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DOE OSTI2026

Effects of Recovery Conditions and Aggregation Mechanisms on the Chemical and Physical Properties of Hybrid Poplar and Corn Stover Lignins

Heterogeneity in the physical properties and processing behavior of lignins recovered from biorefining process streams can hinder their effective utilization and industrial valorization. This work investigates lignin recovery by acidification from alkaline pretreatment liquors of varying sources (corn stover and hybrid poplar), compositions, solid contents, and incubation temperatures prior to filtration. Recovered lignins were characterized for filtration performance, mass yield, chemical composition, particle size and morphology, and color. A transition temperature was identified corresponding to marked shifts in lignin physical properties and was a function of the solid content and liquor source. Filtration below this temperature yielded slow-filtering, dark, brittle lignins with smoother particle surfaces, whereas precipitation above this threshold yielded fast-filtering, lighter, powdery lignins with rougher particle surfaces. The impact of temperature and concentration on universal cluster aggregation mechanisms was proposed to explain the differences between lignin particle properties and filtration behavior.

Aggregation↗

NASA NTRS1992

A comparison of superconductor and manganin technology for electronic links used in space mission applications

The electronic link connecting cryogenically cooled radiation detectors to data acquisition and signal processing electronics at higher temperatures contributes significantly to the total heat load on spacecraft cooling systems that use combined mechanical and cryogenic liquid cooling. Using high transition temperature superconductors for this link has been proposed to increase the lifetime of space missions. Herein, several YBCO (YBa2Cu3O7) superconductor-substrate combinations were examined and total heat loads were compared to manganin wire technology in current use. Using numerical solutions to the heat-flow equations, it is shown that replacing manganin technology with YBCO thick film technology can extend a 7-year mission by up to 1 year.

Caton, R.↗

NASA NTRS2003

Thermal Contributions to the Degradation of Ground Laboratory and Space Irradiated Teflon

The aluminized Teflon fluorinated ethylene propylene outer most layer of the multilayer insulation blankets on the Hubble Space Telescope has become embrittled resulting in severe on-orbit cracking. During the second servicing mission, a piece of aluminized fluorinated ethylene propylene was retrieved that had curled, exposing the back-surface aluminum to space. This extremely embrittled piece reached 200 C on-orbit, 150 C higher than the nominal temperature extreme. Therefore, experiments have been conducted to determine the effect of heating on the degradation of fluorinated ethylene propylene that has been irradiated in a ground laboratory facility or in space on Hubble Space Telescope. Samples of pristine, x-ray irradiated and Hubble Space Telescope retrieved fluorinated ethylene propylene were heat treated from 50 to 200 C at 25 C intervals in a high vacuum facility and tensile tested. Density measurements were also obtained. Results indicate that heating does not embrittle non-irradiated Teflon. However, there is a significant dependence of the embrittlement of irradiated Teflon on heating temperature, with near complete loss of elongation at 100 C and higher. Rate of degradation changes, which were consistent with the glass transition temperature for fluorinated ethylene propylene, were present in the data. The results support chain scission as the primary mechanism of degradation of fluorinated ethylene propylene on Hubble Space Telescope, and indicate the significance of the on-orbit temperature of fluorinated ethylene propylene with respect to its degradation in the space environment.

deGroh, Kim K.↗

NASA NTRS2004

In situ Pulsed Laser Deposition of C-Axis Oriented MgB2 Films and Their Characterization

The recent discovery of an intermetallic superconductor MgB2 has renewed interest in the area of superconductivity not only because of fundamental understanding of superconductivity but also due to its potential applicability in devices such as thermal detectors. Considerable amount of research has been devoted to obtain MgB2 films by an all in situ growth technique. We have grown MgB2 thin films by an all in situ pulsed laser deposition process from pure B and Mg targets. Ultrathin layers of B and Mg were deposited in a multilayer configuration. Hundreds of such Mg-B bilayers with a capping Mg layer on the top were deposited on sapphire substrate. These depositions were done in high vacuum (approx. 10(exp -7) Torr) and at room temperature. After deposition, such a configuration was annealed at high temperature for a short time in a forming gas (4% H2 in Ar). The best films, obtained by this procedure, showed superconducting transition temperature approx. 30 K. These films have been characterized by x-ray diffraction, Rutherford Backscattering Spectrometry, AC susceptibility-, resistivity- (with and without magnetic field) and 1/f noise-measurements. The physical properties of these films will be presented and discussed.

Shinde, Sanjay↗

DOE OSTI2025

Structural Phase Separation and Enhanced Superconductivity in La 1.875 Ba 0.125 CuO 4 Under Uniaxial Strain

Strain engineering has attracted significant attention in recent years due to its capability in tuning lattice and electronic structures of quantum materials. Using moderate uniaxial compressive strain, structural phase separation is induced in the low-temperature phase of x = 1/8 La 2-x Ba x CuO 4 (LBCO) single crystals. These structures are low temperature tetragonal (LTT), low temperature less orthorhombic (LTLO), and a plastically deformed nano-domain structure (PDNS), comprised of few-nanometer-sized orthorhombic domains within an amorphous matrix. These three structures exhibit distinct superconducting behaviors. The volume fraction of the LTT structure is suppressed with increasing strain, while its superconducting transition temperature increases and broadens. The LTLO structure exhibits a sharp superconducting transition above 32 K, which increases up to ≈ 36 K at maximum strain. The PDNS phase exhibits a very broad superconducting transition and persists even after removing the strain. This study illustrates the sensitivity of superconductivity to the structure of the LBCO sample near its stripe instability.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

High-Temperature-Performance Cyanate Ester Composites with Carboranes

Cyanate ester (CE) is an important class of materials among high-temperature performance thermosets. It is used in aerospace launch vehicles, heat sinks, booms, and trusses of satellites etc. due to its high glass transition temperatures (>220°C), excellent thermal stability, and low flammability. Current approaches to improve the thermal stability of CE include incorporation of siloxanes or phosphorus- based flame retardants (PFRs). In this work, we have explored boron-based hydroxy (PD) and epoxy (EP) functionalized carborane additives to improve the thermal properties of CE. Carborane fillers were solvent blended at various mass loadings in the resin and cured to study their effect on thermal properties. PD and EP carboranes react with CE to form iminocarbonate and oxazolidinone linkages respectively. Cure kinetics studies at different wt% loadings explained that carboranes catalyze the curing reaction by reducing curing activation energy by about 54% and 26% for 10 wt% loadings of PD and EP carboranes respectively. In addition, carborane-filled cyanate ester (CE) nanocomposites demonstrate an exceptionally high thermal stability as compared to the pristine resin in air and inert environment. Our thermogravimetric analysis (TGA) experiments show that the ultimate char yield of the resin can be increased from 0% to as high as 76% and 82% with 30 wt% PD and EP carborane loading respectively at 1000 °C in air. The initial degradation temperature T d;5 of the composites decreased with increasing carborane loadings in both air and argon. For instance, T d;5 for CE was 465 and 471.6 °C in argon and air while that for P20 was 437.4 and 452.1 °C. Modulated TGA studies gave evidence of the effect of carboranes on degradation kinetics and the mechanism of the resin in air and inert environment. The effect of bonding between carboranes and CE at various loadings on the thermal expansion of the matrix was also studied using Thermomechanical Analyzer (TMA). PD carborane reduced the T g for P20 to about 225 °C while CE had T g >350 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1974

Hydrogen adsorption and diffusion, and subcritical-crack growth in high-strength steels and nickel base alloys

Coordinated studies of the kinetics of crack growth and of hydrogen adsorption and diffusion were initiated to develop information that is needed for a clearer determination of the rate controlling process and possible mechanism for hydrogen enhanced crack growth, and for estimating behavior over a range of temperatures and pressures. Inconel 718 alloy and 18Ni(200) maraging steel were selected for these studies. 18Ni(250) maraging steel, 316 stainless steel, and iron single crystal of (111) orientation were also included in the chemistry studies. Crack growth data on 18Ni(250) maraging steel from another program are included for comparison. No sustained-load crack growth was observed for the Inconel 718 alloy in gaseous hydrogen. Gaseous hydrogen assisted crack growth in the 18Ni maraging steels were characterized by K-independent (Stage 2) extension over a wide range of hydrogen pressures (86 to 2000 torr or 12 kN/m2 to 266 kN/m2) and test temperatures (-60 C to +100 C). The higher strength 18Ni(250) maraging steel was more susceptible than the lower strength 200 grade. A transition temperature was observed, above which crack growth rates became diminishingly small.

Wei, R. P.↗

NASA NTRS1986

Room temperature deposition of superconducting NbN for superconductor-insulator-superconductor junctions

The deposition of stoichiometric B1-crystal-structure (111) NbN films on glass or sapphire substrates by reactive dc magnetron sputtering is reported. High-purity Ar-N2 mixtures are used in the apparatus described by Thakoor et al. (1985), and typical deposition parameters are given as background pressure about 10 ntorr, voltage -325 V, current 1 A, deposition rate 1.35 nm/s, film thickness 500 nm, P(Ar) 5-17 mtorr, initial P(N2) 2-6 mtorr, and room temperature. The N2 consumption-injection characteristics are studied and found to control NbN formation using well-conditioned Nb targets. Films with transition temperatures 15-16 K are obtained at P(Ar) = 12.9 + or - 0.2 mtorr and P(N2) = 3.7 + or - 0.1 mtorr. SIS junctions of area about 0.001 sq cm fabricated using the NbN films are shown to have I-V characteristics with nonlinearity parameter about 110 and NbN superconducting-gap parameter Delta = about 2.8 meV.

Thakoor, S.↗

NASA NTRS1990

Crystallization behavior and properties of BaO-Al2O3-2SiO2 glass matrices

Glass of stoichiometric celsian composition, BaO-Al2O3-2SiO2, is a potential glass-ceramic matrix for high-temperature composites. The glass has a density of 3.39 g/cu cm, thermal expansion coefficient of 6.6 x 10(exp -6)/deg C glass transition temperature of 910 C, and dilatometric softening point of 925 C. On heat treatment, only hexacelsian crystallized out on the surface, but both celsian and hexacelsian were present in the bulk. Effects of cold isostatic pressing (CIP), sintering, and hot pressing, in the presence and absence of an additive, on the formation of the celsian phase in the glass were studied. CIP'ed samples, after appropriate heat treatments, always crystallized out as celsian whereas the presence of 5 to 10 weight percent of an additive was necessary for formation of celsian in sintered as well as hot pressed specimens. Green density increased with CIP'ing pressure but had no effect on sintered density. Hot pressing resulted in fully dense samples.

Drummond, Charles H., III↗

NASA NTRS1992

C-band superconductor/semiconductor hybrid field-effect transistor amplifier on a LaAlO3 substrate

A single-stage C-band superconductor/semiconductor hybrid field-effect transistor amplifier was designed, fabricated, and tested at 77 K. The large area (1 inch x 0.5 inches) high temperature superconducting Tl-Ba-Ca-Cu-O (TBCCO) thin film was rf magnetron sputtered onto a LaAlO3 substrate. The film had a transition temperature of about 92 K after it was patterned and etched. The amplifier showed a gain of 6 dB and a 3 dB bandwidth of 100 MHz centered at 7.9 GHz. An identical gold amplifier circuit was tested at 77 K, and these results are compared with those from the hybrid amplifier.

Nahra, J. J.↗

NASA NTRS2004

High Temperature Transfer Molding Resins: Preliminary Composite Properties of PETI-375

As part of an ongoing effort to develop materials for resin transfer molding (RTM) of high performance/high temperature composites, a new phenylethynyl containing imide designated as PETI-375 has been under evaluation. PETI-375 was prepared using 2,3,3 ,4 - biphenyltetracarboxylic dianhydride (a-BPDA), 1,3-bis(4-aminophenoxy)benzene and 2,2 - bis(trifluoromethyl)benzidine and endcapped with 4-phenylethynylphthalic anhydride. This material exhibited a stable melt viscosity of 0.1-0.4 Pa sec at 280 C. High quality, void-free laminates were fabricated by high temperature RTM using unsized T-650 carbon fabric and evaluated. After curing for 1 hour at 371 C, the laminates exhibited a glass transition temperature of approx. 375 C by thermomechanical analysis. The laminates were essentially void and microcrack free as evidenced by optical microscopic examination. The chemistry, physical, and composite properties of PETI-375 will be discussed.

Connell, J. W.↗

NASA NTRS2001

Evaluation of Temperature and Material Combinations on Several Lubricants for Use in the Geostationary Operational Environmental Satellite (GOES) Mission Filter Wheel Bearings

A bearing test apparatus was used to investigate lubricant degradation rates and elastohydrodynamic transition temperatures for several perfluoropolyether (Krytox) formulations, a pentasilahydrocarbon, and a synthetic hydrocarbon (Pennzane 2001 A) in an MPB 1219 bearing, which is used in the geostationary operational environmental satellite (GOES) mission filter wheel assembly. Test conditions were the following: 1000-hr duration, 75 C, 20 lb axial load, vacuum level less than 1 x 10(exp -6) Torr, and a 600-rpm rotational speed. Baseline tests were performed using unformulated Krytox 143AB, the heritage lubricant. Krytox additive formulations showed small reductions in degradation rate. Krytox GPL-105, a higher viscosity version, yielded the least amount of degradation products. Both the silahydrocarbon and Pennzane 2001A showed no signs of lubricant degradation and had ample amounts of free oil at test conclusion.

Jansen, Mark J.↗

DOE OSTI2020

Effects of tacticity and chiral center-to-dipole distance on mesogen-free liquid crystalline self-assembly of sulfonyl-containing comb-like polymers

In this report, new approaches were implemented to achieve novel ferroelectric liquid crystalline self-assembly in mesogen-free comb-like isotactic polyoxypropylenes (iPOPs) bearing mono- or di-sulfonyl groups, which have potential to exhibit high spontaneous polarization for applications in advanced electronic devices. iPOPs with n-alkylsulfonylpentylthioether side chains (iPOP-SC 5 SO 2 C n , where C n is the alkyl tail with n being either 12 or 8) were prepared via a post-polymerization substitution reaction from isotactic poly[(R)-(–)-epichlorohydrin]. Here, the effects of main-chain tacticity, chiral center-to-dipole distance, number of sulfonyl dipoles per side chain, and n-alkyl tail length on the liquid crystalline self-assembly behavior were investigated by comparing iPOPs with their atactic counterparts. First, when the sulfonyl dipole was placed far away from the chiral center in iPOP-SC 5 SO 2 C n compared with our previously reported isotactic polyethers with n-alkylsulfonyl side chains (iPOP-SO 2 C n ), the dipole–dipole interactions among the side chains decreased, which led to more liquid crystalline phases. Smectic E (SmE) and A (SmA) phases were observed after crystal melting; however, the main-chain chiral center was found to have an insignificant effect on the liquid crystalline assembly when compared to the atactic samples. Second, the longer C n tails increased the transition temperatures as a result of stronger van der Waals interactions. Third, after the thioether linkage in the side chain was oxidized into the sulfonyl group, the chiral center–dipole and dipole–dipole interactions in the resultant polymers (i.e., iPOP-SO 2 C 5 SO 2 C n ) enhanced. As a result, the liquid crystalline phase transitions (i.e., crystal → SmE → SmA → I) were pushed to higher temperatures. The knowledge gained in this study will help us further design and achieve the ferroelectric smectic C* phase in mesogen-free comb-like sulfonylated liquid crystalline polymers.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Absence of E 2 g Nematic Instability and Dominant A 1 g Response in the Kagome Metal CsV 3 Sb 5

Ever since the discovery of the charge density wave (CDW) transition in the kagome metal CsV 3 Sb 5 , the nature of its symmetry breaking has been under intense debate. While evidence suggests that the rotational symmetry is already broken at the CDW transition temperature ( T CDW ), an additional electronic nematic instability well below T CDW has been reported based on the diverging elastoresistivity coefficient in the anisotropic channel ( m E 2 g ). Verifying the existence of a nematic transition below T CDW is not only critical for establishing the correct description of the CDW order parameter, but also important for understanding low-temperature superconductivity. Here, we report elastoresistivity measurements of CsV 3 Sb 5 using three different techniques probing both isotropic and anisotropic symmetry channels. Contrary to previous reports, we find the anisotropic elastoresistivity coefficient m E 2 g is temperature independent, except for a step jump at T CDW . The absence of nematic fluctuations is further substantiated by measurements of the elastocaloric effect, which show no enhancement associated with nematic susceptibility. On the other hand, the symmetric elastoresistivity coefficient m A 1 g increases below T CDW , reaching a peak value of 90 at T * = 20 K . Our results strongly indicate that the phase transition at T * is not nematic in nature and the previously reported diverging elastoresistivity is due to the contamination from the A 1 g channel. Published by the American Physical Society 2024

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

In Situ High-Temperature Structural Analysis of High-Entropy Rare-Earth Sesquioxides

High-entropy rare-earth (RE) sesquioxides (RE 2 O 3 ) containing five cations in equimolar amounts have been investigated for a variety of applications, but little is known about their polymorphic behavior and coefficient of thermal expansion. Here, in this work, we evaluate the effect of the average ionic radius (AIR) on the polymorphism of high-entropy RE 2 O 3 . Powder samples of compositions 1 (Lu,Y,Ho,Nd,La) 2 O 3 (AIR = 0.938 Å) and 2 (Gd,Eu,Sm,Nd,La) 2 O 3 (AIR = 0.982 Å) were synthesized via a wet chemical method, and bead samples were prepared for aerodynamic levitation by melting the powders in a copper hearth. Structural transitions were monitored upon cooling from the melt to 1000 °C via in situ X-ray diffraction on aerodynamically levitated samples. The phase evolution was liquid, hexagonal H-type, and monoclinic B-type for composition 1 and liquid, cubic X-type, H-type, and B-type for composition 2. Based on their AIR, the general polymorphic transformations of the high-entropy RE 2 O 3 follow the trend of single-RE RE 2 O 3 , but the transition temperatures differ from those of single-RE RE 2 O 3 . The coefficient of thermal expansion values of the B-type phase of compositions 1 and 2 are similar to those of Gd 2 O 3 and previously published high-entropy RE 2 O 3 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Magnetism and magnetotransport in the kagome antiferromagnet Mn 3 Ge

We perform classical Monte Carlo and stochastic Landau-Lifshitz-Gilbert simulations to study the temperature-dependent magnetism of the kagome antiferromagnet Weyl metal Mn3Ge, and we find that a long-range chiral order sets in at a transition temperature well below the Neel temperature (T N ). Based on the crystalline symmetries imposed by the chiral magnetic order, we argue for the presence of multiple isoenergetic Weyl nodes (nodes that are at the same energy and with a congruent Fermi surface around them) near the chemical potential. Using the semiclassical Boltzmann equations, we show that the combined contribution to the net longitudinal magnetoconductance (LMC) and the planar Hall conductance (PHC) from tilted Weyl nodes can lead to signatures that are qualitatively distinct from that of a single pair of Weyl nodes. In particular, we show that magnetic orders with different chiralities can give rise to different periods in LMC and PHC as a function of the in-plane magnetic field direction. As a result, this is ultimately related to differences in the symmetry-imposed constraints on the Weyl nodes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Pairing properties of the $t$–$t$'–$t$"–$J$ model

We study the pairing properties of the two-dimensional t–t'–t"–J model, where t' and t" are second and third neighbor hoppings, at a doping level x ≈ 0.1. Recent studies of the t–t'–J model find strong pairing for t' > 0, associated with electron doping, but an absence of pairing for t'<0, associated with hole doping. This is in contrast to the cuprates, where the highest transition temperatures appear for hole doping. Model parametrizations for the cuprates estimate a t" comparable to t', which, in principle, might fix this discrepancy. However, we find that it does not; we observe a suppression of pairing for the hole-doped system (t' < 0,t" > 0), while for the electron-doped system (t' > 0,t" < 0) d-wave pairing is robust. As a result, extended hoppings appear to be insufficient to make the one-band t–t'–J model capable of describing the pairing in the hole-doped system.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Defect-induced electronic smectic state at the surface of nematic materials

Due to the intertwining between electronic nematic and elastic degrees of freedom, lattice defects and structural inhomogeneities commonly found in crystals can have a significant impact on the electronic properties of nematic materials. Here, we show that defects commonly present at the surface of crystals generally shift the wave-vector of the nematic instability to a non-zero value, resulting in an incommensurate electronic smectic phase. Such a smectic state onsets above the bulk nematic transition temperature and is localized near the surface of the sample. We argue that this effect may explain not only recent observations of a modulated nematic phase in iron-based superconductors, but also several previous puzzling experiments that reported signatures consistent with nematic order before the onset of a bulk structural distortion.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗