A “smart” atom transfer radical polymerization (ATRP) catalytic system comprising Cu-TPMA/DS – (TPMA = tris(2-pyridylmethyl)amine, DS – = dodecyl sulfate anion) ion pair catalyst was efficiently applied in miniemulsion ATRP at low catalyst concentrations. Herein, hairy nanoparticles consisting of hydrophobic poly(n-butyl methacrylate) (P(BMA/EGDMA), EGDMA = ethylene glycol dimethacrylate) network “core” and hydrophilic oligo(ethylene oxide) methyl ether methacrylate (OEOMA) chains as “hair” were prepared by miniemulsion ATRP and a successive chain extension by aqueous ATRP from the particle surface. The addition of an inimer, 2-(α-bromoisobutyryloxy)ethyl methacrylate (HEMA-iBBr) to the P(BMA/EGDMA) network introduced more ATRP initiation sites for ATRP of OEOMA, enabling adjustment of the particle size from >400 nm to <150 nm. The miniemulsion system remained stable after the one pot synthesis of P(BMA/EGDMA)-g-POEOMA and P(BMA/EGDMA/HEMA-iBBr)-g-POEOMA, and the resulting polymer nanoparticles were re-dispersed in water for further modification. A zwitterionic monomer, [2-(methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium hydroxide (SBMA), was grafted from P(BMA/EGDMA/HEMA-iBBr)-g-POEOMA. The resulting hairy nanoparticles provide an avenue for the design and preparation of novel nanostructured materials.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗