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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

High-Resolution Comonomer Sequencing of Blocky Brominated Syndiotactic Polystyrene Copolymers Using 13C NMR Spectroscopy and Computer Simulations

This work demonstrates the first high-resolution comonomer sequencing of Blocky brominated syndiotactic polystyrene (sPS-co-sPS-Br) copolymers based on pentad assign- ments of the quaternary carbon region of the nuclear magnetic resonance spectrum. Copolymers containing p-bromostyrene (Br-Sty) units were prepared in matched sets using postpolymerization bromination methods carried out in the heterogeneous gel state (Blocky) and homogeneous solution state (Random). Quantitative information from the quaternary carbon spectra, heteronuclear multiple bond correlation spectroscopy, electronic structure calculations, and simulated statistically random copolymers was correlated to confirm the carbon resonance assignments for all 20 possible pentad comonomer sequences. Using the experimental pentad sequence prevalences, a computer code was developed to simulate chains with microstructures typical of each sample as a means to visually represent the copolymer blockiness with quantitative precision. Based on the microstructure and distribution of run lengths in these chains, the simulations revealed that the Blocky copolymers contain a high degree of blockiness. By comparing the run lengths in the simulated chains to the average number of styrene units in a crystalline segment of sPS (found by small-angle X-ray scattering), copolymer crystallizability was predicted. For the simulated Blocky B-21% (21 mol % Br-Sty) chain, the probability of randomly selecting a styrene unit in a crystallizable block was 25.8%, while that in the simulated Random R-18% was zero, in excellent agreement with the experimental crystallization behavior measured by differential scanning calorimetry. Additionally, these predictions confirmed that the simulated chains accurately represent the ensemble of chains in their respective copolymer samples. Furthermore, each simulated Blocky chain contained one or more long sPS blocks that paralleled the measured 38-40 styrene units spanning a crystalline segment within the sPS/CCl4 gel. This finding affirmed that the long sPS segments originated from the precise lamellar structure within the heterogeneous gel morphology (i.e., block length is correlated with lamellar thickness). Overall, the ability to tailor the copolymer microstructure through control of the semicrystalline gel morphology opens the door to synthesizing ordered copolymers by postpolymerization functionalization processes with unprecedented levels of compositional control.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1979

Blocky craters - Implications about the lunar megaregolith

Radar, IR, and photogeologic properties of some 1310 lunar craters that have been catalogued as radar or IR anomalies, or both, are studied to determine whether a systematic difference in blocky craters exists between the lunar maria and terrae and whether this difference might be caused by a deep magaregolith of pulverized material forming the terra surface. Examination of Apollo orbital photography confirms that the radar and IR anomalies are correlated with blocky rubble around the craters, and analysis of the radar and IR data indicates systematic terra-mare differences. The data are interpreted by postulating that the maria are rock layers where craters eject boulder fields, that the terrae are covered by a relatively pulverized megaregolith at least 2 km deep, and that the terra craters eject less rocky rubble. It is concluded that blocky rubble, in the form of either actual rocks or partly consolidated blocks, contributes to the radar and IR signatures of the craters.

Thompson, T. W.↗
DOE OSTI2025

Blocky Selective Postpolymerization C–H Functionalization of Polyolefins

C–H functionalization of commodity polyolefins affords functional materials derived from a high-volume, low-cost resource. However, current postpolymerization modification strategies result in randomly distributed functionalization along the length of the polymer backbone, which has a negative impact on the crystallinity of the resultant polymers, and thus the thermomechanical properties. Here, we demonstrate an amidyl radical mediated C–H functionalization of polyolefins to access blocky microstructures, which exhibit a higher crystalline fraction, larger crystallite size, and improved mechanical properties compared to their randomly functionalized analogues. Taking inspiration from the site-selective C–H functionalization of small molecules, we leverage the steric protection provided by crystallites and target polymer functionalization to amorphous domains in a semicrystalline polyolefin gel. The beneficial outcomes of blocky functionalization are independent of the identity of the pendant functional group that is installed through functionalization. Here, the decoupling of functional group incorporation and crystallinity highlights the promise in accessing nonrandom microstructures through selective functionalization to circumvent traditional tradeoffs in postpolymerization modification, with potential impact in advanced materials and upcycling plastic waste.

Neidhart, Eliza K. [The University of North Caroli↗
DOE OSTI2021

Wide-blocky veins explained by dependency of crystal growth rate on fracture surface type: Insights from phase-field modeling

Vein microstructures contain a wealth of information on coupled chemical and mechanical processes of fracturing, fluid transport, and crystal growth. Numerical simulations have been used for exploring the factors controlling the development of vein microstructures; however, they have not been quantitatively validated against natural veins. Here we combined phase-field modeling with microtextural analysis of previously unexplained wide-blocky calcite veins in natural limestone and of the fresh fracture surface in this limestone. Results show that the wide-blocky vein textures can only be reproduced if ~10%–20% of crystals grow faster than the rest. This fraction corresponds to the amount of transgranularly broken grains that were observed on the experimental fracture surfaces, which are dominantly intergranular. We hypothesize that transgranular fractures allow faster growth of vein minerals due to the lack of clay coatings and other nucleation discontinuities that are common along intergranular cracks. Our simulation results show remarkable similarity to the natural veins and reproduce the nonlinear relationship between vein crystal width and vein aperture. This allows accurate simulations of crystal growth processes and related permeability evolution in fractured rocks.

Geology↗
DOE OSTI2020

Formation of wide-blocky calcite veins by extreme growth competition

Liassic limestones on the coast of Somerset in the UK contain dense arrays of calcite microveins with a common, but poorly understood microstructure, characterized by laterally wide crystals that form bridges across the vein. We investigated the mechanisms of formation and evolution of these ‘wide-blocky’ vein microstructures using a combination of high-resolution analytical methods, including virtual petrography, optical cathodoluminescence and scanning electron microscopy techniques (e.g. energy-dispersive X-ray spectrometry, back-scattered electron imaging, cathodoluminescence and electron back-scattered diffraction), laboratory experiments and multiphase field modelling. Our results indicate that the studied veins formed in open, fluid-filled fractures, each in a single opening and sealing episode. As shown by the optical and electron back-scattered diffraction images, the vein crystals grew epitaxially on grains of the wall rock and we hypothesize that their growth rates differed depending on whether the crystals were on a wall rock grain substrate that fractured intergranularly (slow growth rates) or transgranularly (rapid growth rates). Our multiphase field models support this hypothesis, showing that wide, blocky crystals only form where there are significant differences in the growth rate and are dependent on the type of seed grain. These results provide strong evidence for extreme growth competition, a process that we propose controls vein-filling in many micritic carbonate reservoirs, as well as demonstrate that the characteristics of the fracture wall can affect the filling processes in syntaxial veins. Supplementary material: The description and images of the studied thin sections are available at https://doi.org/10.6084/m9.figshare.c.5172371 . High-resolution optical microscopy mosaics (under plane-polarized- and crossed polarized light) of the thin section collection in PetroScan file format are available on request from the authors.

Geology↗
NASA NTRS1991

General patterns of flow field growth - Aa and blocky lavas

Lava flowfields consist of one or more flows. Four ideal emplacement regimes are recognized: that for single flows and that for flowfields dominated by (1) widening, (2) thickening, or (3) lengthening, as a result of generating new flows. Most aa and blocky lavas belong to the flowfield widening or single-flow regimes. These two regimes are analyzed assuming advance is controlled by the distal core of a flow, where motion is treated as steady, uniform, and laminar. Because of low deformation rates, the distal core is also approximated to a Newtonian fluid. Widening and, possibly, lengthening are ultimately limited by crustal resistance. After a critical cooling interval, new flows are generated from the upper reaches of the flowfield. A simple relation is derived linking flowfield dimensions and underlying slope to eruption duration, independent of terms involving gravity or lava chemistry and rheology. The relation well describes field data from several volcanoes (involving lava compositions from K phonolitic tephrite to dacite). This supports the premise that the overall growth of aa and blocky flowfields is systematic and also suggests that such growth may be predictable at timescales greater than, or similar to, the emplacement times of major flows.

Kilburn, Christopher R. J.↗
DOE OSTI2021

Scaling Theory of Neutral Sequence-Specific Polyampholytes

The primary sequence of charged monomers in a polyampholyte has a profound effect on its conformational properties. In this work, theory and simulations are used to predict how the sequence influences the single-chain behavior of globally neutral polyampholytes (PAs) under salt-free conditions. We consider PAs with Markov statistics of charges, where charge “blockiness” is defined by the correlation λ along the chain. These PAs cover a wide spectrum of primary sequences ranging from alternating (λ = –1) to ideally random (λ = 0) to diblock (λ → 1). In a theta solvent, sufficiently long PAs of any primary sequence form globules, but their internal structure, as well as the position and sharpness of the coil–globule transition, crucially depends on λ. Further, using scaling arguments, we demonstrate that the excess charge of the globule correlation volume (blob) increases with increasing λ, thereby inducing stronger Coulomb attractions between neighboring blobs of opposite charge and leading to higher density PA globules. Scaling predictions are supported by the results of the random phase approximation (RPA) and coarse-grained molecular dynamics simulations. A generalization to good and poor solvents is presented that enables the construction of the resulting scaling diagram of PA conformations in terms of solvent quality and charge blockiness, thereby providing a comprehensive molecular understanding of the role of the PA primary sequence in the chain structure.

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

Effect of Charged Block Length Mismatch on Double Diblock Polyelectrolyte Complex Micelle Cores

Polyelectrolyte complex micelles are hydrophilic nanoparticles that self-assemble in aqueous environments due to associative microphase separation between oppositely charged blocky polyelectrolytes. In this work, we employ a suite of physical characterization tools to examine the effect of charged block length mismatch on the equilibrium structure of double diblock polyelectrolyte complex micelles (D-PCMs) by mixing a diverse library of peptide and synthetic charged-neutral block polyelectrolytes with a wide range of charged block lengths (25–200 units) and chemistries. Early work on D-PCMs suggested that this class of micelles can only be formed from blocky polyelectrolytes with identical charged block lengths, a phenomenon referred to as chain length recognition. Here, we use salt annealing to create PCMs at equilibrium, which shows that chain length recognition, a longstanding hurdle to repeatable self-assembly from mismatched polyelectrolytes, can be overcome. Interestingly, D-PCM structure–property relationships display a range of values that vary systematically with the charged block lengths and chemical identity of constituent polyelectrolyte pairings and cannot be described by generalizable scaling laws. We discuss the interdependent growth behavior of the radius, ionic pair aggregation number, and density in the micelle core for three chemically distinct diblock pairings and suggest a potential physical mechanism that leads to this unique behavior. By comparing the results of these D-PCMs to the scaling laws recently developed for single diblock polyelectrolyte complex micelles (S-PCMs: diblock + homopolymer), we observe that D-PCM design schemes reduce the size and aggregation number and restrict their growth to a function of charged block length relative to S-PCMs. Understanding these favorable attributes enables more predictive use of a wider array of charged molecular building blocks to anticipate and control macroscopic properties of micelles spanning countless storage and delivery applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1974

Problems in the interpretation of lunar mare stratigraphy and relative ages indicated by ejecta from small impact craters

The numbers of large ejecta blocks in excess of several meters in diameter ('blockiness') around the rims of small craters in southeastern Mare Serenitatis exceed those around similar craters in southern Mare Imbrium (and some other regions) at all but the final stages of crater degradation. Terrestrial explosion crater analogs, studies of impact processes, and a layered mare model suggest that the nature of the layering in the subsurface, including lavas, ejecta and buried regolith horizons, could account for the variable blockiness of crater ejecta and, possibly, for some variation in crater size-frequency distributions. Such effects would limit the reliability and utility of counting postmare craters for the purpose of estimating the relative ages of mare surfaces. Similarly, comparisons of the effects of progressive degradation on small impact craters to determine relative or absolute ages of individual craters may be limited by the influence of stratigraphy on ejecta fragment size distributions, which would in turn affect micrometeorite erosion rates and regolith production models.

Young, R. A.↗
NASA NTRS1980

Remote sensing data of SP mountain and SP lava flow in north-central Arizona

Multifrequency airborne radar image data of SP Mountain and SP flow in north-central Arizona were obtained in diverse viewing directions and direct and cross-polarization and compared with surface and aerial photography, Landsat multispectral scanner data, airborne thermal infrared imagery, surface geology, and surface roughness statistics. The extremely blocky, basaltic andesite of SP flow is brighter on direct-polarization K-band images than on cross-polarized images taken simultaneously. This effect is explained by multiple scattering and the strong wavelength dependence of polarization effects caused by the rectilinear basaltic andesite scatters. Two distinct types of surface relief on SP flow, one extremely blocky, the other subdued, are clearly discriminated on the visible and thermal wavelength images but are separable only on the longer wavelength L-band radar image data.

Schaber, G. G.↗
NASA NTRS1991

Soil crusts on Mars

Three distinct soillike materials sampled by the Viking landers (VL) on Mars are (in order of increasing strength): (1) drift; (2) crusty to cloddy; and (3) blocky. Relative strengths of these materials are manifested by footpad penetrations during landing (VL 1), depths of deep holes, motor currents during sampling, sampler backhoe penetrations, comminutor motor currents, impact pits, trench tailings, and successful acquisitions of the coarse fraction (only blocky material). Cementation by S Cl compounds probably contributes to the relative strengths. This is shown where the weight pct. of SO3 + Cl of each material is plotted against their relative strengths. A similar result is obtained using SO3 alone, but not with Cl which is deficient in VL 2 samples.

Moore, H. J.↗
NASA NTRS1999

Location and Geologic Setting for the Three U.S. Mars Landers

Super resolution of the horizon at both Viking landing sites has revealed "new" features we use for triangulation, similar to the approach used during the Mars Pathfinder Mission. We propose alternative landing site locations for both landers for which we believe the confidence is very high. Super resolution of VL-1 images also reveals some of the drift material at the site to consist of gravel-size deposits. Since our proposed location for VL-2 is NOT on the Mie ejecta blanket, the blocky surface around the lander may represent the meter-scale texture of "smooth palins" in the region. The Viking Lander panchromatic images typically offer more repeat coverage than does the IMP on Mars Pathfinder, due to the longer duration of these landed missions. Sub-pixel offsets, necessary for super resolution to work, appear to be attributable to thermal effects on the lander and settling of the lander over time. Due to the greater repeat coverage (particularly in the near and mid-fields) and all-panchromatic images, the gain in resolution by super resolution processing is better for Viking than it is with most IMP image sequences. This enhances the study of textural details near the lander and enables the identification rock and surface textures at greater distances from the lander. Discernment of stereo in super resolution im-ages is possible to great distances from the lander, but is limited by the non-rotating baseline between the two cameras and the shorter height of the cameras above the ground compared to IMP. With super resolution, details of horizon features, such as blockiness and crater rim shapes, may be better correlated with Orbiter images. A number of horizon features - craters and ridges - were identified at VL-1 during the misison, and a few hils and subtle ridges were identified at VL-2. We have added a few "new" horizon features for triangulation at the VL-2 landing site in Utopia Planitia. These features were used for independent triangulation with features visible in Viking Orbiter and MGS MOC images, though the actual location of VL-1 lies in a data dropout in the MOC image of the area. Additional information is contained in the original extended abstract.

Parker, T. J.↗
NASA NTRS2005

Comparison of Morphologies of Apollo 17 Dust Particles with Lunar Simulant, JSC-1

Lunar dust (< 20 microns) makes up approx.20 wt.% of the lunar soil. Because of the abrasive and adhering nature of lunar soil, a detailed knowledge of the morphology (size, shape and abundance) of lunar dust is important for dust mitigation on the Moon. This represents a critical step towards the establishment of long-term human presence on the Moon (Taylor et al. 2005). Machinery design for in-situ resource utilization (ISRU) on the Moon also requires detailed information on dust morphology and general physical/chemical characteristics. Here, we report a morphological study of Apollo 17 dust sample 70051 and compare it to lunar soil stimulant, JSC-1. W e have obtained SEM images of dust grains from sample 70051 soil (Fig. 1). The dust grains imaged are composed of fragments of minerals, rocks, agglutinates and glass. Most particles consist largely of agglutinitic impact glass with their typical vesicular textures (fine bubbles). All grains show sub-angular to angular shapes, commonly with sharp edges, common for crushed glass fragments. There are mainly four textures: (1) ropey-textured pieces (typical for agglutinates), (2) angular shards, (3) blocky bits, and (4) Swiss-cheese grains. This last type with its high concentration of submicron bubbles, occurs on all scales. Submicron cracks are also present in most grains. Dust-sized grains of lunar soil simulant, JSC-1, were also studied. JSC-1 is a basaltic tuff with relatively high glass content (approx.50%; McKay et al. 1994). It was initially chosen in the early 90s to approximate the geotechnical properties of the average lunar soil (Klosky et al. 1996). JSC-1 dust grains also show angular blocky and shard textures (Fig. 2), similar to those of lunar dust. However, the JSC-1 grains lack the Swiss-cheese textured particles, as well as submicron cracks and bubbles in most grains.

Liu, Yang↗
NASA NTRS2012

The Origin of Ina: Evidence for Inflated Lava Flows on the Moon

Ina is an enigmatic volcanic feature on the Moon known for its irregularly shaped mounds, the origin of which has been debated since the Apollo Missions. Three main units are observed on the floor of the depression (2.9 km across, < or =64 m deep) located at the summit of a low-shield volcano: irregularly shaped mounds up to 20 m tall, a lower unit 1 to 5 m in relief that surrounds the mounds, and blocky material. Analyses of Lunar Reconnaissance Orbiter Camera images and topography show that features in Ina are morphologically similar to terrestrial inflated lava flows. Comparison of these unusual lunar mounds and possible terrestrial analogs leads us to hypothesize that features in Ina were formed through lava flow inflation processes. While the source of the lava remains unclear, this new model suggests that as the mounds inflated, breakouts along their margins served as sources for surface flows that created the lower morphologic unit. Over time, mass wasting of both morphologic units has exposed fresh surfaces observed in the blocky unit. Ina is different than the terrestrial analogs presented in this study in that the lunar features formed within a depression, no vent sources are observed, and no cracks are observed on the mounds. However, lava flow inflation processes explain many of the morphologic relationships observed in Ina and are proposed to be analogous with inflated lava flows on Earth.

Garry, W. B.↗
NASA NTRS2014

Improved Discrimination of Volcanic Complexes, Tectonic Features, and Regolith Properties in Mare Serenitatis from Earth-Based Radar Mapping

Radar images at 70 cm wavelength show 4-5 dB variations in backscatter strength within regions of relatively uniform spectral reflectance properties in central and northern Mare Serenitatis, delineating features suggesting lava flow margins, channels, and superposition relationships. These backscatter differences are much less pronounced at 12.6 cm wavelength, consistent with a large component of the 70 cm echo arising from the rough or blocky transition zone between the mare regolith and the intact bedrock. Such deep probing is possible because the ilmenite content, which modulates microwave losses, of central Mare Serenitatis is generally low (2-3% by weight). Modeling of the radar returns from a buried interface shows that an average regolith thickness of 10m could lead to the observed shifts in 70 cm echo power with a change in TiO2 content from 2% to 3%. This thickness is consistent with estimates of regolith depth (10-15m) based on the smallest diameter for which fresh craters have obvious blocky ejecta. The 70 cm backscatter differences provide a view of mare flow-unit boundaries, channels, and lobes unseen by other remote sensing methods. A localized pyroclastic deposit associated with Rima Calippus is identified based on its low radar echo strength. Radar mapping also improves delineation of units for crater age dating and highlights a 250 km long, east-west trending feature in northern Mare Serenitatis that we suggest is a large graben flooded by late-stage mare flows.

Radar echoes↗
NASA NTRS2016

Secondary Crater-Initiated Debris Flow on the Moon

In recent work, radar circular polarization echo properties have been used to identify "secondary" craters without distinctive secondary morphologies. Because of the potential for this method to improve our knowledge of secondary crater population-in particular the effect of secondary populations on crater- derived ages based on small craters-it is important to understand the origin of radar polarization signatures associated with secondary impacts. In this paper, we utilize Lunar Reconnaissance Orbiter Camera photographs to examine the geomorphology of secondary craters with radar circular polarization ratio enhancements. Our investigation reveals evidence of dry debris flow with an impact melt component at such secondary craters. We hypothesize that these debris flows were initiated by the secondary impacts themselves, and that they have entrained blocky material ejected from the secondaries. By transporting this blocky material downrange, we propose that these debris flows (rather than solely ballistic emplacement) are responsible for the tail-like geometries of enhanced radar circular polarization ratio associated with the secondary craters investigated in this work. Evidence of debris flow was observed at both clustered and isolated secondary craters, suggesting that such flow may be a widespread occurrence, with important implications for the mixing of primary and local material in crater rays.

Martin-Wells, K. S.↗
NASA NTRS2015

Lunar Crater Ejecta: Physical Properties Revealed by Radar and Thermal Infrared Observations

We investigate the physical properties, and changes through time, of lunar impact ejecta using radar and thermal infrared data. We use data from two instruments on the Lunar Reconnaissance Orbiter (LRO) - the Diviner thermal radiometer and the Miniature Radio Frequency (Mini-RF) radar instrument - together with Earth-based radar observations. We use this multiwavelength intercomparison to constrain block sizes and to distinguish surface from buried rocks in proximal ejecta deposits. We find that radar-detectable rocks buried within the upper meter of regolith can remain undisturbed by surface processes such as micrometeorite bombardment for greater than 3 Gyr. We also investigate the thermophysical properties of radar-dark haloes, comprised of fine-grained, rock-poor ejecta distal to the blocky proximal ejecta. Using Diviner data, we confirm that the halo material is depleted in surface rocks, but show that it is otherwise thermophysically indistinct from background regolith. We also find that radar-dark haloes, like the blocky ejecta, remain visible in radar observations for craters with ages greater than 3 Ga, indicating that regolith overturn processes cannot replenish their block populations on that timescale.

Ghent, R. R.↗