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DOE OSTI2025

Aqueous Zr/Hf IV ‐Oxo Cluster Speciation and Separation

Abstract Many industrial separations of chemically‐similar elements are achieved by solvent extraction, exploiting differences in speciation and solubility across aqueous‐organic interfaces. We recently identified [OM 4 (OH) 6 (SCN) 12 ] 4− (OM 4 , M=Zr/Hf IV ) tetrahedral oxoclusters as the main species in industrial processes that produce nuclear‐grade Zr and Hf from crude ore. However, isostructural/isoelectronic OM 4 ‐oxoclusters do not explain selective extraction of Hf into the organic phase. Here we have characterized heterometal Hf−Zr clusters in solution and the solid‐state yielding key information about their fundamentally different chemistry that engenders separation. Clusters prepared with both ammonium (industrial process) and tetramethylammonium counter cations revealed that 1) heterometal clusters (instead of a mixture of homometal clusters) assemble, and 2) Hf‐rich OM 4 selectively precipitates over Zr‐rich OM 4 , providing a separation process that does not require an organic extractant. Mass spectrometry, small‐angle X‐ray scattering, solution‐state 1 H nuclear magnetic resonance (NMR) spectroscopy, and solid‐state 17 O NMR evidence both mixed‐metal speciation and selective Hf‐precipitation. Raman spectroscopy suggests greater Zr‐ligand lability than Hf‐ligand lability, consistent with higher aqueous solubility of Zr‐rich clusters, enabling both extraction and precipitation‐based separation. Fundamentally, we also identify a key difference between these chemically similar elements that has enabled diversification of Zr‐polyoxocation chemistry over the last decade, while Hf‐polyoxocation chemistry lags.

Roseborough, Alexander [Department of Chemistry Or↗

DOE OSTI2024

A New Class of Oxyhalide Solid Electrolytes NaNbCl 6‐2x O x for Solid‐state Sodium Batteries

Abstract Sodium‐based batteries are gaining momentum due to the abundance and lower cost of sodium compared to lithium. Solid‐state sodium batteries can also provide further safety advantages. However, sodium‐based solid‐state electrolytes (SSEs) that meet all the rigorous requirements, such as high ionic conductivity, oxidative stability with the cathode, and ease of processability, are lacking. We present here a new class of sodium‐based oxyhalide electrolytes NaNbCl 6‐2x O x with a facile mechanochemical synthesis. The oxyhalide NaNbCl 4 O exhibits close to two orders of magnitude higher ambient‐temperature sodium‐ion conductivity (1.03×10 −4 S cm −1 ) compared to the halide counterpart NaNbCl 6 (3×10 −6 S cm −1 ). Structural motifs unique to the oxygen content in NaNbCl 6‐2x O x are identified with 23 Na and 93 Nb magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy and x‐ray diffraction (XRD). Solid‐state sodium batteries assembled with NaNbCl 4 O electrolyte and the cobalt‐ and nickel‐free layered Na 0.70 Fe 0.3 Mn 0.65 Al 0.05 O 2 cathode exhibit a maximum discharge capacity of 155 mAh g −1 with good cycle life at ambient temperature.

Kmiec, Steven↗

DOE OSTI2024

A New Class of Oxyhalide Solid Electrolytes NaNbCl 6‐2x O x for Solid‐state Sodium Batteries

Kmiec, Steven↗

DOE OSTI2016

Dual analyzer system for surface analysis dedicated for angle-resolved photoelectron spectroscopy at liquid surfaces and interfaces

The investigation of liquid surfaces and interfaces with the powerful toolbox of ultra-high vacuum (UHV)-based surface science techniques generally has to overcome the issue of liquid evaporation within the vacuum system. In the last decade, however, new classes of liquids with negligible vapor pressure at room temperature—in particular, ionic liquids (ILs)—have emerged for surface science studies. It has been demonstrated that particularly angle-resolved X-ray Photoelectron Spectroscopy (ARXPS) allows for investigating phenomena that occur at gas-liquid and liquid-solid interfaces on the molecular level. The results are not only relevant for IL systems but also for liquids in general. In all of these previous ARXPS studies, the sample holder had to be tilted in order to change the polar detection angle of emitted photoelectrons, which restricted the liquid systems to very thin viscous IL films coating a flat solid support. We now report on the concept and realization of a new and unique laboratory “Dual Analyzer System for Surface Analysis (DASSA)” which enables fast ARXPS, UV photoelectron spectroscopy, imaging XPS, and low-energy ion scattering at the horizontal surface plane of macroscopically thick non-volatile liquid samples. It comprises a UHV chamber equipped with two electron analyzers mounted for simultaneous measurements in 0° and 80° emission relative to the surface normal. The performance of DASSA on a first macroscopic liquid system will be demonstrated.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS1978

Penetration depth at green wavelengths in turbid waters

A laboratory and field measurement program was conducted to determine apparent remote sensing penetration depths at a wavelength of 520 nm. Tests were made for various types of sediments under controlled conditions in a laboratory. Field tests were conducted in several different water bodies over a wide range of solar elevation angles. Laboratory results indicate that apparent penetration depth is significantly influenced by mineral content and/or size of suspended sediments. Field measurements show wide variation in apparent penetration depth, even when suspended solids concentration is nearly constant. Apparent penetration depth does not appear to be a strong function of solar elevation angle so long as the water mixture remains constant.

Whitlock, C. H.↗

NASA NTRS1997

Use of Variable Angle Spectroscopic Ellipsometry in Order to Determine Contaminant Optical Properties

In order to measure contaminant levels found in the manufacture of the Redesigned Solid Rocket Motor (RSRM), optical properties of the contaminants are needed to develop standards for calibration purposes. Specific to our efforts is the determination of the complex index of refraction for a hydrocarbon mixture and a commercial methyl siloxane. Using ellipsometric measurements with multiple angles of incident and a range of wavelengths in the near infrared a determination of the index of refraction and the extinction coefficient were made for the contaminants. This paper will present the optical techniques and modeling approach used to determine these optical constants of the hydrocarbon mixture and the methyl siloxane studied.

Hughes, C.↗

NASA NTRS1973

Analytical study on a two-dimensional plane of the off-design flow properties of tandem-bladed compressor stators

The flow characteristics of several tandem bladed compressor stators were analytically evaluated over a range of inlet incidence angles. The ratios of rear-segment to front-segment chord and camber were varied. Results were also compared to the analytical performance of a reference solid blade section. All tandem blade sections exhibited lower calculated losses than the solid stator. But no one geometric configuration exhibited clearly superior characteristics. The front segment accepts the major effect of overall incidence angle change. Rear- to front-segment camber ratios of 4 and greater appeared to be limited by boundary-layer separation from the pressure surface of the rear segment.

Sanger, N. L.↗

DOE OSTI2017

Synchrotron X-ray studies of model SOFC cathodes, part II: Porous powder cathodes

Infiltrated La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ (LSCF) sintered porous powder cathodes for solid oxide fuel cells have been investigated by synchrotron ultra-small angle x-ray scattering (USAXS). Here, we demonstrated that atomic layer deposition (ALD) is the method for a uniform coating and liquid-phase infiltration for growing nanoscale particles on the porous LSCF surfaces. The MnO infiltrate, grown by ALD, forms a conformal layer with a uniform thickness throughout the pores evidenced by USAXS thickness fringes. The La 0.6 Sr 0.4 CoO 3 (LSC) and La 2 Zr 2 O 7 (LZO) infiltrates, grown by liquid-phase infiltration, were found to form nanoscale particles on the surfaces of LSCF particles resulting in increased surface areas. In conclusion, impedance measurements suggest that the catalytic property of LSC infiltrate, not the increased surface area of LZO, is important for increasing oxygen reduction activities.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Direct Determination of Hydroxymethyl Conformations of Plant Cell Wall Cellulose Using 1 H Polarization Transfer Solid-State NMR

In contrast to the well-studied crystalline cellulose of microbial and animal origins, cellulose in plant cell walls is disordered due to its interactions with matrix polysaccharides. Plant cell wall (PCW) is an undisputed source of sustainable global energy; therefore, it is important to determine the molecular structure of PCW cellulose. The most reactive component of cellulose is the exocyclic hydroxymethyl group: when it adopts the tg conformation, it stabilizes intrachain and interchain hydrogen bonding, while gt and gg conformations destabilize the hydrogen-bonding network. So far, information about the hydroxymethyl conformation in cellulose has been exclusively obtained from 13 C chemical shifts of monosaccharides and oligosaccharides, which do not reflect the environment of cellulose in plant cell walls. Here, we use solid-state Nuclear Magnetic Resonance (ssNMR) spectroscopy to measure the hydroxymethyl torsion angle of cellulose in two model plants, by detecting distance-dependent polarization transfer between H4 and H6 protons in 2D 13 C– 13 C correlation spectra. We show that the interior crystalline portion of cellulose microfibrils in Brachypodium and Arabidopsis cell walls exhibits H4–H6 polarization transfer curves that are indicative of a tg conformation, whereas surface cellulose chains exhibit slower H4–H6 polarization transfer that is best fit to the gt conformation. Joint constraints by the H4–H6 polarization transfer curves and 13 C chemical shifts indicate that it is unlikely for interior cellulose to have a significant population of the gt and gg conformation mixed with the tg conformation, while surface cellulose may adopt a small percentage of the gg conformation. These results provide new constraints to the structure and matrix interactions of cellulose in plant cell walls, and represent the first direct determination of a torsion angle in an important noncrystalline carbohydrate polymer.

09 BIOMASS FUELS↗

DOE OSTI2020

The Role of the Organic Solvent Polarity in Isolating Uranyl Peroxide Capsule Fragments

Uranyl peroxide capsules are a fascinating class of polyoxometalates (POMs), discovered only in the 21st century. Understanding the reactivity between peroxide, alkali cations, and uranyl in alkaline solutions is important in nuclear science disciplines including mineralogy, nuclear energy, and legacy nuclear wastes. In this work, we have developed a general procedure to isolate different fragments of the uranyl-peroxide POM capsules, using organic solvents to partially remove K + salts from crude solids of the monomer building block UO 2 (O 2 ) 3 4– (K–U 1 ), leading to stabilization of these reactive fragments. Higher polarity organic solvents remove more K + salts from the crude solid, owed to higher solubility, resulting in more extensive linking of uranyl peroxide building units. By this strategy we have isolated and structurally characterized a dimer K 6 [(UO 2 ) 2 (O 2 ) 4 (OH) 2 ]·7H 2 O (K–U 2 ) and a hexamer face frequently observed in the capsules, K 12 [(UO 2 ) 6 (O 2 ) 9 (OH) 6 ]$·x$H 2 O(K–U 6 ). Comparing experimental and computed Raman spectra shows that these intermediates crystallize by a solid-to-solid transformation, via polymerization of the monomer building block. By small-angle X-ray scattering (SAXS), we track the conversion of the fragments to POM capsules; the reaction rate increases from K–U 1 (days) < K–U 2 (hours) < K–U 6 (instantaneous). This study provides a general synthetic procedure to isolate metastable uranyl peroxide oligomers and control the oligomerization, which will be later applied to systems with the heavier alkalis that are even less stable.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

Measuring the Degree of Crystallinity in Semicrystalline Regioregular Poly(3-hexylthiophene)

By using a combination of wide-angle X-ray diffraction (WAXD), mass density, and 13 C solid-state nuclear magnetic resonance (NMR) measurements, a quantification of the absolute degree of crystallinity in regioregular poly(3-hexylthiophene) (rr-P3HT) is presented. A regiorandom P3HT (rra-P3HT), lacking long-range order, was used to separate the crystalline contribution from the total scattering in WAXD, thus yielding degrees of crystallinity in the range of 47–56% at room temperature for three different rr-P3HTs. For the same rr-P3HT with identical processing history, NMR yields degrees of crystallinity that are consistently ~10% greater than that obtained by WAXD, which can only be explained by ordered chain segments in the amorphous phase. NMR results also suggest that rra-P3HT contains weakly ordered chain segments, which likely contribute to an underestimation of degree of crystallinity when determined from mass density measurements, if rra-P3HT is used to approximate a fully amorphous P3HT. The results shown in this study provide direct proof of three different types of P3HT chain segments: crystallites (i.e., long-range ordered chain packing), amorphous phase (i.e., disordered chain packing), and short-range ordered chain packing embedded in the amorphous phase. Here, the presence of the short-range ordered chain packing is particularly important when correlating the morphology to macroscopic charge transport properties in P3HT-based devices. In general, those locally ordered chain segments, though not constituting a distinct phase, are believed to be of critical importance in determining the transport characteristics of conjugated semiconducting polymers with or without a distinct crystalline phase present.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Supported Aluminum Catalysts for Olefin Hydrogenation

Three-coordinate alkylaluminum sites were developed on a catechol-containing porous organic polymer support (CatPOP A2B1). The CatPOP-based alkylaluminum sites were characterized by solid-state attenuated total reflectance IR spectroscopy, 1H and 27Al magic-angle-spinning NMR spectroscopy, pair-distribution function X-ray absorption spectroscopy, and elemental analysis. The low-coordinate organoaluminum sites can hydrogenate and isomerize a range of mono- and disubstituted alkenes and alkynes under mild conditions (75–100 °C, 5–14 bar H2, 20 h). Results of experimental and computational mechanistic investigations suggest a heterolytic mechanism for the observed hydrogenation–isomerization activity.

alkene hydrogenation↗

DOE OSTI2015

Sealed rotors for in situ high temperature high pressure MAS NMR

Magic angle spinning (MAS) nuclear magnetic resonance (NMR) investigations on heterogeneous samples containing solids, semi-solids, liquid and gases or a mixture of them under non-conventional conditions of a combined high pressure and high temperature, or cold temperature suffer from the unavailability of a perfectly sealed rotor. Here, we report the design of reusable and perfectly-sealed all-zircornia MAS rotors. The rotors are easy to use and are suitable for operation temperatures from below 0 to 250 °C and pressures up to 100 bar. As an example of potential applications we performed in situ MAS NMR investigations of AlPO₄-5 molecular sieve crystallization, a kinetic study of the cyclohexanol dehydration reaction using 13C MAS NMR, and an investigation of the metabolomics of intact biological tissue at low temperature using 1H HR-MAS NMR spectroscopy. The in situ MAS NMR experiments performed using the reported rotors allowed reproduction of the results from traditional batch reactions, while offering more detailed quantitative information at the molecular level, as demonstrated for the molecular sieve synthesis and activation energy measurements for cyclohexanol dehydration. The perfectly sealed rotor also shows promising application for metabolomics studies using 1H HR-MAS NMR.

36 MATERIALS SCIENCE↗

NASA NTRS1975

An investigation in the NASA MSFC 14-inch trisonic wind tunnel to determine the pressure distribution over the components of a 0.004 scale version of the Rockwell MCR 0074 baseline shuttle ascent configuration (IA32F), volume 1

Data were obtained for Mach numbers from 0.6 to 3.48, angles of attack from -10 to 10 degrees, and angles of sideslip from -10 to 10 degrees at zero angle of attack. Also, -4 and 4 degrees sideslip were run for an angle of attack of -5 and 5 degrees. Aerodynamic configurations of the solid rocket motors, external tank, and orbiter are shown. Graphs of plotted pressure data (pressure coefficients) for the external tank and solid rocket motors are given. A description of the test facility is included.

Ramsey, P. E.↗

NASA NTRS2006

Low-Cost Propellant Launch From a Tethered Balloon

A document presents a concept for relatively inexpensive delivery of propellant to a large fuel depot in low orbit around the Earth, for use in rockets destined for higher orbits, the Moon, and for remote planets. The propellant is expected to be at least 85 percent of the mass needed in low Earth orbit to support the NASA Exploration Vision. The concept calls for the use of many small ( 10 ton) spin-stabilized, multistage, solid-fuel rockets to each deliver 250 kg of propellant. Each rocket would be winched up to a balloon tethered above most of the atmospheric mass (optimal altitude 26 2 km). There, the rocket would be aimed slightly above the horizon, spun, dropped, and fired at a time chosen so that the rocket would arrive in orbit near the depot. Small thrusters on the payload (powered, for example, by boil-off gases from cryogenic propellants that make up the payload) would precess the spinning rocket, using data from a low-cost inertial sensor to correct for small aerodynamic and solid rocket nozzle misalignment torques on the spinning rocket; would manage the angle of attack and the final orbit insertion burn; and would be fired on command from the depot in response to observations of the trajectory of the payload so as to make small corrections to bring the payload into a rendezvous orbit and despin it for capture by the depot. The system is low-cost because the small rockets can be mass-produced using the same techniques as those to produce automobiles and low-cost munitions, and one or more can be launched from a U.S. territory on the equator (Baker or Jarvis Islands in the mid-Pacific) to the fuel depot on each orbit (every 90 minutes, e.g., any multiple of 6,000 per year).

Wilcox, Brian↗

DOE OSTI2024

Evaporation from thin porous Coatings: Pore size effects and predictive equation for homogeneous coatings

Evaporation of small water droplets on solids is hindered because surface tension pulls the droplet into a spherical cap that has a small perimeter. Our solution is to coat a solid with a very thin, porous layer into which the droplet flows to create a large-area disk with concomitant high rate of evaporation. We investigate evaporation by varying factors that have not been previously considered: pore size and distribution, contact angle, temperature, and relative humidity (RH). A larger pore size resulted in faster evaporation, which we explain through faster transport within the coating. Even faster evaporation occurred for a bilayer structure with small particles on the air side and larger particles on the solid side. Further, the water advancing contact angle had an insignificant effect in the range from < 10° through to 60°. Our results for different pore sizes, temperature, humidity, and contact angle all collapse onto a single curve when appropriately normalized. This validates an equation that can be used for the evaporation from a homogeneous coating that depends only one empirical factor and the droplet volume. Since the volume is often user-controlled, we envisage that this equation can be used to predict evaporation and guide design of fast-drying coatings.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1979

Landsat test of diffuse reflectance models for aquatic suspended solids measurement

Landsat radiance data were used to test mathematical models relating diffuse reflectance to aquatic suspended solids concentration. Digital CCT data for Landsat passes over the Bay of Fundy, Nova Scotia were analyzed on a General Electric Co. Image 100 multispectral analysis system. Three data sets were studied separately and together in all combinations with and without solar angle correction. Statistical analysis and chromaticity analysis show that a nonlinear relationship between Landsat radiance and suspended solids concentration is better at curve-fitting than a linear relationship. In particular, the quasi-single-scattering diffuse reflectance model developed by Gordon and coworkers is corroborated. The Gordon model applied to 33 points of MSS 5 data combined from three dates produced r = 0.98.

Munday, J. C., Jr.↗

DOE OSTI2015

Mesoscale evolution of voids and microstructural changes in HMX-based explosives during heating through the β-δ phase transition

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensive microstructural damage resulting from the temperature cycle and solid-state phase transition.

36 MATERIALS SCIENCE↗