Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “phase change composite”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,189 records · Page 66

From Coherence to Function: Exploring the Connection in Chemical Systems

The role of quantum mechanical coherences or coherent superposition states in excited state processes has received considerable attention in the last two decades largely due to advancements in ultrafast laser spectroscopy. These coherence effects hold promise for enhancing the efficiency and robustness of functionally relevant processes, even when confronted with energy disorder and environmental fluctuations. Understanding coherence deeply drives us to unravel mechanisms and dynamics controlled by order and synchronization at a quantum mechanical level, envisioning optical control of coherence to enhance functions or create new ones in molecular and material systems. In this frontier, the interplay between electronic and vibrational dynamics, specifically the influence of vibrations in directing electronic dynamics, has emerged as the leading principle. Here, two energetically disparate quantum degrees of freedom work in-sync to dictate the trajectory of an excited state reaction. Moreover, with the vibrational degree being directly related to the structural composition of molecular or material systems, new molecular designs could be inspired by tailoring certain structural elements. In the realm of chemical kinetics, our understanding of the dynamics of chemical transformations is underpinned by fundamental theories, such as transition state theory, activated rate theory, and Marcus theory. These theories elucidate reaction rates by considering the energy barriers that must be overcome for reactants to transform into products. Those barriers are surmounted by the stochastic nature of energy gap fluctuations within reacting systems, emphasizing that the reaction coordinate, the pathway from reactants to products, is not rigidly defined by a specific vibrational motion but encompasses a diverse array of molecular motions. While less is known about the involvement of specific intramolecular vibrational modes, their significance in certain cases cannot be overlooked. In this Account, we summarize key experimental findings that offer deeper insights into the complex electronic–vibrational trajectories encompassing excited states afforded from state-of-the-art ultrafast laser spectroscopy in three exemplary processes: photoinduced electron transfer, singlet–triplet intersystem crossing, and intramolecular vibrational energy flow in molecular systems. We delve into the rapid decoherence, or loss of phase and amplitude correlations, of vibrational coherences along promoter vibrations during subpicosecond intersystem crossing dynamics in a series of binuclear platinum complexes. This rapid decoherence illustrates the vibration-driven reactive pathways from the Franck–Condon state to the curve crossing region. We also explore the generation of new vibrational coherences induced by impulsive reaction dynamics rather than by the laser pulse in these systems, which sheds light on specific energy dissipation pathways and thereby on the progression of the reaction trajectory in the vicinity of the curve crossing on the product side. Another property of vibrational coherences, amplitude, reveals how energy can flow from one vibration to another in the electronic excited state of a terpyridine–molybdenum complex hosting a nonreactive dinitrogen substrate. In conclusion, a slight change in vibrational energy triggers a quasi-resonant interaction, leading to constructive wavepacket interference and ultimately intramolecular vibrational redistribution from a Franck–Condon active terpyridine vibration to a dinitrogen stretching vibration, energizing the dinitrogen bond.

Electrical energy↗

Initial Conditions of Planet Formation: Time Constraints from Small Bodies and the Lifetime of Reservoirs in the Solar Protoplanetary Disk

This review explores the timescales of the initial phase of planet formation, from nebular dust (CAIs and chondrules) to planetesimal accretion and differentiation, using evidence from meteorite research. Aluminium-Mg systematics of CAIs indicate either an extended period of CAI formation (∼0.3 Ma) or an initial 26 Al heterogeneity, with evidence supporting a homogeneous 26 Al abundance in the protoplanetary disk. Thermal and aqueous alteration on the parent body can disturb the U-Pb and Al-Mg chronometers in chondrules. Focusing on relatively robust isochron data from plagioclase of pristine (types ≤3.05) chondrites indicates a shift in chondrule formation locations, moving from the inner to the outer disk over time. Ages of basaltic achondrites show that silicate differentiation on small bodies was well underway within the first few million years (Ma) of our solar system. Their age record, however, reveals inconsistencies between different chronometers, partly caused by (i) secondary disturbances due to thermal metamorphism, aqueous alteration, or impacts, (ii) the presence of xenolithic minerals, and (iii) potentially variable initial 26 Al abundances due to disturbances at the mineral scale. Nucleosynthetic isotope data indicate that parent bodies of iron and stony meteorites formed in two distinct regions within the protoplanetary disk: the inner, non-carbonaceous (NC) and the outer, carbonaceous (CC) region. Based on Hf-W chronometry it has been demonstrated that NC and CC parent bodies of magmatic iron meteorites segregated their cores within ∼1–3 Ma after CAI formation, implying that parent body accretion occurred within <1 Ma in both reservoirs. Combining accretion ages with nucleosynthetic data further reveals that, at first order, NC and CC reservoirs in the solar protoplanetary disk were established within 1 Ma and existed over several Ma with limited exchange between them. In the CR chondrite accretion region of the disk, planetary bodies formed over at least 3 Ma, while in most other regions, formation spanned at least 1 Ma, with minimal changes in nucleosynthetic isotope compositions. Aerodynamical size sorting of dust likely introduced or amplified some of these variations.

26Al distribution↗

Chemical Evolution of Interstellar Dust into Planetary Materials

Comets are believed to retain some interstellar materials, stored in fairly pristine conditions since-their formation. The composition and properties of cometary dust grains should reflect those of grains in the outer part of the protosolar nebula which, at least in part, were inherited from the presolar molecular cloud. However, infrared emission features in comets differ from their interstellar counterparts. These differences imply processing of interstellar material on its way to incorporation in comets, but C and N appear to be retained. Overall dust evolution from the interstellar medium (ISM) to planetary materials is accompanied by an increase in proportion of complex organics and a decrease in pure carbon phases. The composition of cometary dust grains was measured in situ during fly-by missions to comet Halley in 1986. The mass spectra of about 5000 cometary dust grains with masses of 5 x 10(exp -17) - 5 x 10(exp -12) g provide data about the presence and relative abundances of the major elements H, C, N, O,Na, Mg, Al, Si, S, Cl, K, Ca, Ti, Cr, Fe, Ni. The bulk abundances of major rock-forming elements integrated over all spectra were found to be solar within a factor of 2, while the volatile elements H, C, N, O in dust are depleted in respect to their total cosmic abundances. The abundances of C and N in comet dust are much closer to interstellar than to meteoritic and are higher than those of dust in the diffuse ISM. In dense molecular clouds dust grains are covered by icy mantles, the average composition of which is estimated to be H:C:N:O = 96:14:1:34. Up to 40% of elemental C and O may be sequestered in mantles. If we use this upper limit to add H, C, N and O as icy mantle material to the abundances residing in dust in the diffuse ISM, then the resulting values for H. C, and N match cometary abundances. Thus, ice mantles undergoing chemical evolution on grains in the dense ISM appear to have been transformed into less volatile and more complex organic residues wherein the H, C and N are largely retained and ultimately accreted in cometary dust. The abundance of O is about the same for cometary dust, meteorites and interstellar dust. In all these samples, most of O in a solid phase is bonded to silicates. In dense molecular clouds, the abundance of O in dust+mantles is significantly higher then in cometary dust. This difference may reflect the greater lability of oxygenated species toward astrophysical processing. Laboratory studies show that O-bearing functional groups in organic compounds tend to be relatively easily removed by heating and/or UV and particle irradiation . In Halley's coma, O-containing organic grains, being unstable, were located closest to the nucleus. The decomposition of the organic grain component in the coma provided a significant extended source contribution to O-containing gaseous species such as CO and H2CO.

Fomenkova, M. N.↗

Seasonal Variability of Saturn's Tropospheric Temperatures, Winds and Para-H2 from Cassini Far-IR Spectroscopy

Far-IR 16-1000 micrometer spectra of Saturn's hydrogen-helium continuum measured by Cassini's Composite Infrared Spectrometer (CIRS) are inverted to construct a near-continuous record of upper tropospheric (70-700 mbar) temperatures and para-H2 fraction as a function of latitude, pressure and time for a third of a saturnian year (2004-2014, from northern winter to northern spring). The thermal field reveals evidence of reversing summertime asymmetries superimposed onto the belt/zone structure. The temperature structure is almost symmetric about the equator by 2014, with seasonal lag times that increase with depth and are qualitatively consistent with radiative climate models. Localised heating of the tropospheric hazes (100-250 mbar) create a distinct perturbation to the temperature profile that shifts in magnitude and location, declining in the autumn hemisphere and growing in the spring. Changes in the para-H2 (f(sub p)) distribution are subtle, with a 0.02-0.03 rise over the spring hemisphere (200-500 mbar) perturbed by (i) low-f(sub p) air advected by both the springtime storm of 2010 and equatorial upwelling; and (ii) subsidence of high-f(sub p) air at northern high latitudes, responsible for a developing north-south asymmetry in f(sub p). Conversely, the shifting asymmetry in the para-H2 disequilibrium primarily reflects the changing temperature structure (and hence the equilibrium distribution of f(sub p)), rather than actual changes in f(sub p) induced by chemical conversion or transport. CIRS results interpolated to the same point in the seasonal cycle as re-analysed Voyager-1 observations (early northern spring) show qualitative consistency from year to year (i.e., the same tropospheric asymmetries in temperature and f(sub p)), with the exception of the tropical tropopause near the equatorial zones and belts, where downward propagation of a cool temperature anomaly associated with Saturn's stratospheric oscillation could potentially perturb tropopause temperatures, para-H2 and winds. Quantitative differences between the Cassini and Voyager epochs suggest that the oscillation is not in phase with the seasonal cycle at these tropospheric depths (i.e., it should be described as quasi-periodic rather than 'semi annual'). Variability in the zonal wind field derived from latitudinal thermal gradients is small (less than 10 m/s per scale height near the tropopause) and mostly affects the broad retrograde jets, with the notable exception of large variability on the northern flank of the equatorial jet. The meridional potential vorticity (PV) gradient, and hence the 'staircase of PV' associated with spatial variations in the vigour of vertical mixing, has varied over the course of the mission but maintained its overall shape. PV gradients in latitude and altitude are used to estimate the atmospheric refractive index for the propagation of stationary planetary (Rossby) waves, predicting that such wave activity would be confined to regions of real refractivity (tropical regions plus bands at 35-45 in both hemispheres). The penetration depth of these regions into the upper troposphere is temporally variable (potentially associated with stratification changes), whereas the latitudinal structure is largely unchanged over time (associated with the zonal jet system).

Fletcher, Leigh N.↗

Physical, Chemical, and Petrological Characteristics of Chondritic Materials and Their Relationships to Small Solar System Bodies: Chapter - 2

Chondrite materials with varying abundances of volatile-bearing phases are expected at the destinations for the asteroid sample-return missions Hayabusa2 and OSIRIS-REx. The targets of the missions are 162173 (1999 JU3) Ryugu and 101955 (1999 RQ36) Bennu. Spectroscopic analyses of these asteroids suggest that their surface materials are related to types 1 and 2 carbonaceous chondrites. Some studies suggest that the parent bodies of these chondrites may have also experienced some thermal and/or shock metamorphism. The physical properties of boulders at asteroid surfaces and fine particles in asteroid regoliths are consequences of the diverse processes that fragmented them, mobilized them, and redeposited them in unique accumulations. Sample-return missions are likely to encounter a broad range of carbonaceous chondrite (CC)-like materials, to which aqueous alteration, thermal, and shock metamorphism imparted changes affecting their sub-micron- to meter-scale physical properties. Consequently, implementation of scale-dependent analytical techniques to the study of the chemical, physical, and geotechnical characteristics of these CC-like materials is fundamental to safe mission operations, sample selection, and return. However, most of the available knowledge for informing and formulating expectations about regolith processes, products, and properties on carbonaceous small bodies comes from missions that studied anhydrous (e.g., Itokawa studied by Hayabusa) and/or much larger asteroids (e.g., Vesta studied by Dawn). No previous mission is likely directly relevant to small ice-free carbonaceous NEOs 162173 Ryugu or 101955 Bennu, although the Rosetta Spaceraft performed a flyby of the large asteroid Lutetia which has variously been classified as M and C type (Pätzold et al., 2011). Carbonaceous chondrites carry the best record of the history, distribution, and activity of water in the early solar system. Ordinary and Enstatite chondrites carry only partial records, but these are still critical to understanding the full story. We will describe the records of water-rock interactions on asteroids, as recorded in these meteorites, with particular emphasis on the timing, nature, settings, and fluid compositions. An integral part of this story is the rare, but fortunate, preservation of actual early solar system water as aqueous fluid inclusions.

Zolensky, Michael E.↗

Examining the effects of chemical cleaning, leaching, and partial dissolution on zinc and cadmium isotope fractionation in marine carbonates

The application of zinc (Zn) and cadmium (Cd) isotopes as palaeo-proxies in carbonate sediment is rapidly expanding due to their potential for tracing changes in biological productivity in the modern and past oceans. However, there are limited investigations into the chemical cleaning methods required to produce the most consistent and accurate data for these novel isotope systems. This could impact their use as palaeo-proxies to reconstruct ocean-atmosphere-climate interactions throughout Earth's history. To address this concern and expand the utility of the Zn and Cd stable isotope systems as palaeo-productivity tracers, the performance of two standard chemical cleaning protocols for acquiring robust and reliable Zn and Cd isotope datasets were assessed. These include (i) the Cd-cleaning method that uses a reductive step to selectively leach contaminating secondary iron (Fe)-manganese (Mn) (oxyhydr)oxide coatings from the carbonate surface, and an oxidative step that is used to remove post-depositional organic matter and sulphide precipitates; and (ii) the magnesium/calcium cleaning protocol that includes an oxidative step only, leaving secondary Fesingle bondMn (oxyhydr)oxide coatings largely intact. Well-preserved Holocene-, and Mesozoic-aged carbonate sediments were used to test the reliability of these two chemical cleaning methods. The Holocene samples comprised not only aliquots of bulk sediment, but also individual species of planktic and benthic foraminifera. Our results show that the best practice chemical cleaning method for retrieving consistent and accurate Zn and Cd isotope, and Zn/Ca and Cd/Ca datasets for carbonate sediments, requires both reductive and oxidative cleaning following the Cd-cleaning method. This differs from most methodological approaches applied to date that remove the reductive step from the chemical cleaning protocol and apply an oxidative step only, or no chemical cleaning at all. Inclusion of the reductive step in the chemical cleaning method typically shifts δ 66 Zn by ~0.1‰ lower and δ 114 Cd by 0.3‰ higher in the solid phase, while Zn/Ca and Cd/Ca typically decrease 2-fold. The benthic foraminifera, C. wuellerstorfi, that live in ocean bottom waters where the seawater Zn and Cd isotope composition is homogeneous display evidence of Zn and Cd isotope fractionation between seawater and carbonate on the order of 0.08 ± 0.08‰ (2SE, n = 4) and -0.25 ± 0.13‰ (2SE, n = 4), respectively, in agreement with experimental constraints. Furthermore, evidence of Zn isotope fractionation effects are recorded in a naturally-dissolved carbonate sediment, together with laboratory-controlled carbonate dissolution experiments. Based on these results, we recommend the Cd-cleaning method and the application of Zn and Cd isotope fractionation factors to accurately reconstruct past seawater Zn and Cd isotope compositions from carbonate sediments.

58 GEOSCIENCES↗

Toward Realistic Dynamics of Rotating Orbital Debris, and Implications for Lightcurve Interpretation

Optical observations of rotating space debris near GEO contain important information on size, shape, composition, and rotational states, but these aspects are difficult to extract due to data limitations and the high number of degrees of freedom in the modeling process. For tri-axial rigid debris objects created by satellite fragmentations, the most likely initial rotation state has a large component of initial angular velocity directed along the intermediate axis of inertia, leading to large angular reorientations of the body on the timescale of the rotation period. This lends some support to the simplest possible interpretation of light curves -- that they represent sets of random orientations of the objects of study. However, effects of internal friction and solar radiation are likely to cause significant modification of rotation states within a time as short as a few orbital periods. In order to examine the rotational dynamics of debris objects under the influences of these effects, a set of seven first-order coupled equations of motion were assembled in state form: three are Euler equations describing the rates of change of the components of angular velocity in the body frame, and four describe the rates of change of the components of the unit quaternion. Quaternions are a four-dimensional extension of complex numbers that form a seamless, singularity-free representation of body orientation on S3. The Euler equations contain explicit terms describing torque from solar radiation in terms of spherical harmonics, and terms representing effects of a prescribed rate of internal friction. Numerical integrations of these equations of motion are being performed, and results will be presented. Initial tests show that internal friction without solar radiation torque leads to rotation about the maximum principal axis of inertia, as required, and solar radiation torque is expected to lead to spin-up of objects. Because the axis of maximum rotational inertia tends to be roughly coincident with the normal to the largest projected cross-sectional area, internal friction is expected to lead to reduced variation of light curve amplitudes at a given phase angle, but a large dependence of the same on phase angle. At a given phase angle, databases are generated which contain reflected intensities for comprehensive sets of equally-likely orientations, represented as unit quaternions. When projected onto three dimensions (S2) and color-coded by intensity, the set is depicted as points within a solid, semi-transparent unit sphere, within which all possible reflected intensities for an object at a given phase angle may be inspected simultaneously. Rotational sequences are represented by trajectories through the sphere. Databases are generated for each of a set of phase angles separately, forming a comprehensive dataset of reflected intensities spanning all object orientations and solar phase angles. Symmetries in the problem suggest that preferred rotation states are likely, defined relative to the object-sun direction in inertial space and relative to the maximum principal axis of inertia in the body coordinate system. Such rotation states may greatly simplify the problem of light curve interpretation by reducing the number of degrees of freedom in the problem.

Ojakangas, Gregory W.↗

Comparative Dissolution of Iron-Bearing Minerals by Catecholate and Hydroxamate Siderophores under Oxic and Anoxic Conditions

Siderophores play a crucial role in biological iron (Fe) acquisition and mobilization by promoting Fe mineral and rock weathering. While the effects of the hydroxamate siderophore desferrioxamine B (DFOB) have been extensively studied, the role of catecholates in the dissolution of Fe mineral and rock under varying redox conditions remain limited. Moreover, despite Fe being one of the most redox-active metals, the siderophore-mediated redox transformations of solid-phase Fe and their impact on mineral dissolution are not well understood. Herein, this study systematically investigated dissolution behavior of both Fe(II) and Fe(III)-bearing minerals and rocks (Fe(II)- bearing basalt and olivine, and Fe(III)- bearing nontronite and goethite), by two structurally distinct biological siderophores, catecholate protochelin and hydroxamate DFOB, under both oxic and anoxic conditions. Batch experiments quantified Fe and transition metals (Mn, Ni, Zn, Mo) released from the tested minerals in the presence of siderophores. Throughout the dissolution experiments, siderophore concentrations and Fe-siderophore complexation in solutions were measured using UV-vis spectrometry. Fe redox changes under oxic and anoxic conditions by siderophores were determined, and mineral surface alterations following siderophore treatments were characterized through scanning electron microscopy (SEM) and time-of-flight secondary ion mass spectroscopy (ToF-SIMS). Results revealed distinct interplays of dissolution mechanisms, including ligand-exchange promoted dissolution and reductive dissolution, along with Fe(III) reduction and Fe(II) oxidation, contributing to the Fe(II)- and Fe(III)-rich mineral weathering under varying redox conditions. Under oxic conditions, both protochelin and DFOB enhanced Fe release from Fe(II)-rich basalt and olivine more effectively than from Fe(III)-rich minerals. DFOB induced greater Fe(II)-mineral dissolution than protochelin. This difference was attributed to a higher level of Fe(II) oxidation by DFOB in contrast to protochelin, as well as the protochelin oxidation with the loss of Fe binding groups (catechols). Under anoxic conditions, both siderophores significantly reduced Fe(III) in nontronite and goethite, with protochelin demonstrating substantially stronger Fe(III) reduction capacity than DFOB. However, Fe(III) reduction negatively impacted Fe release from Fe(III)-rich minerals. Instead, Fe release from Fe(II)-rich minerals was enhanced under anoxic conditions due to the absence of Fe(II) oxidation and labile Fe(II). Variations in siderophore adsorption also contributed to dissolution differences. Beyond iron, the release of transition metals from tested minerals was influenced by elemental contents, mineral compositions, and siderophore types, revealing distinct metal- and siderophore-dependent patterns. This systematic investigation highlights the roles of siderophores in Fe redox cycling and metal mobilization, enhancing our understanding of different siderophore behaviors in siderophore-mediated microbial metal acquisition within redox-dynamic environments, with implications for bioleaching industries and applications in agriculture and climate change mitigation.

Guo, Dongyi↗

Reply to Comment by Cole-dai Et Al. on "Climatic Impact of the Long-lasting Laki Eruption: Inapplicability of Mass-independent Sulfur Isotope Composition Measurements"

Here we respond to the comments by Cole-Dai et al. [2014] on our article Schmidt et al. [2012]. Specifically, in response to section 2 of their reply, we argued in Schmidt et al. [2012] that based on previously published estimates of the volatile release height during the 1783-1784 C.E. Laki eruption, the lack of a sulfur massindependent fractionation (MIF) anomaly is expected. In other words, no previous study on Laki ever argued that this eruption emitted SO2 into altitudes >13-15 km. In section 2.3, Cole-Dai et al. [2014] argue that the nonzero Δ33S value of their Laki sample 1 may be explained by a short-lived explosive phase at Laki during which volatiles reached the stratosphere. In Schmidt et al. [2012] in section 2, we argued in agreement with Cole-Dai et al. [2014] (section 3.1) that for a MIF anomaly to be preserved, the Laki volatiles would have had to be emitted in >20 km altitude. Our main point is that eruption column heights >20 km are unlikely based on the historical accounts and plume-rise modeling for the Laki eruption [Stothers et al., 1986; Woods, 1993; Thordarson and Self, 2003]. In Schmidt et al. [2012], we argued that to deduce a short-lived climatic impact of the Laki eruption based on the lack of a MIF anomaly and the length of the sulfate deposition in Greenland ice cores may be misleading because the climatic impact will outlast the radiative forcing of the Laki aerosol cloud. Cole-Dai et al. [2014] acknowledge the latter in their reply in section 4.2. We agreewith Cole-Dai et al. [2014] in that themagnitude and length of the climatic impact during the winter of 1783-1784 depends on the altitude of the volatile release during the eruption (sections 2.3 and 4.2). However, even if we assumed that during Laki all sulfur dioxide (SO2) would have been released in the troposphere, then the aerosol cloud would still be present in the upper troposphere during March 1784, as is evident from independent model simulations of this "tropospheric-only" scenario [Stevenson et al., 2003]. We acknowledge that there is uncertainty on the volatile release height for Laki; however, it is worth considering that those climate model simulations that used an injection altitude between 9 km and 13 km for the Laki SO2 [Highwood and Stevenson, 2003; Oman et al., 2006a, 2006b; Schmidt et al., 2012] best match the observed temperature changes during summer of 1783 [Angell and Korshover, 1985; Brázdil et al., 2010; Briffa et al., 1998; D'Arrigo and Jacoby, 1999; Jacoby et al., 1999; Kington, 1988; Manley, 1974; Parker et al., 1992; Thordarson and Self, 2003]. Based on these model simulations, a climatic impact during the winter of 1783-1784, albeit weaker than during the climactic phases of Laki, is expected (and our argument here does not exclude the role of natural variability in contributing to the cold winter of 1783-1784 as discussed in Schmidt et al. [2012]). Therefore, we continue to argue that for high-latitude eruptions such as Laki, the applicability of sulfur isotopic measurements to interpret the climatic relevance has yet to be demonstrated. Itmay transpire that the interpretation of MIF signals for the climate-relevance of an eruption is valid and unambiguous only for short-lived explosive eruptions in the tropics. In terms of the processes producing a MIF anomaly (section 3.3 in Cole-Dai et al. [2014]), the works by Hattori et al. [2013] and Ono et al. [2013] suggest that there are remaining issues not discussed by Cole-Dai et al. [2014], for instance, self-shielding of SO2 due to high column densities typical for eruptions of Pinatubo-scale and greater, and the preservation of the MIF signature in general.

general circulation model↗

Tracking the phase changes in micelle-based NiGa nanocatalysts for methanol synthesis under activation and working conditions

The hydrogenation of CO 2 into high energy density fuels such as methanol, where the required H 2 is obtained from renewable sources, is of utmost importance for a sustainable society. In recent years, NiGa alloys have attracted attention as promising catalyst material systems for the hydrogenation of CO 2 into methanol at ambient pressures. They thus represent an energy-saving alternative to the Cu-based catalysts employed in today's catalytic industry that require high pressures for the CO 2 hydrogenation. However, the underlying reaction mechanisms for the NiGa system are still under debate. One of the challenges here is to unravel the evolution and coexistence of the different species in the heterogeneous NiGa catalyst system under activation and reaction conditions. To shed light on their evolution under activation in H 2 and their catalytic roles under CO 2 hydrogenation working conditions on well-defined Ni 3 Ga 1 and Ni 5 Ga 3 nanoparticle (NP) catalysts, we employed a multi-probe approach in this study. It included advanced machine learning-based analysis of operando X-ray absorption spectroscopy data combined with operando powder X-ray diffraction and near ambient pressure X-ray photoelectron spectroscopy measurements, as well as reactivity studies using bed-packed mass flow reactors. In addition, we employed atomic force microscopy and scanning transmission electron microscopy for structural characterization. Under H 2 activation at 1 bar total pressure, we concluded the formation of metallic Ni, starting for Ni 3 Ga 1 at 300 °C, and for Ni 5 Ga 3 at 400 °C. At higher temperatures, the formation of NiGa alloys follows. The α'-Ni 3 Ga 1 alloy phase is predominantly formed for the Ni 3 Ga 1 NPs, while the coexistence of α'-Ni 3 Ga 1 , δ-Ni 5 Ga 3 and Ga 2 O 3 phases is observed for the Ni 5 Ga 3 NPs after the H 2 activation. The formation of the Ga 2 O 3 phase also results in the presence of excess metallic Ni. Under CO 2 hydrogenation reaction conditions, Ga partially oxidizes again to form a Ga 2 O 3 -rich particle shell for both NP compositions, yet, to a larger extent for the Ni 3 Ga 1 NPs, which, in turn, feature a higher amount of excess Ni. We reveal that metallic Ni is responsible for the high selectivity of the Ni 3 Ga 1 NPs towards the production of methane in our catalytic tests. In contrast, the Ni 5 Ga 3 NPs display a strong selectivity toward methanol production (>92%), more than one order of magnitude higher than that for the Ni 3 Ga 1 NPs, which we ascribe to the presence of the δ-Ni 5 Ga 3 phase.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Microstructural Changes and Pb Mobility During the Zircon to Reidite Transformation: Implications for Planetary Impact Chronology

Impact events modify and leave behind a complex history of rock metamorphism on terrestrial planets. Evidence for an impact event may be recorded in physical changes to minerals, such as mineral deformation and formation of high P-T polymorphs, but also in the form of chemical fingerprints, such as enhanced elemental diffusion and isotopic mixing. Here we explore laboratory shock-induced physical and chemical changes to zircon and feldspar, the former of which is of interest because its trace elements abundances and isotope ratios are used extensively in geochemistry and geochronology. To this end, a granular mixture of Bishop Tuff sanidine and Kuehl Lake zircon, both with well characterized Pb isotope compositions, was prepared and then shocked via a flat plate accelerator. The peak pressure of the experiment, as calculated by the impedance matching method, was ~24 GPa although a broader range of P-T conditions is anticipated due to starting sample porosity. Unshocked and shocked materials were characterized via scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), and Raman spectroscopy. These methods show that the starting zircon material had abundant metamict regions, and the conversion of the feldspar to glass in the post-shock material. Analyses of the shocked product also yielded multiple occurrences of the high-pressure ZrSiO 4 polymorph reidite, with some domains up to 300 μm across. The possibility of U-Pb system disturbance was evaluated via laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and secondary ion mass spectrometry (SIMS). The isotopic data reveal that disturbance of the U-Pb geochronometer in the reidite was minimal (<2% for the main U-Pb geochronometers). To better constrain the P-T conditions during the shock experiment, we complement impedance matching pressure calculations with iSALE2D impact simulations. The simulated results yield a range of P-T conditions experienced during the experiment and show that much of the sample may have reached >30 GPa, which is consistent with formation of reidite. In the recovered shocked material, we identified lamellae of reidite, some of which interlock with zircon lamellae. Reidite {112} twins were identified, which we interpret to have formed to reduce stress between the crystal structure of the host zircon and reidite. These two findings support the interpretation that shear transformation enabled the transition of zircon to reidite. The size and presence of reidite found here indicate that this phase is probably common in impact-shocked crustal rocks that experienced ~25 to ~35 GPa, especially when the target material has porosity. Additionally, shock loading of the zircon and transformation to reidite at these pressures in porous materials is unlikely to significantly disturb the U-Pb system in zircon and that the reidite inherits the primary U and Pb elemental and isotopic ratios from the zircon.

Bishop Tuff↗

Twisted Tin‐Chloride Perovskite Single‐Crystal Heterostructures

Self-assembly affords simpler synthetic routes to heterostructures compared with manual layer-by-layer stacking, yet controlling interlayer twist angles in a bulk solid remains an outstanding challenge. We report two new single-crystal heterostructures: (Sn 2 Cl 2 )(CYS) 2 SnCl 4 (CYS = + NH 3 (CH 2 ) 2 S – ; Sn_CYS) and (Sn 2 Cl 2 )(SeCYS) 2 SnCl 4 (SeCYS = + NH 3 (CH 2 ) 2 Se – ; Sn_SeCYS) synthesized in solution, with alternating perovskite and intergrowth layers. Notably, compared to the recently reported lead analog, (Pb 2 Cl 2 )(CYS) 2 PbCl 4 (Pb_CYS), the tin heterostructures feature a twist between the perovskite and intergrowth layers. We trace this twist to local distortions at the Sn centers, which change the interfacial lattice-matching requirements compared to those of the Pb analog. Electronic band structure calculations show that the striking differences in the relative energies of perovskite- and intergrowth-derived bands in Sn_CYS and Pb_CYS arise from structural and not compositional differences. The structural anisotropy of Sn_CYS is also reflected in a large in-plane photoluminescence linear anisotropy ratio. Interfacial strain further affords differential incorporation of Pb into the perovskite and intergrowth layers of the Sn heterostructures, resulting in redshifted optical absorption onsets. Thus, we posit that local structural distortions may be exploited to manipulate the twist angle and interfacial strain in bulk heterostructures, providing a new handle for tuning the band alignments of bulk quantum-well electronic structures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Preservation of high-pressure volatiles in nanostructured diamond capsules

High pressure induces dramatic changes and novel phenomena in condensed volatiles(1,2) that are usually not preserved after recovery from pressure vessels. In this study we report a process that pressurizes volatiles into nanopores of type 1 glassy carbon precursors, converts glassy carbon into nanocrystalline diamond by heating and synthesizes free-standing nanostructured diamond capsules (NDCs) capable of permanently preserving volatiles at high pressures, even after release back to ambient conditions for various vacuum-based diagnostic probes including electron microscopy. As a demonstration, we perform a comprehensive study of a high-pressure argon sample preserved in NDCs. Synchrotron X-ray diffraction and high-resolution transmission electron microscopy show nanometre-sized argon crystals at around 22.0 gigapascals embedded in nanocrystalline diamond, energy-dispersive X-ray spectroscopy provides quantitative compositional analysis and electron energy-loss spectroscopy details the chemical bonding nature of high-pressure argon. The preserved pressure of the argon sample inside NDCs can be tuned by controlling NDC synthesis pressure. To test the general applicability of the NDC process, we show that high-pressure neon can also be trapped in NDCs and that type 2 glassy carbon can be used as the precursor container material. Additional experiments on other volatiles and carbon allotropes open the possibility of bringing high-pressure explorations on a par with mainstream condensed-matter investigations and applications.

36 MATERIALS SCIENCE↗

Evidence of an oxidation induced phase transformation for a delta phase plutonium-gallium alloy

The oxidation of an ~1.5 at% Ga plutonium metal alloy in dry air as a function of time was studied using a combination of FIB-SEM, AES, and XRD. Analysis of SEM images of FIB cross-sections of the oxide allowed for direct measurement of the oxide thickness as well as determination of heterogeneity in the extent of the oxide. AES analysis performed on cross-sections of the oxide allowed for quantitative analysis of the atomic composition and semi-quantitative analysis of the chemical composition. Initial preparation of the sample was found to induce a martensitic transformation to α' - Pu with an average thickness of 233 nm. Electropolishing was found to be sufficient to fully remove the α' layer with creation of only a minimum oxide layer. Growth of the oxide in dry air was found to initially follow parabolic kinetics, with a parabolic rate constant orders of magnitude higher than expected for δ-Pu but in-line with values extrapolated to room temperature for α-Pu. Following complete oxidation of the initial α` layer, further regions of plutonium metal depleted in gallium were observed to form at the oxide / metal interface. However, gallium, as Ga 2 O 3 , was found to be enriched at the surface and present in the oxide in an amount comparable to the relative Ga:Pu ratio of the bulk metal alloy. Finally, the results presented here serve to bridge a diverse array of previous experimental and theoretical data and provide the first comprehensive view of the fate of the δ-stabilizer during formation of an oxide.

36 MATERIALS SCIENCE↗

Measurement and evaluation of the radiative properties of a thin solid fuel

Accurate modeling of combustion systems requires knowledge of the radiative properties of the system. Gas phase properties are well known, but detailed knowledge of surface properties is limited. Recent work has provided spectrally resolved data for some solid fuels, but only for the unburned material at room temperature, and for limited sets of previously burned and quenched samples. Due to lack of knowledge of the spectrally resolved properties at elevated temperatures, as well as processing limitations in the modeling effort, graybody values are typically used for the fuels surface radiative properties. However, the spectrally resolved properties for the fuels at room temperature can be used to give a first-order correction for temperature effects on the graybody values. Figure 1 shows a sample of the spectrally resolved emittance/absorptance for a thin solid fuel of the type commonly used in combustion studies, from approximately 2 to 20 microns. This plot clearly shows a strong spectral dependence across the entire range. By definition, the emittance is the ratio of the emitted energy to that of a blackbody at the same temperature. Therefore, to determine a graybody emittance for this material, the spectrally resolved data must be applied to a blackbody curve. The total area under the resulting curve is ratioed to the total area under the blackbody curve to yield the answer. Due to the asymmetry of the spectrally resolved emittance and the changing shape of the blackbody curve as the temperature increases, the relative importance of the emittance value at any given wavelength will change as a function of temperature. Therefore, the graybody emittance value for a given material will change as a function of temperature even if the spectral dependence of the radiative properties remains unchanged. This is demonstrated in Figures 2 and 3, which are plots of the spectrally resolved emittance for KimWipes (shown in Figure 1) multiplied by the blackbody curves for 300 K (Figure 2) and 800 K (Figure 3). Each figure also shows the blackbody curve for that temperature. Ratioing the areas under the curve for each of these figures give a graybody emittance of 0.64 at 300 K, and 0.46 at 800 K. It is recognized that materials undergoing pyrolysis will change in composition as they heat up, and that the radiative properties of the materials may have inherent temperature dependence. Both of these effects will contribute to changes in the radiative characteristics of a given material, and are not accounted for here. However, this paper demonstrates the temperature dependence of graybody radiative properties, and provides a method for a first-order correction (for temperature) to the graybody values if the spectrally resolved properties are known.

Pettegrew, Richard↗

Mineralogical and isotopic constraints on early, high-temperature events and reservoirs recorded in the interior of a Type B Ca-Al-rich inclusion from the reduced CV3 chondrite Vigarano

A coordinated mineralogical and oxygen and Al-Mg isotopic study of a Type B Ca-Al-rich inclusion (CAI) from the reduced CV3 chondrite Vigarano was carried out using electron microprobe analysis, transmission electron microscopy, and secondary ion mass spectrometry. This CAI, a once molten igneous object, shows heterogeneous oxygen isotopic compositions among its constituent mineral phases. Spinel is uniformly 16 O-rich with Δ 17 O ≤ −23 ‰. The Δ 17 O values of Al,Ti-diopside in the CAI core range from −11 ‰ to −18 ‰, which are positively correlated with its TiO 2 contents, whereas diopside in the Wark–Lovering (WL) rim is 16 O-rich with Δ 17 O = −23 ‰. Melilite in the CAI mantle shows Δ 17 O values ≤ −10 ‰ only when Åk <15 but becomes more 16 O-poor (Δ 17 O = −3 ‰ to −9 ‰) when Åk >15 . These correlated chemical and oxygen isotopic variations were likely established during crystallization of melilite and Al,Ti-diopside from a partial melt, while spinel preserves the original 16 O-rich composition of the CAI precursor. We infer that a partial melt was isotopically evolving from 16 O-rich to 16 O-poor during melilite crystallization, then back to 16 O-rich during Al,Ti-diopside crystallization via exchange with different gas reservoirs of 16 O-poor and 16 O-rich compositions during heating event(s). Our Al-Mg isotopic measurements of the CAI core and mantle define a single isochron with an inferred initial 26 Al/ 27 Al ratio of (4.93 ± 0.18) × 10 −5 , indistinguishable from that of the WL rim. This indicates that multiple high-temperature events and oxygen isotope exchange with isotopically distinct gas reservoirs occurred rapidly during the CAI formation.

Al-Mg isotopic systematic↗

Competing Effects of Network Architecture and Composition on Polydomain Liquid Crystal Elastomers

Main-chain liquid crystal elastomers (LCEs) are synthesized to investigate the interplay of the composition and network structure on LCE nematic-to-isotropic (N–I) transitions. We focus on networks synthesized from liquid crystalline oligomers reacted with tri- or tetrafunctional nonmesogenic cross-linker molecules. We find that coupling between mesogens and the polymer backbone increases with the degree of cross-linking. However, this enhanced coupling competes with mesogenic dilution arising from the cross-linker molecules to determine the N–I transition temperature (T NI ). When cross-linker molecules are dilute, the degree of cross-linking directly correlates to the change in T NI from the oligomer to LCE (ΔT NI ) through mesogen–backbone coupling. In this regime, ΔT NI ranges from 2.9 to 12.2 °C and 2.9–13.9 °C for tri- and tetrafunctional cross-linkers, respectively. At high cross-linker concentrations, deviations from this linear relationship appear. Further, the fractional mesogen content within an oligomer chain induces molecular weight-dependent mesogenic dilution effects arising from the flexible spacer molecules. Analysis of the N–I transition peak reveals a maximum latent heat per gram of mesogen (ΔH NI,mes ) for this system.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Molecular Layer Deposited Aluminum‐Based Hybrid Resist for High‐Resolution Nanolithography and Direct Ultra‐High Aspect Ratio Pattern Transfer

Inorganic-containing hybrid photoresists are critical for next-generation extreme ultraviolet (EUV) lithography and angstrom-era semiconductor miniaturization. However, associated conventional solution processing struggles to achieve ultrathin, uniform films with high conformality and compositional control, limiting overall patterning performance. Here, this study reports the systematic lithographic patterning characterization of an Al-based hybrid resist synthesized via vapor-phase molecular layer deposition (MLD), using the trimethylaluminum (TMA) metal precursor and the hydroquinone (HQ) aromatic organic linker. The resist supports both sub-20 nm high-resolution nanolithography and virtually infinite silicon plasma etch selectivity. Lithographic performance studied using electron beam lithography (EBL) as a proxy for EUV shows that, under an optimized process adopting post-exposure bake, the resist achieves the best resolution of 15.4 nm linewidth under stringent 1:1 line-space high-density patterning—limited only by the minimum beam size of the EBL system. The resist also shows wide dose latitude and balanced performance in resolution, roughness, and sensitivity. The infinite silicon etch selectivity, stemming from spontaneous aluminum oxyfluoride passivation layer formation, enables fabrication of micrometer-tall, 40 nm-wide silicon nanofin structures using only a ≈30 nm-thick resist layer, without no hard mask. These results highlight the potential of MLD-based hybrid resists for developing next-generation resist materials for micro/nanoelectronics manufacturing.

36 MATERIALS SCIENCE↗