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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Revealing the mechanism of lignin re-polymerization inhibitor in acidic pretreatment and its impact on enzymatic hydrolysis

Phenolic additives, including 2-naphthol, 2-naphthol-7-sulfonate, and resorcinol were evaluated for their impact on the lignin re-polymerization and subsequent hydrolysis of bamboo residues. Low surface lignin concentration (65.68%) of the substrate and high Tg value (185 °C) of lignin was observed for 2-naphthol-7-sulfonate assisted pretreatment, leading to the most significant increase (14%) in enzymatic hydrolysis efficiency of pretreated bamboo residues. Meanwhile, physicochemical properties of lignin revealed that the introduced sulfonic acid groups increased the surface charge, decreased the molecular weight, promoted the cleavage of β-O-4 linkages, and prevented the re-condensation of lignin. Even though resorcinol-assisted pretreatment, by contrast, was found to be an inhibitor for enzymatic hydrolysis. NMR analysis of modified lignin showed that resorcinol led to a higher amount of non-condensed phenolic OH groups and promoted the cleavage of β-O-4 linkages, acting as an inhibitor in lignin re-polymerization during the dilute acidic pretreatment. In short, the above findings present a detailed view of suppressing lignin re-polymerization for boosting the utilization of bioresources with acidic pretreatment.

09 BIOMASS FUELS↗
DOE OSTI2022

Catalysts by pyrolysis: Direct observation of transformations during re-pyrolysis of transition metal-nitrogen-carbon materials leading to state-of-the-art platinum group metal-free electrocatalyst

Transition metal-nitrogen-carbon (M-N-C) materials have been the focus of scientists’ efforts to address the rising need for earth-abundant materials solutions for energy technology and decarbonization of the economy. They are viewed as one of the most promising candidates to replace platinum group metal (PGM) catalysts in the fuel cell and energy conversion fields, including the application of oxygen reduction reaction, carbon dioxide reduction reaction, and nitrogen reduction reaction. In the effort to improve M-N-C materials properties and achieve atomic dispersity of the transition metal in the carbonaceous matrix, a re-pyrolysis process has been proposed. This secondary heat treatment process of already obtained primary pyrolysis-derived M-N-C materials has been widely reported to substantially improve the electrochemical performance and operational stability of the catalysts. Here, we report a systematic investigation of this process used on samples of templated M-N-C catalysts to obtain state-of-the-art catalysts via in situ heating X-ray photoelectron spectroscopy (XPS), scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDS), electron energy loss spectroscopy (EELS), X-ray diffraction (XRD), and X-ray computed tomography (CT) characterization methods. It is found that the re-pyrolysis of M-N-C materials could result in the partial amorphization of the carbonaceous substrate. It causes the rearrangement and transformation of multitudinous N moieties, leading to optimization of their morphological display and association with atomically dispersed transition metal dopants. Ultimately, the re-pyrolysis results in an increase in uniformity of the active Fe-Nx sites distribution without the formation of nano-crystalline phases (metallic or carbide) and with overall preservation of the morphology of the carbonaceous framework achieved during the first formative pyrolysis step of the templated synthesis. Finally, these observations provide confirmation that empirically established re-pyrolysis is recommended to be used on all M-N-C materials despite the different synthesis routes to obtain a practical advanced catalytic material.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Vaporization behavior of Ir 4 (CO) 12 and Re 2 (CO) 10 measured by torsion effusion gravimetric method

Metal carbonyls are of great importance in chemical vapor deposition (CVD), composite materials fabrication, and other near-net shape technologies. Carbonyl CVD is used for deposition of high-purity metallic and alloy coatings for which vapor pressure data is essential. In this study, we report vapor pressures of solid Ir 4 (CO) 12 and Re 2 (CO) 10 carbonyls measured by using the Knudsen Cell methodology using a torsion effusion thermogravimetric system. The vapor pressure of the Ir 4 (CO) 12 exhibited incongruent vaporization, as the molecular weight (MW) of the effusing species was determined as 128 g/mol as compared to the theoretical MW of 1105 g/mol. It is proposed that the Ir 4 (CO) 12 (s) partially decomposed (~66%) to Ir 4 (CO) 12 (g), Ir(s), and CO(g). The Re 2 (CO) 10 on the other hand, showed congruent behavior with Re 2 (CO) 10 (s) vaporizing to Re 2 (CO) 10 (g) in the measured temperature range. The raw data for vapor pressures was measured using two sets of Knudsen cells with different orifice sizes, and the equilibrium vapor pressures were calculated using Whitman-Motzfeldt methodology. The equilibrium vapor pressures of these carbonyls, partial pressures of gaseous species in case of decomposition, average molecular weights of the effusing gasses were determined. The vapor pressures and Gibbs energies of vaporization reactions of the two above mentioned carbonyls, as well as comparison of vaporization thermodynamics these two carbonyls with other carbonyls from Group VIB to VIIIB are presented in this work.

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

Synthesis and Surface Attachment of Molecular Re(I) Complexes Supported by Functionalized Bipyridyl Ligands

Eleven 2,2'-bipyridine (bpy) ligands functionalized with attachment groups for covalent immobilization on silicon surfaces were prepared. Five of the ligands feature silatrane functional groups for attachment to metal oxide coatings on the silicon surfaces, while six contain either alkene or alkyne functional groups for attachment to hydrogen-terminated silicon surfaces. The bpy ligands were coordinated to Re(CO) 5 Cl to form complexes of the type Re(bpy)(CO) 3 Cl, which are related to known catalysts for CO 2 reduction. Six of the new complexes were characterized using X-ray crystallography. As proof of principle, four molecular Re complexes were immobilized on either a thin layer of TiO 2 on silicon or hydrogen-terminated silicon. The surface-immobilized complexes were characterized using X-ray photoelectron spectroscopy, IR spectroscopy, and cyclic voltammetry (CV) in the dark and for one representative example in the light. The CO stretching frequencies of the attached complexes were similar to those of the pure molecular complexes, but the CVs were less analogous. For two of the complexes, comparison of the electrocatalytic CO 2 reduction performance showed lower CO Faradaic efficiencies for the immobilized complexes than the same complex in solution under similar conditions. In particular, a complex containing a silatrane linked to bpy with an amide linker showed poor catalytic performance and control experiments suggest that amide linkers in conjugation with a redox-active ligand are not stable under highly reducing conditions and alkyl linkers are more stable. So a conclusion of this work is that understanding the behavior of molecular Re catalysts attached to semiconducting silicon is more complicated than related complexes, which have previously been immobilized on metallic electrodes.

14 SOLAR ENERGY↗
DOE OSTI2020

Magnetic Tunability in RE-DOBDC MOFs via NO x Acid Gas Adsorption

The magnetic susceptibility of NO x -loaded RE-DOBDC (rare earth (RE): Y, Eu, Tb, Yb; DOBDC: 2,5-dihydroxyterephthalic acid) metal–organic frameworks (MOFs) is unique to the MOF metal center. RE-DOBDC samples were synthesized, activated, and subsequently exposed to humid NO x . Each NO x -loaded MOF was characterized by powder X-ray diffraction, and the magnetic characteristics were probed by using a VersaLab vibrating sample magnetometer (VSM). Lanthanide-containing RE-DOBDC (Eu, Tb, Yb) are paramagnetic with a reduction in paramagnetism upon adsorption of NO x . Y-DOBDC has a diamagnetic moment with a slight reduction upon adsorption of NO x . The magnetic susceptibility of the MOF is determined by the magnetism imparted by the framework metal center. The electronic population of orbitals contributes to determining the extent of magnetism and change with NO x (electron acceptor) adsorption. Eu-DOBDC results in the largest mass magnetization change upon adsorption of NO x due to more available unpaired f electrons. Experimental changes in magnetic moment were supported by density functional theory (DFT) simulations of NO x adsorbed in lanthanide Eu-DOBDC and transition metal Y-DOBDC MOFs.

36 MATERIALS SCIENCE↗
DOE OSTI2021

The Impact of U.S. Re-engagement in Climate on the Paris Targets

The Paris Agreement is meant to bind together international efforts to reduce temperature increase to well-below 2ºC. While so far, ambitions in many signatories of the Paris Agreement have been insufficient to achieve this goal, optimism prevailed in the second half of 2020, with several major emitters enhancing their mitigation targets and a change of leadership in the United States (U.S.). Expectations are high for an active re-engagement in climate action by the Biden Administration, which immediately re-entered the Paris Agreement and announced a net-zero goal for 2050. Apart from the impact that U.S. federal re-engagement could have on national greenhouse gas emissions levels, there are several channels through which U.S. re-engagement in climate action could positively impact ambitions in other countries. This Policy Forum explores the impact of renewed U.S. engagement on national emissions, global emissions and end-of-century temperatures by comparing five combinations of climate ambitions in the U.S. and the rest of the world through an integrated assessment model.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Operando video microscopy of Li plating and re-intercalation on graphite anodes during fast charging

Despite the demand for fast-charging lithium (Li)-ion batteries, high-energy-density batteries with thick graphite anodes are limited by Li plating when charging at >4C rates. In this work, plan-view operando video microscopy is applied on >3 mA h cm –2 calendared graphite electrodes to study the dynamic evolution of local state-of-charge (SoC) and Li plating during fast charging. This technique allows for visualization of the spatial heterogeneity in SoC across the electrode, nucleation and growth of Li filaments, Li re-intercalation into graphite, “dead Li” formation, and SoC equilibration. The operando microscopy analysis is complemented by ex situ imaging of through-plane gradients in SoC to gain a three-dimensional visualization of spatial heterogeneity. We demonstrate that (1) Li plating preferentially nucleates on the graphite particles that lithiate fastest during fast charging; (2) the onset of Li plating correlates with the local minimum of the graphite electrode potential; (3) galvanic corrosion currents are responsible for Li re-intercalation, dead Li formation, and SoC re-equilibration after fast charging; and (4) electrochemical signatures during OCV rest or discharge are associated with Li re-intercalation into graphite. Furthermore, this work provides insight into the Li–graphite interactions at the composite electrode level and can be used to inform strategies to diagnose and mitigate Li plating during fast charging.

25 ENERGY STORAGE↗
DOE OSTI2022

Thermoelectric Figure of Merit of a Superatomic Crystal Re 6 Se 8 I 2 Monolayer

Superatomic materials are newly emerging candidates for high-performance thermoelectric (TE) devices due to their intrinsic ultralow thermal conductivities. However, the low TE power factor becomes a huge obstacle to reaching the required the dimensionless figure of merit (ZT) values for practical applications. Here, motivated by the recently synthesized superatomic Re 6 Se 8 I 2 monolayer [J. Am. Chem. Soc. 144, 74 (2022)], we study its superior thermoelectric properties by using density functional theory combined with phonon Boltzmann transport theory and deep potential molecular dynamics. We show that the large mass and anharmonic Re-I bonds introduce strong phonon scattering and result in low lattice thermal conductivity of 1.20 W m -1 K -1 at 300 K, while the strong and harmonic Re-Se network ensures the high TE power factor of 4344 μW m -1 K -2 in b direction for n-type doping. This is an order of magnitude higher than that of other cluster-based materials. Due to the low thermal conductivity and high TE power factor, Re 6 Se 8 I 2 exhibits high ZT values of 1.20 (500 K) and 1.43 (900 K) with n-type doping along the b direction among all the cluster-based thermoelectric materials reported so far.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Suppression of metal-to-insulator transition and stabilization of superconductivity by pressure in Re 3 Ge 7

The effect of pressure on the low-temperature states of the Re 3 ⁡Ge 7 is investigated by both electrical and Hall resistance and magnetization measurements. At ambient pressure, the temperature-dependent resistance of Re 3 ⁡Ge 7 behaves quasilinearly from room temperature down to 60 K, then undergoes a two-step metal-to-insulator transition (MIT) at temperatures T 1 =59.4K and T 2 =58.7K, which may be related to a structural phase transition or occurrence of charge-density wave ordering. Upon applying pressure, the two-step (T 1 ,T 2 ) MIT splits into three steps (T 1 ,T 2 . and T 3 ) above 1 GPa, and all traces of MITs are fully suppressed by ~8 GPa. Subsequently, the onset of bulk superconductivity (SC) occurs between 10.8 and 12.2 GPa and persists to our highest pressure of 26.8 GPa. At 12.2 GPa the superconducting transition temperature, T c , and upper critical field, H c ⁢2 reach the maximum of T c (onset) ~5.9 K and H c ⁢2 (1.8 K) ~14 kOe. Finally, our results not only present the observation of SC under high pressure in Re 3 ⁡Ge 7 but also delineate the interplay between SC and other competing electronic states by creating a T-p phase diagram for this potentially topologically nontrivial system Re 3 ⁡Ge 7 .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Crystal structures and comparisons of potassium rare-earth molybdates KRE(MoO 4 ) 2 (RE = Tb, Dy, Ho, Er, Yb, and Lu)

Six potassium rare-earth molybdates KRE(MoO 4 ) 2 (RE = Tb, Dy, Ho, Er, Yb, and Lu) were synthesized by flux-assisted growth in K 2 Mo 3 O 10 . The crystal structures were determined using single-crystal X-ray diffraction data. The synthesized molybdates crystallize with the orthorhombic Pbcn space group (No. 60). Trendlines for unit-cell parameters were calculated using data from the current study. The unit-cell parameters a and c increase linearly whereas b decreases with larger RE cations, based on crystal radii. The unit-cell volumes increase linearly and the densities decrease linearly with larger RE cations. The average distances between the RE cations and the nearest O atoms increase with larger cations whereas the average distances of Mo—O and K—O do not show specific trends.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Acoustic Observations of the OSIRIS-REx Sample Return Capsule Re-Entry from Wendover Airport

The Origins, Spectral Interpretation, Resource Identification, and Security‐Regolith Explorer sample return capsule (SRC) re‐entered the Earth’s atmosphere at hypersonic speeds from interplanetary space on 24 September 2023. The current work reports on 18 ground‐based acoustic sensors deployed at Wendover Airport, the same location that the Genesis and Stardust SRC re‐entries were recorded. Four different sensors (Chaparral Physics, Gem, Wilson Engineering Research and Development [WERD], and RedVox) were deployed in close proximity to compare their performance. All the sensors captured an N‐wave signal associated with the SRC re‐entry shock wave followed by a broadband coda. The Chaparral Physics array served as the high‐fidelity reference measurement. The N‐wave signal had a peak‐to‐peak amplitude of 4.07 Pa with a fundamental frequency of 4.98 Hz from 167.5° measured clockwise from north, nearly perpendicular to the SRC trajectory. In addition, high coherence in the coda was shown to be associated reflections from the surrounding mountains. In general, the more economical sensors (Gem, WERD, and RedVox) produced results that were consistent with these observations and sensor specifications. Beamforming with these single sensors arranged as an array showed agreement with the high‐fidelity array to within a couple of degrees. Furthermore, the current high‐fidelity results were compared with the measurements during the Genesis and Stardust SRC re‐entries. All three entries produced a broadband fundamental peak at a frequency that was inversely related to the SRC diameter as well as evidence of reflections from the surrounding topography.

KC, Real J. [Oklahoma State University, Stillwater↗
NASA NTRS1972

Studies of the performance of W-Re type thermocouples.

The effect of exposure of bare-wire and BeO-insulated commercial W-Re thermocouple materials to high temperatures in gaseous environments was investigated. The temperature range of interest was primarily 2000 to 2400 K, and the investigations were confined to thermocouple wires of 0.25 mm diameter. Thermoelements were examined for metallurgical structural changes and chemical changes by conventional methods. In the temperature range of interest, grain growth was inhibited in the chemically doped W-3% Re alloy, and excellent room-temperature ductility was retained subsequent to the exposure. The compatibility of high purity (in excess of 99.8%), sintered BeO insulators with the thermoelements differed, depending upon whether the BeO-insulated thermoelement assemblies were self-heated electrically or heated in a furnace; in tests in argon environments, highly reliable performance occurred when the assemblies were heated in a furnace. BeO-insulated W-3% Re vs W-25% Re thermocouples, constructed with degassed and aged materials, exhibited drifts equivalent to about 3 mK/hr during 1000 hours of exposure at 2073 K in argon while in the presence of tantalum.

Burns, G. W.↗
NASA NTRS1995

RE J1255+266: Detection of an extremely bright EUV transient

During a pointed ROSAT observation in the direction of the Coma cluster of galaxies an exceptionally bright EUV source, RE J1255+266, was detected serendipitously. The source is located close to the Galactic North Pole, at b(sub II) is approximately or equal to 89 deg. Its observed EUV flux (62 - 110 eV) at the time of the detection was of order 7 x 10(exp -9) ergs/sq cm, making RE J1255+266 temporarily one of the brightest EUV sources on the sky. The EUV flare of RE J1255+266 has a light curve with a decay time of about 0.86 days. With respect to earlier non-detections, the source brightened by a factor of approximately 7000. Such a behavior has not been observed before. Thus, it is unclear what type of source RE J1255+266 might be. Up to now no positive identification with any known source could be obtained. Emission at the position of the source was previously only detected in the 1987 Green Bank radio continuum survey. Simultaneous observations with Compton Gamma Ray Observatory/Burst and Transient Source Experiment (CGRO/BATSE) resulted in non-detections of the source in the 8 - 50 keV energy range.

Dahlem, M.↗
NASA NTRS1995

Re-scheduling as a tool for the power management on board a spacecraft

The scheduling of events on board a spacecraft is based on forecast energy levels. The real time values of energy may not coincide with the forecast values; consequently, a dynamic revising to the allocation of power is needed. The re-scheduling is also needed for other reasons on board a spacecraft like the addition of new event which must be scheduled, or a failure of an event due to many different contingencies. This need of rescheduling is very important to the survivability of the spacecraft. In this presentation, a re-scheduling tool will be presented as a part of an overall scheme for the power management on board a spacecraft from the allocation of energy point of view. The overall scheme is based on the optimal use of energy available on board a spacecraft using expert systems combined with linear optimization techniques. The system will be able to schedule maximum number of events utilizing most energy available. The outcome is more events scheduled to share the operation cost of that spacecraft. The system will also be able to re-schedule in case of a contingency with minimal time and minimal disturbance of the original schedule. The end product is a fully integrated planning system capable of producing the right decisions in short time with less human error. The overall system will be presented with the re-scheduling algorithm discussed in detail, then the tests and results will be presented for validations.

Albasheer, Omar↗
NASA NTRS2000

Long-Term Cyclic Oxidation Behavior of Uncoated and Coated Re-108 and In-939 at 980 and 870 C

Very long-term cyclic oxidation behavior of Re108 and In939 with and without a protective coating was evaluated at 980 and 870 C, respectively. Re-108 and In-939 without a protective coating began to show a rapid weight loss at 3000 h due to scale spallation, indicating the need for an oxidation protective coating for longer than thousands of hours of oxidative life. NiAl-base coatings of a vapor phase aluminide (VPA), a pack aluminide (CODEP), and a slurry paint aluminide (SERMALOY J) were applied on Re-108 and In-939. The VPA and CODEP on Re-108 and all three coatings on In-939 showed excellent cyclic oxidation resistance out to 10,000 h. Coated alloys were annealed in an inert atmosphere to determine the loss of Al from the coating into the alloy substrate through diffusion. The Al loss from the coating through diffusion was twice as great as the Al loss through oxidation after 10,000 h of cyclic exposure. The oxidation life of VPA-coated Re-108 was estimated by calculating the amount of Al initially available for protective oxidation and the amount of Al lost through oxidation and diffusion.

Lee, K. N.↗
NASA NTRS2001

Trajectory Design and Control for the Compton Gamma Ray Observatory Re-Entry

The Compton Gamma Ray Observatory (CGRO) controlled re-entry operation was successfully conducted in June of 2000. The surviving parts of the spacecraft landed in the Pacific Ocean within the nominal impact target zone. The design of the maneuvers to control the trajectory to accomplish this re-entry presented several challenges. These challenges included the timing and duration of the maneuvers, propellant management, post-maneuver state determination, collision avoidance with other spacecraft, accounting for the break-up of the spacecraft into several pieces with a wide range of ballistic coefficients, and ensuring that the impact footprint would remain within the desired impact target zone in the event of contingencies. This paper presents the initial re-entry trajectory design and traces the evolution of that design into the maneuver sequence used for the re-entry. The paper also discusses the spacecraft systems and operational constraints imposed on the trajectory design and the required modifications to the initial design based on those constraints. Data from the reentry operation are also presented.

Hoge, Susan↗
NASA NTRS2002

Investigations of Control Surface Seals for Re-entry Vehicles

Re-entry vehicles generally require control surfaces (e.g., rudders, body flaps) to steer them during flight. Control surface seals are installed along hinge lines and where control surface edges move close to the vehicle body. These seals must operate at high temperatures and limit heat transfer to underlying structures to prevent them from overheating and causing possible loss of vehicle structural integrity. This paper presents results for thermal analyses and mechanical testing conducted on the baseline rudder/fin seal design for the X-38 re-entry vehicle. Exposure of the seals in a compressed state at the predicted peak seal temperature of 1900 F resulted in loss of seal resiliency. The vertical Inconel rudder/fin rub surface was re-designed to account for this loss of resiliency. Room temperature compression tests revealed that seal unit loads and contact pressures were below limits set to protect Shuttle thermal tiles on the horizontal sealing surface. The seals survived an ambient temperature 1000 cycle scrub test over sanded Shuttle tiles and were able to disengage and re-engage the tile edges during testing. Arc jet tests confirmed the need for seals in the rudder/fin gap location because a single seal caused a large temperature drop (delta T = 1710 F) in the gap.

Dunlap, Patrick H., Jr.↗
NASA NTRS2003

Re-Os Systematics and HSE Distribution in Metal from Ochansk (H4) Chondrite

Previous studies of the Re-Os systematics of chondrites have documented considerable variation in the Re/Os ratios of whole rock samples. For some whole rock chondrites, Re-Os systematics display large deviations from the primitive isochron that are considerably larger than deviations in other isotope systems. Possible interpretation of these facts is that the Re-Os system in chondrites is particularly sensitive to post-formation alteration processes, thus providing a useful tool to examine such processes. Significant variations that have been detected in highly siderophile element (HSE) patterns for ordinary chondrites support this conclusion. We report Re-Os isotope data for metal separates from the Ochansk H4 chondrite coupled with abundance data for Ru, Pd, Ir, and Pt, determined in the same samples by isotope dilution. We chose this meteorite mainly because it is an observed fall with minimal signs of weathering, and its low metamorphic grade (H4) and shock stage (S3).

Smoliar, M. I.↗