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At least 325 records · Page 18
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Carbonylative Co- and Terpolymerizations of 10-Undecen-1-ol: A Route to Polyketoesters with Tunable Compositions

A strategy to synthesize branched polyketoesters from the carbonylative polymerization of bifunctional α,ω-alkenols such as 10-undecen-1-ol is presented. This strategy hinges on the competitive application of two related catalytic manifolds, alternating alkene/CO copolymerization, and alkene hydroesterification, which share a common metal acyl intermediate. Small molecule model studies of cationic Pd-catalyzed alkene carbonylation in the presence of alcohols demonstrate that the relative rates of ketone formation (through alternating alkene/CO insertion) and ester formation (through metal acyl alcoholysis) can be tuned across a wide range through judicious bis(phosphine) ligand design. Carbonylative polymerization of 10-undecen-1-ol with a (dppp(3,5-CF 3 ) 4 )Pd(OTs) 2 catalyst (dppp(3,5-CF 3 ) 4 = 1,3-bis[bis[3,5-bis(trifluoromethyl)phenyl]-phosphino]propane) led to the formation of high molecular weight polyketoesters with intermediate dispersity (M n > 20,000 g/mol, D- = 2.6) and a ketone/ester microstructure ratio of approximately 1:2. In these polymerization reactions, deploying electron-deficient bis(phosphines) to suppress deleterious alkene isomerization was the key to accessing the high molecular weight polymer. Further, terpolymerization reactions of 1-hexene/10-undecen-1-ol/CO or 1-fluoro-10-undecene/10-undecen-1-ol/CO by (dppp(3,5-CF 3 ) 4 )Pd(OTs) 2 were also successful. Furthermore, this proof of concept polymerization unlocks access to tunable polymer microstructures without extensive postpolymerization treatment.

10-undecen-1-ol↗
DOE OSTI2025

Controlling Ligand Excimer Formation with Dipole Changes in Emissive Rare-Earth/Phosphonic Acid Complexes

The interactions between substituted arylvinyl phosphonic acid (AVPA) ligands within a Eu-AVPA complex are shown to influence the outcomes of excited state evolution after photoexcitation. Compared with unfunctionalized AVPAs, pairs of ligands functionalized with CF 3 in the para position preassociate in the ground state of complexes with Eu 3+ according to calculated geometry optimizations. The CF 3 -substituted AVPA complexes show evidence of red-shifted optical absorption and undergo more efficient excimer formation, as revealed by transient absorption spectroscopy. We rationalize this behavior through simulations of excited-state geometry optimizations that reveal evolution toward interligand phenyl-phenyl planarity for specific excited states. Emission from complexed Eu 3+ after energy transfer from the ligand is found to be weaker with CF 3 substitution, which we hypothesize is due to intracomplex, interligand aggregates with excimer-promoting geometries. These observations point to the need to consider ground-state geometries as well as dynamic excited-state processes to understand the flow of energy in rare earth coordination complexes.

09 BIOMASS FUELS↗
DOE OSTI2021

Expanding the Ambient-Pressure Phase Space of CaFe 2 O 4 -Type Sodium Postspinel Host–Guest Compounds

CaFe 2 O 4 -type sodium postspinels (Na-CFs), with Na + occupying tunnel sites, are of interest as prospective battery electrodes. While many compounds of this structure type require high-pressure synthesis, several compounds are known to form at ambient pressure. Here we report a large expansion of the known Na-CF phase space at ambient pressure, having successfully synthesized NaCrTiO 4 , NaRhTiO 4 , NaCrSnO 4 , NaInSnO 4 , NaMg 0.5 Ti 1.5 O 4 , NaFe 0.5 Ti 1.5 O 4 , NaMg 0.5 Sn 1.5 O 4 , NaMn 0.5 Sn 1.5 O 4 , NaFe 0.5 Sn 1.5 O 4 , NaCo 0.5 Sn 1.5 O 4 , NaNi 0.5 Sn 1.5 O 4 , NaCu 0.5 Sn 1.5 O 4 , NaZn 0.5 Sn 1.5 O 4 , NaCd 0.5 Sn 1.5 O 4 , NaSc 1.5 Sb 0.5 O 4 , Na 1.16 In 1.18 Sb 0.66 O 4 , and several solid solutions. In contrast to earlier reports, even cations that are strongly Jahn–Teller active (e.g., Mn 3+ and Cu 2+ ) can form Na-CFs at ambient pressure when combined with Sn 4+ rather than with the smaller Ti 4+ . Order and disorder are probed at the average and local length-scales with synchrotron powder X-ray diffraction and solid-state NMR spectroscopy. Strong ordering of framework cations between the two framework sites is not observed, except in the case of Na 1.16 In 1.18 Sb 0.66 O 4 . This compound is the first example of an Na-CF that contains Na + in both the tunnel and framework sites, reminiscent of Li-rich spinels. Trends in the thermodynamic stability of the new compounds are explained on the basis of crystal-chemistry and density functional theory (DFT). Further DFT calculations examine the relative stability of the CF versus spinel structures at various degrees of sodium extraction in the context of electrochemical battery reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

PCET-Based Ligand Limits Charge Recombination with an Ir(III) Photoredox Catalyst

Upon photoinitiated electron transfer, charge recombination limits the quantum yield of photoredox reactions for which the rates for the forward reaction and back electron transfer are competitive. Taking inspiration from a proton-coupled electron transfer (PCET) process in Photosystem II, here a benzimidazole-phenol (BIP) has been covalently attached to the 2,2'-bipyridyl ligand of [Ir(dF(CF 3 )ppy) 2 (bpy)][PF 6 ] (dF(CF 3 )ppy = 2-(2,4-difluorophenyl)-5-(trifluoromethyl)pyridine; bpy = 2,2'-bipyridyl). Excitation of the [Ir(dF(CF 3 )ppy) 2 (BIP-bpy)][PF 6 ] photocatalyst results in intramolecular PCET to form a charge-separated state with oxidized BIP. Subsequent reduction of methyl viologen dication (MV 2+ ), a substrate surrogate, by the reducing moiety of the charge separated species demonstrates that the inclusion of BIP significantly slows the charge recombination rate. The effect of ~24-fold slower charge recombination in a photocatalytic phthalimide ester reduction resulted in a greater than 2-fold increase in reaction quantum efficiency.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2025

Proton-Catalyzed Interconversion of Tungsten(VI) Imido Isopropylidene and Propylene Complexes

Additions of two equivalents of (CF 3 ) 3 COH (R F9 OH) or (CF 3 ) 2 MeCOH (R F6 OH) to W(NAr) 2 R 2 complexes (Ar = 2,6-diisopropylphenyl, R = n-propyl or i-propyl) offer the opportunity to synthesize propylene or isopropylidene olefin metathesis-active complexes in the absence of free propylene. Propylene and isopropylidene complexes (W(NAr)(ArNH 2 )(OR F9 ) 2 (propylene) and W(NAr)(ArNH 2 )(OR F9 ) 2 (CMe 2 )) are formed at room temperature from both W(NAr) 2 (i-propyl) 2 and W(NAr) 2 (n-propyl) 2 complexes upon addition of two equivalents of R F9 OH; no W = CHCH 2 Me complexes are observed. Similar results are found for W(NAd) 2 (propyl) 2 complexes (Ad = 1-adamantyl). Both RNH 2 and RNH 2 B(C 6 F 5 ) 3 (R = Ar or Ad) catalyze the interconversion of propylene and isopropylidene complexes. Addition of R F6 OH to W(NAr) 2 R 2 or W(NAd) 2 R 2 complexes leads to mixtures that contain largely propylene complexes. Addition of (CF 3 )Me 2 COH (R F3 OH) to W(NAr) 2 (i-Pr) 2 yields only propylene complexes. One propylene complex, W(NAd)(OR F9 ) 2 (CH 2 ═CHMe)(dme), was isolated, structurally characterized, and found to react with AdNH 2 to reform W(NAd)(OR F9 ) 2 (CMe 2 )(AdNH 2 ). Furthermore, it is proposed that propylene and isopropylidene complexes interconvert through the formation of an intermediate isopropyl complex.

Alkyls↗
DOE OSTI2020

High-throughput phase-field simulations and machine learning of resistive switching in resistive random-access memory

Metal oxide-based Resistive Random-Access Memory (RRAM) exhibits multiple resistance states, arising from the activation/deactivation of a conductive filament (CF) inside a switching layer. Understanding CF formation kinetics is critical to achieving optimal functionality of RRAM. Here a phase-field model is developed, based on materials properties determined by ab initio calculations, to investigate the role of electrical bias, heat transport and defect-induced Vegard strain in the resistive switching behavior, using MO 2- x systems such as HfO 2- x as a prototypical model system. It successfully captures the CF formation and resultant bipolar resistive switching characteristics. High-throughput simulations are performed for RRAMs with different material parameters to establish a dataset, based on which a compressed-sensing machine learning is conducted to derive interpretable analytical models for device performance (current on/off ratio and switching time) metrics in terms of key material parameters (electrical and thermal conductivities, Vegard strain coefficients). These analytical models reveal that optimal performance (i.e., high current on/off ratio and low switching time) can be achieved in materials with a low Lorenz number, a fundamental material constant. This work provides a fundamental understanding to the resistive switching in RRAM and demonstrates a computational data-driven methodology of materials selection for improved RRAM performance, which can also be applied to other electro-thermo-mechanical systems.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Synthesis and molecular structure of perhalogenated rhenium-oxo corroles

Abstract As part of our efforts to develop rhenium-oxo corroles as photosensitizers for oxygen sensing and photodynamic therapy, we investigated the potential β -perhalogenation of five ReO meso -tris( para -X-phenyl)corroles, Re[T p XPC](O) (X = CF 3 , H, F, CH 3 , and OCH 3 ), with elemental chlorine and bromine. With Cl 2 , β -octachlorinated products Re[Cl 8 T p XPC](O) were rapidly obtained for X = CF 3 , H, and CH 3 , but X = OCH 3 resulted in overchlorination on the meso -aryl groups. Full β -octabromination proved slower relative to Cu and Ir corroles, but the desired Re[Br 8 T p XPC](O) products were finally obtained for X = H and F after a week at room temperature. For X = CH 3 and OCH 3 , these conditions led to undecabrominated products Re[Br 11 T p XPC](O). Compared to the β -unsubstituted starting materials, the β -octahalogenated products were found to exhibit sharp 1 H NMR signals at room temperature, indicating that the aryl groups are locked in place by the β -halogens, and substantially redshifted Soret and Q bands. Single-crystal X-ray structures of Re[Cl 8 T p CF 3 PC](O), Re[Cl 8 T p CH 3 PC](O), and Re[Br 8 T p FPC](O) revealed mild saddling for one Cl 8 structure and the Br 8 structure. These structural variations, however, appear too insignificant to explain the slowness of the β -octabromination protocols, which seems best attributed to the deactivating influence of the high-valent Re center.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Molecular insights into photostability of fluorinated organic photovoltaic blends: role of fullerene electron affinity and donor–acceptor miscibility

In this report, the photostability of certain organic photovoltaic (OPV) active layers was demonstrated to improve by as much as a factor of five under white light illumination in air with the use of 1,7-bis-trifluoromethylfullerene (C 60 (CF 3 ) 2 ) as the acceptor in place of PC 60 BM. However, the results were highly dependent on the structure and functionality within the donor material. Twelve combinations of active layer blends were studied, comprised of six different high-performance donor polymers (two fluorinated and four non-fluorinated donors) and two fullerene acceptors (PC 60 BM and C 60 (CF 3 ) 2 ). The relative rates of irreversible photobleaching of the active layer blends were found to correlate well with the electron affinity of the fullerene when the polymer and fullerene were well blended, but a full rationalization of the photobleaching data requires consideration of both the electron affinity of the fullerene as well as the relative miscibility of the polymer–fullerene components in the blend. Miscibility of those components was probed using a combination of time-resolved photoluminescence (TRPL) measurements and scanning tunneling microscopy (STM) imaging. The presence of fluorinated aromatic units in the donor materials tend to promote more intimate mixing with C 60 (CF 3 ) 2 as compared to PC 60 BM. The full results of these photobleaching studies and measurements of donor–acceptor miscibility, considered alongside additional photoconductance measurements and preliminary device work, provide new molecular optimization insights for improving the long-term stability of OPV active layers.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Selective heterogeneous capture and release of actinides using carborane-functionalized electrodes

Here we report the heterogenization of molecular, electrochemically switchable ortho-substituted carboranes ( PO Cb, PO Cb-Pyr) for selective metal capture. Films of PO Cb and PO Cb-Pyr on glassy carbon and carbon fiber (CF) electrodes demonstrated heterogeneous electrochemical behaviour that was enhanced by the inclusion of single-walled carbon nanotubes (CNTs). Galvanostatically charged CF|CNT| PO Cb and CF|CNT| PO Cb-Pyr electrodes selectively captured and released actinides (Th 4+ , UO 2 2+ ) from mixed solutions containing alkali (Cs + ), lanthanide (Nd 3+ , Sm 3+ ) and actinide (Th 4+ , UO 2 2+ ) metal ions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

In situ studies of reversible solid–gas reactions of ethylene responsive silver pyrazolates

Solid–gas reactions and in situ powder X-ray diffraction investigations of trinuclear silver complexes {[3,4,5-(CF 3 ) 3 Pz]Ag} 3 and {[4-Br-3,5-(CF 3 ) 2 Pz]Ag} 3 supported by highly fluorinated pyrazolates reveal that they undergo intricate ethylene-triggered structural transformations in the solid-state producing dinuclear silver–ethylene adducts. Despite the complexity, the chemistry is reversible producing precursor trimers with the loss of ethylene. Less reactive {[3,5-(CF 3 ) 2 Pz]Ag} 3 under ethylene pressure and low-temperature conditions stops at an unusual silver–ethylene complex in the trinuclear state, which could serve as a model for intermediates likely present in more common trimer–dimer reorganizations described above. Complete structural data of three novel silver–ethylene complexes are presented together with a thorough computational analysis of the mechanism.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Trinuclear gold chains and octanuclear copper gyrobifastigia stabilized using a fluorinated pyridyl ligand

The fluorinated pyridyl ligand [6-(CF 3 )-2-Py] − with gold( I ) affords trinuclear Au 3 assemblies that further organize into a supramolecular helical column through aurophilic interactions. Its chemistry with copper( I ) is even more remarkable, leading to an unprecedented octanuclear copper–pyridyl cluster complex featuring a central Cu 8 core with an approximate gyrobifastigium geometry. Solid powders of compounds {(6-(CF 3 )-2-Py)Au} 3 and {(6-(CF 3 )-2-Py)Cu} 8 exhibit intense photoluminescence at room temperature, displaying green and yellow colors to the naked eye, respectively. Here, the octanuclear copper complex is also an effective catalyst for azide–alkyne cycloaddition, producing triazoles. Detailed computational analyses confirm the preference for experimental geometries and provide insights into the observed luminescence.

Phan, Vo Quang Huy [University of Texas at Arlingt↗
DOE OSTI2025

Formation of tungsten ethylidene complexes from diethyl complexes through a proton-catalyzed rearrangement of ethylene

Here, W(NAr) 2 Et 2 (Ar = 2,6-diisopropylphenyl) reacts with two equivalents of R F9 OH (OR F9 = OC(CF 3 ) 3 ) to yield W(NAr)(ArNH 2 )(OR F9 )2(C 2 H 4 ) complexes and ethane. In solution W(NAr)(ArNH 2 )(OR F9 ) 2 (C 2 H 4 ) decomposes to give R F9 OH, ethane, W(NAr)(OR F9 ) 2 (C 2 H 4 ), and W(NAr)(NHAr′)(ArNH 2 )(OR F9 ), in which Ar′ contains a dehydrogenated isopropyl group (Ar′ = (2-i-Pr)(6-CMe=CH 2 )C 6 H 3 ) coordinated to the metal. On a similar time scale W(NAr)(OR F9 ) 2 (CHCH 3 ) complexes are formed from W(NAr)(OR F9 ) 2 (C 2 H 4 ) through an ArNH 2 -catalyzed rearrangement of the ethylene ligand. W(NAr)(NHAr′)(ArNH 2 )(OR F9 ) reacts with cyclohexene to form methylenecyclohexene and complexes that contain an NHAr″ ligand where Ar″ is a disubstituted (methyl/aryl) alkylidene, (2-i-Pr)(6-CMe)C 6 H 3 ) that is tethered to the metal through the amido nitrogen. In contrast to W(NAr)(ArNH 2 )(OR F9 ) 2 (C 2 H 4 ), analogous OR F6 (OCMe(CF 3 ) 2 ) and OR F3 (OCMe 2 (CF 3 )) complexes are relatively stable at 22 °C.

Maji, Milan [University of California, Riverside, ↗
DOE OSTI2023

Mass-selected ion–molecule cluster beam apparatus for ultrafast photofragmentation studies

We describe an apparatus for investigating the excited-state dissociation dynamics of mass-selected ion–molecule clusters by mass-resolving and detecting photofragment-ions and neutrals, in coincidence, using an ultrafast laser operating at high repetition rates. The apparatus comprises a source that generates ion–molecule clusters, a time-of-flight spectrometer, and a mass filter that selects the desired anions, and a linear-plus-quadratic reflectron mass spectrometer that discriminates the fragment anions after the femtosecond laser excites the clusters. The fragment neutrals and anions are then captured by two channeltron detectors. The apparatus performance is tested by measuring the photofragments: I – , CF 3 I – , and neutrals from photoexcitation of the ion–molecule cluster CF 3 I·I – using femtosecond UV laser pulses with a wavelength of 266 nm. Here, the experimental results are compared with our ground state and excited state electronic structure calculations as well as the existing results and calculations, with particular attention to the generation mechanism of the anion fragments and dissociation channels of the ion–molecule cluster CF 3 I·I – in the charge-transfer excited state.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2024

Single-event burnout in homojunction GaN vertical PiN diodes with hybrid edge termination design

GaN devices play a major role in modern electronics, providing high-power handling, efficient high-frequency operation, and resilience in harsh environments. However, electric field crowding at the edge of the anode often limits its full potential, leading to single-event effects (SEEs) at lower bias voltages under heavy ion radiation. Here, in this work, we report on the performance of homojunction GaN vertical PiN diodes with a hybrid edge termination design under heavy ion irradiation, specifically, oxygen ions, chlorine ions, Cf-252 fission fragments, and alpha particles from an Am-241 source. The unique hybrid edge termination (HET) design provides better electric field management, preventing breakdown from occurring at the edge of the anode at lower voltages. The results of this study reveal that these devices exhibit excellent tolerance to 12-MeV oxygen and 16-MeV chlorine ions, owing to their low linear energy transfer (LET) and range in GaN. However, single-event burnout (SEB) is observed during the Cf-252 exposure at about 50% of the diodes' electrical breakdown voltage due to the presence of higher LET and longer-range ions. Optical and scanning electron microscopy (SEM) reveal that the damage that caused by SEB lies close to the center of these devices rather than the anode edge. Devices with junction termination extension (JTE) instead of HET edge termination also show similar SEB when irradiated with Cf-252 fission fragments. Physical damage due to SEB occurs at the edge of the anode for these devices. These comparative results show the benefits of HET for enhancing the resistance of GaN-based PiN diodes to heavy ion irradiation.

42 ENGINEERING↗
DOE OSTI2025

Introduction, Investigation, and Experimental Validation of a Novel Passive Neutron Spectrometer

Unfolding neutron energy spectra are instrumental for determining personal health effects and calculating dose received. This area of study is heavily researched, and Lawrence Livermore National Laboratory (LLNL) is investigating a passive neutron spectrometer for the purpose of acquiring the information needed to determine personnel dose in the event of a criticality accident. A part of this investigation is presented in this article through the examination of four experimental detector responses (DRs). These four DRs were acquired in the presence of 252 Cf, AmBe, GODIVA, and National Ignition Facility (NIF) neutron sources. An algorithm developed at LLNL was used to unfold the neutron fluence from each of the four DRs, and subsequently, fluence-to-dose conversion factors provided by the American National Standards Institute were used to calculate dose. Additionally, a multistep unfolding process was developed and employed to calculate the effects of both direct (from the source) and indirect (from room return) neutrons. The average error when unfolding the direct DR was less than 8%. The dose from 252 Cf was predicted with only 8% error. The multistep approach allowed for the identification of the low-energy neutrons in the 252 Cf, AmBe, and NIF DRs.

Nuclear Criticality Safety Program (NCSP)↗
DOE OSTI2024

Role of gas composition in weakened nonlinear standing wave excitation and improved plasma radial uniformity in very-high-frequency asymmetric capacitive Ar/CF 4 discharges

Abstract The higher harmonics generated by nonlinear sheath motion would enhance the standing wave effect, and thus lead to center-peaked plasma density profile in very-high-frequency (VHF) capacitive discharges. In this work, a nonlinear transmission line (NTL) model introduced in Zhouet al(2021Plasma Sources Sci. Technol.30125017) has been extended, with radial transport of various particles and nonlinear sheath motion into account, to investigate the effects of CF 4 fraction α on the nonlinear standing wave excitation and plasma radial uniformity in VHF (60 MHz) capacitively coupled Ar/CF 4 plasmas at 3 Pa. The results indicate that for pure Ar discharges (i.e. α = 0%), the nonlinearly excited harmonics with short wavelength significantly enhance the electron power absorption at the radial center, resulting in a pronounced central-high plasma density profile. As α increases, the high-order harmonics are gradually damped due to the increase of resistance, as well as the longer wavelength caused by thicker sheath thickness. Thus, the radial profile of the electron absorbed power density shifts from center-peak to edge-high. Besides, at the radial center, the electron density and Ar + ion density decrease with α , CF 3 + ion density shows an increasing trend, while F − ion density initially rises and then decreases. Moreover, the density profiles of all the species become more uniform at higher CF 4 fraction, due to the suppressed nonlinear standing wave excitation and the longer wavelength of the nonlinear harmonics.

Physics↗
DOE OSTI2023

The structure of molten calcium ferrite under various redox conditions

Laser-heated melts based on the 43CaO–57Fe 2 O 3-x eutectic, close to the calcium ferrite (CF) composition, were measured with high-energy X-ray diffraction using aerodynamic levitation over a range of redox states controlled by CO/CO 2 gas atmospheres. The iron–oxygen coordination number was found to rise from 4.4 ± 0.3 at 15% Fe 3+ to 5.3 ± 0.3 at 87% Fe 3+ . Empirical potential structure refinement modelling was used to obtain the ferric and ferrous partial pair distribution functions. It was found that the Fe 2+ iron–oxygen coordination number is consistently approximately 10% higher in CF than in pure iron oxide, while Fe 3+ is essentially identical in all but the most oxygen-rich environments (where it is higher in CF compared with FeO x ). The model also shows calcium octahedra to be the dominant species across all redox environments, although the population of CaO 7 increases with the availability of oxygen at the expense of CaO 4 and CaO 5 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Fingerprints of composite fermion Lambda levels in scanning tunneling microscopy

A composite fermion (CF) is a topological quasiparticle that emerges from a nonperturbative attachment of vortices to electrons in strongly correlated two-dimensional materials. Similar to noninteracting fermions that form Landau levels in a magnetic field, CFs can fill analogous “Lambda” levels, giving rise to the fractional quantum Hall (FQH) effect of electrons. Here, we show that Lambda levels can be directly visualized through the characteristic peak structure in the signal obtained via spectroscopy with scanning tunneling microscopy (STM) on a FQH state. Complementary to transport, which probes the low-energy properties of CFs, we show that high-energy features in STM spectra can be interpreted in terms of Lambda levels. We numerically demonstrate that STM spectra can be accurately modeled using Jain's CF theory. Our results show that STM provides a powerful tool for revealing the anatomy of FQH states and identifying physics beyond the noninteracting CF paradigm.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗