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At least 37 records · Page 2

Solvation Environment and Interface Dynamics of Li 2 B 12 H 12 and Li 2 B 12 F 12 Electrolytes Uncovered by Theory and Operando Optical and FTIR Spectroelectrochemistry

In this work, we evaluated two closo-borate salts (Li 2 B 12 H 12 and Li 2 B 12 F 12 ) in propylene carbonate from theoretical and experimental perspectives to understand how the coordination environment influences their spectroscopic and electrochemical properties. The coordination environments of the closo-borate salts were modeled via density functional theory (DFT) and molecular dynamics (MD). Vibrational spectra calculated from the predicted coordination environments are in agreement with experimentally measured steady-state FTIR data. This theoretical investigation also suggested that Li 2 B 12 F 12 would possess a higher ionic conductivity than Li 2 B 12 H 12 , which was corroborated experimentally. Additionally, an electrochemical cell was designed and fabricated that enabled operando optical and FTIR spectroelectrochemical (OP-IR-SEC) measurements. This allowed for the simultaneous measurement of the relative changes of species at a lithium electrode-liquid electrolyte interface and the visualization of lithium plating at the electrode surface. This technique could provide new chemical insights and potentially link optical changes at the electrode–electrolyte interface to specific chemical species in similar electrochemical systems. The Li 2 B 12 F 12 electrolyte was found to have a higher thermal stability, which may find utility in applications for batteries that are subject to high-temperature conditions.

36 MATERIALS SCIENCE

Boron-Based Neutron Scintillator Screen Characterization with X-Rays and Neutrons

Recent work on boron-based neutron scintillator screens suggests these screens can offer superior performance when compared to commonly used screens. Borated neutron scintillator screens perform well in terms of light output (5-6 times greater than a standard Gadox screen) and detection effi-ciency (larger than standard LiF+ZnS screens). However, previously manu-factured boron-based screens have exhibited non-uniform surface coating and a poor mixture between phosphor and converter particles. The objective of this work was to evaluate newly fabricated scintillator screens to deter-mine if enhanced fabrication methods produced a more homogeneous distribution between neutron converter and scintillation phosphor particles. Uniformity of scintillator material deposition was also inspected. This new iteration of screens appeared more uniform than previous generations with the new coating method improving surface chemistry and scintillator material homogeneity. Additionally, a new methodology for screen characterization, involving the correlation of a neutron image taken with a borated scintillator screen to X-ray computed tomography of that same screen, was demonstrated to elucidate a relationship between scintillator screen thickness and relative light output of the screen under neutron exposure. This method suggested that the ideal thickness of scintillator material was ~150 µm to maximize light output of the screen.

36 - MATERIALS SCIENCE

From Electronic Structure to Ion Transport: Photoelectron Spectroscopy and Molecular Dynamics Simulations Reveal the Role of Anions in Lithium Battery Electrolytes

Electrolyte anions are pivotal for lithium battery performance, yet their fundamental electronic structural properties are not well understood. In this work, we employ a combination of negative-ion photoelectron spectroscopy (NIPES), ab initio calculations, and molecular dynamics (MD) simulations to investigate the electronic structures of three representative electrolyte anions. This multiscale approach enables us to elucidate how their intrinsic electronic properties govern anion–solvent interactions in gas-phase clusters, as well as lithium-ion (Li + ) solvation structures and ion transport behavior in the condensed phase. NIPES reveals that difluoro(oxalato)borate (DFOB – ), bis(fluorosulfonyl)imide (FSI – ), and bis(oxalato)borate (BOB – ) all exhibit high electron binding energies, with vertical/adiabatic detachment energies increasing from DFOB – (6.09/5.70 eV) to FSI – (6.80/6.10 eV) to BOB – (6.82/6.40 eV), correlating with enhanced oxidation stability. Ab initio calculations reveal that DFOB – /FSI – –solvent complexes bind Li + ∼ 10 kcal/mol stronger than BOB – series, aligning with the strength of a Li + –anion model. DFOB – exhibits pronounced charge localization on both oxygen and fluorine atoms, enabling their involvement in Li + coordination. In contrast, fluorine atoms in FSI – are largely electron-depleted and remain excluded from direct Li + binding. MD simulations further demonstrate that LiDFOB and LiFSI systems exhibit Li + diffusion coefficients three and five times higher than those of LiBOB across four common solvents. Notably, LiFSI salt in acetonitrile (AN) exhibits the fastest Li + diffusion among 12 electrolyte systems, highlighting the synergistic effect of FSI – and AN in promoting ion mobility. In conclusion, these findings provide a molecular-level understanding of the critical roles of anion and its microsolvation in optimizing Li + diffusion dynamics, once again emphasizing the positioning of FSI – and DFOB – as prime candidates for next-generation electrolytes.

25 ENERGY STORAGE

A low-cost, fluorine-free electrolyte for improved sodium batteries

Sodium batteries are an attractive alternative to lithium-ion technologies due to sodium’s lower cost and natural abundance—over 1,000 times greater than lithium, comprising approximately 2.4% of the Earth’s crust. However, most current electrolytes rely on fluorine-containing components, which raise economic and environmental concerns. This study explores fluorine-free, borate-based electrolytes that offer improved cycling stability and significant cost and sustainability benefits. We demonstrate stable sodium metal stripping and plating on aluminum foil, enabling anode-free cell configurations with over 50% capacity retention after 700 cycles. Spectroscopic and electrochemical analyses reveal the effects of solvents and salt composition on solvation, ionic conductivity, and oxidative stability. In full-cell configurations, the fluorine-free electrolyte maintains more than 98% capacity retention after 400 cycles. Furthermore, these findings represent a critical step toward the development of cost-effective, environmentally friendly, and high-performance sodium battery systems suitable for future electrification.

anode-free sodium batteries

Seamless aperture and length enlargement of single crystalline materials for high-energy laser applications

An optically seamless method for increasing the aperture or length of nonlinear materials has been developed, which is suitable for optics in high energy laser systems and other applications. Differences between aperture and length scaling are analyzed. Bonding of component pairs of a nonlinear crystal, lithium tri-borate, is experimentally demonstrated by GAMDAN Optics Inc. and tested at the Laboratory of Laser Energetics at the University of Rochester. Here, a bonded crystal is shown to deliver beam quality and second harmonic conversion efficiency that is equivalent to that of a monolithic crystal of similar dimensions.

aperture scaling

Mastering the Copolymerization Behavior of Ethyl Cyanoacrylate as Gel Polymer Electrolyte for Lithium‐metal Battery Application

Polymers with strong electron-withdrawing groups (e.g., cyano-containing polymers) are attractive for a wide range of applications due to their high dielectric constant and outstanding electrochemical stability. However, the polymerization of such monomers is difficult to control with trace of water affording instant reactions, and copolymerization with other monomers without using strong acid is even more challenging. The present study demonstrates a facile approach enabling efficient and controllable copolymerization of ethyl cyanoacrylate (ECA) without adding undesired additives, achieving mechanically robust and high ion-conduction gel polymer electrolyte (GPE) for safe and long cycle-life lithium-metal batteries (LMBs). The incorporated dual-lithium salts, i.e., lithium difluoro(oxalato)borate (LiDFOB) and lithium bis(trifluoromethanesulphonyl)imide (LiTFSI) not only facilitate radical polymerization of ECA monomers by suppressing their anionic polymerization, but also promote the formation of high-ionic conducting GPE. The incorporated methyl methacrylate (MMA) monomer accelerates the radical polymerization of ECA (confirmed by DFT calculations), achieving controlled copolymerization of ECA-based copolymers. Here, the mechanically robust polymer network made by the ECA copolymer enables LMBs with both LFP cathodes and high-voltage LCO cathodes (4.5 V) operatable at different temperatures with ultra-long cycle life at 1 C (capacity retention of 81.1 % and 83.8 %, respectively, over 1000 cycles).

Min, Weixing [Nankai University, Tianjin (China)]

The Psyche Gamma-Ray and Neutron Spectrometer

A Gamma-Ray and Neutron Spectrometer (GRNS) instrument has been developed as part of the science payload for NASA’s Discovery Program Psyche mission to the M-class asteroid (16) Psyche. The GRNS instrument is designed to measure the elemental composition of Psyche with the goal to understand the origin of this mysterious, potentially metal-rich planetary body. The GRNS will measure the near-surface abundances for the elements Ni, Fe, Si, K, S, Al, and Ca, as well as the spatial distribution of Psyche’s metal-to-silicate fraction (or metal fraction). These measurements address three of the five Psyche mission science objectives: determine if Psyche is a core; determine whether small metal bodies incorporate light elements into the metal phase; and determine whether Psyche was formed under reducing conditions. The Gamma-Ray Spectrometer (GRS) uses a cryocooled, high-purity Ge (HPGe) sensor to detect cosmic-ray generated gamma rays in the 60 to 9000-keV energy range. The HPGe sensor is surrounded by a borated plastic anticoincidence shield that provides three functions: active background rejection from charged particle interactions in the HPGe sensor; fast neutron measurements; and direct measurements of the incident galactic cosmic ray flux. The Neutron Spectrometer (NS) uses three 3 He gas proportional sensors, each with different material wraps to measure thermal (<0.4 eV), low-energy epithermal (0.4 eV to 1 keV), and high-energy epithermal (up to 100 keV) neutrons. This paper provides an overview of the Psyche GRNS, including: its science and measurement objectives; the design of the instrument hardware, software, and operation; pre-launch performance measurements and its initial performance in space; and an overview of its data products and expected operation for different Psyche mission phases.

Engineering - Instrumentation related to nuclear s

Ground calibration and in-flight commissioning of the Gamma-Ray and Neutron Spectrometer (GRNS) for NASA’s Psyche mission

NASA's Psyche spacecraft is currently enroute to the asteroid 16 Psyche, where it will perform an orbital investigation focused on determining the nature of the asteroid. A key part of this investigation is measurements of elemental composition to determine if the asteroid is rich in iron-nickel metal. To that end, the Psyche spacecraft payload includes a Gamma-Ray and Neutron Spectrometer (GRNS). GRNS is composed of two subsystems; a Gamma-Ray Spectrometer (GRS) with a high-purity germanium γ-ray sensor surrounded by a borated plastic scintillator Anti-Coincidence Shield (ACS), and a Neutron Spectrometer (NS) with three 3 He-filled gas proportional counters that are sensitive to different neutron energy regimes. We describe results from the pre-launch calibration campaign, along with early in-flight results from post-launch instrument commissioning. The information detailed here is focused on providing future users of GRNS data with the information needed to properly interpret the observations from the instrument.

Peplowski, Patrick N. [Johns Hopkins Univ., Baltim

Characterizing the Experiment for Calibration with Uranium (Excalibur) neutron source for use in warhead verification

Neutron sources can play a variety of roles in warhead verification. For transmission radiography, a source of directed high energy neutrons is required, while for applications to detect fissile isotopes, sub-MeV neutrons are preferred. The Excalibur (Experiment for Calibration with Uranium) neutron source has been built and used in a variety of verification-related experiments. Excalibur is based on a commercial deuterium-tritium neutron generator specified and measured to be capable of producing 14 MeV neutrons at rates of up to 8.2 × 10 8 neutrons/s. Here, the generator is enclosed in a carbon-steel 32" diameter, 23.62" high carbon-steel cylinder that moderates the mean neutron energy to under 500 keV. This, in turn, is encased in 5%-borated polyethylene such that the entire assembly is a 48" x 48" box that is 30" tall. For radiographic applications, a narrow, tapered channel in the steel and polyethylene allows 14 MeV neutrons to stream directly from the generator to a test object. Its collimating capability is demonstrated by measuring the neutron flux profile. In the moderated mode of operation, the generator is fully enclosed in the steel, but a large section of the polyethylene is removed, providing a flux of sub-MeV neutrons from a wide range of angles. Neutron angular and spectral measurements using both a nested neutron spectrometer and a commercial liquid scintillator coupled with a 3 He detector show the expected softer neutron spectrum in moderated mode in good agreement with MCNP6 calculations. The gamma-ray spectrum from Excalibur is also in good agreement with MCNP modeling. Based on these findings, the future application of Excalibur in its two configurations is discussed.

Fissile material detection

Mitigating Calendar Aging in Si-NMC Batteries with Advanced Dual-Salt Glyme Electrolytes

In addressing the critical challenge of calendar aging in silicon (Si)-based lithium-ion batteries, this study introduces a groundbreaking strategy utilizing glyme-type dual-salt electrolytes (lithium bis(trifluoromethanesulfonyl)imide [LiTFSI] and lithium difluoro(oxalato)borate [LiDFOB]). These electrolytes are demonstrated to significantly mitigate parasitic reactions and capacity loss in Si-NMC (lithium nickel manganese cobalt oxide) full cells, especially when compared with traditional carbonate-based electrolytes. Further, our exhaustive mechanistic analysis reveals that such electrolytes not only preserve the integrity of the Si anode but also improve the cathode/electrolyte interphases (CEI) through the formation of a conformal coating on the high-voltage cathode surface. This dual-salt approach, enhanced by the addition of a phosphate additive, effectively decelerates calendar aging, marking a substantial advance in the quest for durable and reliable Si-based energy storage technologies. The findings underscore the vital role of electrolyte composition in extending the calendar life of Si batteries, offering an alternative avenue toward maximizing the performance and longevity of next-generation Li-Si batteries.

36 MATERIALS SCIENCE

Magnetic and EPR Spectroscopic Studies of Thiolate Bridged Divalent Ni, Pd, and Pt Ions Capped with VO(N 2 S 2 ) Metalloligands

Reactions of the metallodithiolate complex VO(bme-dach) (hereafter abbreviated as V, where bme-dach = N,N ′-bis(2-mercaptoethyl)-1,4-diazacycloheptane) with [Pd II (CH 3 CN) 4 ](BF 4 ) 2 and [Pt II (CH 3 CN) 4 ](BF 4 ) 2 yield the V–M–V trimetallic compounds [VPdV](BF 4 ) 2 (2) and [VPtV](BF 4 ) 2 (3). Reaction of a similar metalloligand, VO(bme-daco) (hereafter abbreviated as V′ where bme-daco = N,N′-bis(2-mercaptoethyl)-1,5-diazacyclooctane) with [Ni II (CH 3 CN) 6 ](BF 4 ) 2 afforded the related salt [V′NiV′](BF 4 ) 2 (1). X-ray structural analyses revealed that cations in 1, 2, and 3 adopt a stairstep C 2h structure consisting of two terminal VO(N 2 S 2 ) moieties bridged via thiolate sulfur to the group 10 metal ions. Weak ferromagnetic superexchange coupling (J = 0.282 cm –1 for 1, 0.954 cm –1 for 2, and 1.372 cm –1 for 3) was observed between the two S = 1/2 V IV centers separated by distances in the range of 5.9–6.3 Å, with J values varying following the order Ni < Pd < Pt. Frozen-solution EPR spectra measured on the more soluble [BArF 24 ] − (BArF 24 – = tetrakis((3,5-trifluoromethyl)phenyl)borate) analogues revealed that the [VPtV] 2+ cation exhibits a 15-line hyperfine splitting of 225 MHz at g = 4 in parallel mode, confirming exchange coupling between the two 51 V, I = 7/2 nuclei. Density-functional theory (DFT) calculations indicate an S = 1 ground state for 1–3. These results demonstrate that the choice of paramagnetic metallodithiolate ligand and diamagnetic bridge in such trimetallic species influences the sign and magnitude of magnetic interactions.

anions

Synthesis and Reactivity of Heteroleptic U 4+ Alkyl, Benzyl, and Hydride Imidophosphorane Complexes

A series of heteroleptic U 4+ benzyl, neopentyl, and methyl complexes supported by the imidophosphorane ligand, [N = P(N,N′-ditert-butylethylenediamide)(diethylamide)] 1− (NP*), were synthesized from the monoiodide precursor, [UI(NP*) 3 ]. These heteroleptic complexes were synthesized through the selective formation of [UI(NP*) 3 ] under transmetalation conditions in the reaction between [UI 4 (1,4-dioxane) 2 ] and K[NP*]. Formation of the homoleptic complex [U(NP*) 4 ] was not observed even in the presence of excess K[NP*]. The oxidation and hydrogenolysis reactivity of the neopentyl complex, [U(Npt)- (NP*) 3 ] (Npt = neopentyl) was explored. While cyclic voltammetry indicates a potentially isolable U5+ alkyl cation, chemical oxidation of the neopentyl complex results in the isolation of a cationic U 4+ complex with a bound diethyl ether in the primary coordination sphere, [U4+(NP*)) 3 (Et 2 O)][(BArF 24 )] (BArF 24 = tetrakis(3,5-bis(trifluoromethyl)phenyl)borate). Notably, hydrogenolysis of [U(Npt)(NP*) 3 ] with H2 gas at −20 °C results in the formation of a terminal hydride intermediate confirmed by in situ NMR spectroscopy and deuterium labeling with D 2 . The connectivity and structural parameters of this hydride intermediate, [UH(NP*) 3 ], which rapidly thermally decomposes to the homoleptic complex, [U(NP*) 4 ], can be confirmed by single-crystal X-ray diffraction studies of a crystal grown by chilling the reaction mixture. The identity of [U(NP*) 4 ] was confirmed by its direct, bulk synthesis from [U(Me)(NP*) 3 ] and HNP* in a protonolysis reaction.

Alkyls

Multi-Ion Complexes and Competition from Bulky BArF – Anions for Chloride Binding in Ion Pairing Conditions

Cationic charges have long been used to enhance anion binding. Embedding charge introduces strong ion pairing for target anions but also for off-target ions, ultimately generating a mixture of multi-ion species that are hard to identify and quantify. While many sidestep this problem using polar solvents and weakly coordinating ions, these approaches exclude a substantial cross-section of conditions found in applications spanning recognition, assembly, separations, templation, and catalysis. To confront this complexity, we study the binding of an anion to a cationic receptor featuring low shape complementarity in a low-polarity solvent to maximize ionic interactions. We prepared the receptor as a salt of the weakly coordinating tetrakis­[3,5-bis­(trifluoromethyl)­phenyl]­borate (BArF – ) anion and studied the binding of small chloride (Cl – ) and medium-sized iodide (I – ) anions. Surprisingly, the use of the bulky BArF – anion does not suppress ion pairing interactions, with 65% of the receptor being paired at 0.5 mM in dichloromethane. We observe multi-ion receptor-Cl – complexes (2:1, 1:1, 1:2), reinforcing the complexity that emerges when working in low-polarity media. Here, we reveal the dependence of affinity on anion charge density and size and that bulky BArF – counteranions compete for chloride binding. These studies reveal the noninnocence of BArF – anions and strategies to quantify multi-ion species.

Ion pairing

Ionic-Based Electrochemical Gas Sensors for Low-Cost, High-Sensitivity SO2 Detection

Sulfur dioxide (SO2) is a toxic gas associated with adverse health and environmental effects that necessitate reliable monitoring techniques. Here, we report the development of an all-solid-state electrochemical sensor utilizing a lithium borate (Li3BO3) solid electrolyte capable of subppm of SO2 detection. While subppm of SO2 sensing has been previously demonstrated in other solid-state electrolyte systems─such as stabilized zirconia, natrium super ionic conductors (NASICON) under mixed-potential conditions─here we establish Li3BO3 as an alternative solid electrolyte enabling equilibrium potentiometric sensing in an all-solid architecture. This sensor demonstrates a detection limit of at least 0.25 ppm, surpassing the human-olfactory threshold and meeting the rigorous requirements for industrial and personal monitoring applications. The sensing mechanism relies on the formation of Li2SO4 on the electrode surface, as evidenced by multimodal characterization techniques, including Raman spectroscopy, scanning electron microscopy (SEM), and scanning transmission electron microscopy (STEM). The strong linear correlation between the open-circuit potential (OCV) and the logarithm of SO2 concentration between 0.25 and 2 ppm indicates that the response is Nernstian in nature.

Lagunas, Francisco (ORCID:000000026377683X)

Influence of Electrolyte Additives on Interfacial Stability of Manganese-Rich Lithium-Ion Battery Cathodes

Affordable, long-lasting energy storage has become critical to support increased electricity demand in recent years. Cobalt-free, lithium- and manganese-rich lithium nickel manganese oxide (LMR-NM) cathodes stand to reduce cost and supply-chain concerns associated with traditional cobalt-containing cathodes for lithium-ion batteries by leveraging more earth-abundant materials; however, they have shown issues with long-term cycling stability. Here, we investigate lithium difluoro(oxalate)borate (LiDFOB), tris(trimethylsilyl) phosphite (TMSPi), and vinylene carbonate (VC) electrolyte additives for their ability to improve cycling performance of LMR-NM (0.3 Li 2 MnO 3 + 0.7 LiMn 0.5 Ni 0.5 0 2 ) cells. Cryogenic scanning transmission electron microscopy (cryo-STEM) with electron energy loss spectroscopy enables the construction of a structure–function relationship between cathode electrolyte interphase (CEI) characteristics and the electrochemical performance of cells aged with these additives. We find the combination of 2 wt % TMSPi + 1 wt % LiDFOB performs better than any single additive, achieving a 28% improvement in specific capacity over the baseline electrolyte after long-term cycling. We attribute this to LiDFOB mitigating Mn ion dissolution, with cryo-STEM showing Mn stabilized up to the CEI surface, coupled with improved CEI structure and chemistry enabled by TMSPi, evidenced by a moderately thick (∼7–15 nm) CEI that appears to protect against further electrolyte reactions with the particle. These results, achieved through site-specific nanoscale characterization, directly reveal mechanisms through which electrolyte engineering can improve the performance of earth-abundant cathodes, enabling informed development of more affordable and reliable batteries to meet future energy storage needs.

25 ENERGY STORAGE

Integrative Additive Design for Robust SEI Formation in NMC811||Silicon Batteries

Silicon (Si) is considered a promising replacement for graphite anodes in lithium-ion batteries (LIBs) due to its high abundance and exceptional specific capacity, but its widespread commercialization has been hindered by poor electrochemical performance. Among various strategies, the use of functional additives has emerged as one of the most effective and cost-efficient methods to enhance the electrochemical properties of LIBs. In this study, several additives—vinylene carbonate (VC), vinyl ethylene carbonate (VEC), lithium difluorophosphate (LiDFP), lithium difluoro(oxalato)borate (LiDFOB), lithium tetrafluorooxalatophosphate (LiTFOP), and lithium difluorobis(oxalato)phosphate (LiDFBOP)—were systematically investigated in LiNi₀.₈Mn₀.₁Co₀.₁O₂ (NMC811)||Si full cells. Notably, LiDFBOP, a lithium salt containing two oxalate groups, outperformed all other additives, delivering the best capacity retention after 300 cycles. Comprehensive characterizations, including FTIR, SEM, and XPS, revealed that LiDFBOP's superior performance stems from its ability to form a more stable solid electrolyte interphase (SEI) on the Si anode, owing to its favorable molecular structure that integrates the beneficial features of the other additives.

25 ENERGY STORAGE

Fast-Charging Li-Ion Battery Enabled by an Acetonitrile-Based Electrolyte

Fast charging remains a critical challenge for current-generation lithium-ion batteries (LIBs), particularly in electric vehicle applications. Here, in this study, we present a highly conductive electrolyte formulation based on a ternary solvent system consisting of acetonitrile (AN), fluoroethylene carbonate (FEC), and ethylene carbonate (EC), combined with a tailored additive, lithium difluoro­(oxalato)­borate (LiDFOB). This electrolyte demonstrates significantly enhanced ionic conductivity and a higher Li + transference number, enabling accelerated Li + transport kinetics. The synergistic effect of the solvents and the additive promotes the formation of a robust, low-resistance, inorganic-rich solid-electrolyte-interphase (SEI) that effectively passivates the graphite surface and suppresses AN decomposition. As a result, the electrolyte substantially reduces internal cell resistance and overpotential, both of which are critical for reliable fast charging. These findings highlight the essential role of rational electrolyte design in addressing the limitations of fast-charging LIBs.

Wu, Dezhen [Argonne National Laboratory (ANL), Arg