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DOE OSTI2020

Probing Thermal Stability of Li-Ion Battery Ni-Rich Layered Oxide Cathodes by means of Operando Gas Analysis and Neutron Diffraction

Thermal stability is a crucial parameter that must be considered within the overall performance metrics of Ni-rich layered oxide cathodes. While the intrinsic structural stability of the cathode materials under thermal conditions is important, it is also critical to consider their reaction with electrolytes. In this study, operando gas analysis, ex situ neutron diffraction, and differential scanning calorimetry were combined to give a broader picture of the thermal stability of Ni-rich NMC cathodes. Li 1– x Ni 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) composite materials with four different states of charge were investigated with and without the presence of an electrolyte. It has been found that electrolyte can greatly accelerate both the structural and thermal decomposition of the cathode materials. A higher state of charge will also make cathode materials more susceptible to thermal shock. Without an electrolyte, O 2 release inducing a structural change from layered to rock salt was the major observation during thermal runaway. However, all samples retained some levels of layered structure after annealing up to 300 °C without the electrolyte. In comparison, almost all the O3-type layered phase transformed to the rock-salt phase for the cathode materials heated with the electrolyte at the same experimental conditions. Moreover, the amount of CO 2 increased by nearly two orders of magnitude when annealing cathode materials with electrolyte in operando gas analysis experiments. More delithiated NMC811 samples released larger amounts of CO 2 at earlier onset temperatures, resonating well with the differential scanning calorimetry (DSC) results showing that more delithiated samples release more heat during thermal shock.

25 ENERGY STORAGE↗

NASA NTRS1977

Linear magnetization feature associated with Rima Sirsalis

Measurements of the magnetic fields by the electron reflection method in the neighborhood of the long structural rille Rima Sirsalis show that a magnetic field with a strength of at least 100 nT (100 gammas) is present over a region of the order of 10 km in width and at least 300 km long. The center of the magnetized region closely parallels and is centered on the rille. The linear magnetization feature extends at least to latitude 8 deg S, 60 km beyond the place where the rille disappears at the edge of Oceanus Procellarum. This extension is coincident with the extrapolation of the rille based on photographs. However, the magnetization is much weaker or entirely absent at 5 deg S and has vanished at 0 deg latitude. These results suggest that the rille is indeed a structural feature and has associated with it magnetization, either in the form of intrusive magnetized rock or of a gap in an otherwise more or less uniformly magnetized layer of rock of large extent in two dimensions. Furthermore, the rille structure evidently is present for some distance beneath the lava flows of the Oceanus Procellarum basin.

Anderson, K. A.↗

NASA NTRS2010

Rapid Active Sampling Package

A field-deployable, battery-powered Rapid Active Sampling Package (RASP), originally designed for sampling strong materials during lunar and planetary missions, shows strong utility for terrestrial geological use. The technology is proving to be simple and effective for sampling and processing materials of strength. Although this originally was intended for planetary and lunar applications, the RASP is very useful as a powered hand tool for geologists and the mining industry to quickly sample and process rocks in the field on Earth. The RASP allows geologists to surgically acquire samples of rock for later laboratory analysis. This tool, roughly the size of a wrench, allows the user to cut away swaths of weathering rinds, revealing pristine rock surfaces for observation and subsequent sampling with the same tool. RASPing deeper (.3.5 cm) exposes single rock strata in-situ. Where a geologist fs hammer can only expose unweathered layers of rock, the RASP can do the same, and then has the added ability to capture and process samples into powder with particle sizes less than 150 microns, making it easier for XRD/XRF (x-ray diffraction/x-ray fluorescence). The tool uses a rotating rasp bit (or two counter-rotating bits) that resides inside or above the catch container. The container has an open slot to allow the bit to extend outside the container and to allow cuttings to enter and be caught. When the slot and rasp bit are in contact with a substrate, the bit is plunged into it in a matter of seconds to reach pristine rock. A user in the field may sample a rock multiple times at multiple depths in minutes, instead of having to cut out huge, heavy rock samples for transport back to a lab for analysis. Because of the speed and accuracy of the RASP, hundreds of samples can be taken in one day. RASP-acquired samples are small and easily carried. A user can characterize more area in less time than by using conventional methods. The field-deployable RASP used a Ni/Cad rechargeable battery. Power usage was less than 1 Wh/ cm3 even when sampling strong basalts, so many samples could be taken on a single battery charge.

Peters, Gregory↗

NASA NTRS1979

Preliminary results of penetrator field test program, Tonopah, Nevada, 16-28 April 1979

Subscale (0.63 scale) penetrators impacted various sizes of volcanic rocks resting on and within compacted plays sediments. All penetrators were identical in size, shape, weight, and impact velocity. Although minor variations in impact angle were documented, the final orientation of the buried penetrators was primarily a consequence of the size, shape, and depth of the rocks encountered during impact. In situ measurements of impacted penetrators revealed that surface and buried layers of rocks having diameters up to 3 times the penetrator diameter caused only small ( 10 deg) angles of deflection. Only large single rocks greater than 10 times the penetrator diameter caused deflections appreciably greater than 10 deg. The large deflection angles followed by the penetrator were strongly influenced by fracture planes that developed in the rock as it broke apart. No catastrophic failure of the penetrator occurred during these tests. A cross section of the path of each penetrator through the ground is shown together with details on orientation before, during, and after the tests. Comparisons are made with results of previous subscale penetrator tests, and conclusions are drawn with respect to full-scale Mars penetrator performance.

Blanchard, M. B.↗

NASA NTRS2006

Radar Probing of Planetary Regoliths: An Example from the Northern Rim of Imbrium Basin

Imaging radar measurements at long wavelengths (e.g., >30 cm) allow deep (up to tens of meters) probing of the physical structure and dielectric properties of planetary regoliths. We illustrate a potential application for a Mars orbital synthetic aperture radar (SAR) using new Earth-based 70-cm wavelength radar data for the Moon. The terrae on the northern margin of Mare Imbrium, the Montes Jura region, have diffuse radar backscatter echoes that are 2-4 times weaker at 3.8-cm, 70-cm, and 7.5-m wavelengths than most other lunar nearside terrae. Possible geologic explanations are (1) a pyroclastic deposit associated with sinuous rilles in this region, (2) buried mare basalt or a zone of mixed highland/basaltic debris (cryptomaria), or (3) layers of ejecta associated with the Iridum and Plato impacts that have fewer meter-sized rocks than typical highlands regolith. While radar data at 3.8-cm to 7.5-m wavelengths suggest significant differences between the Montes Jura region and typical highlands, the surface geochemistry and rock abundance inferred from Clementine UV-VIS data and eclipse thermal images are consistent with other lunar terrae. There is no evidence for enhanced iron abundance, expected for basaltic pyroclastic deposits, near the source vents of the sinuous rilles radial to Plato. The regions of low 70-cm radar return are consistent with overlapping concentric ''haloes'' about Iridum and Plato and do not occur referentially in topographically low areas, as is observed for radar-mapped cryptomaria. Thus we suggest that the extensive radar-dark area associated with the Montes Jura region is due to overlapping, rock-poor ejecta deposits from Iridum and Plato craters. Comparison of the radial extent of low-radar-return crater haloes with a model for ejecta thickness shows that these rock-poor layers are detected by 70-cm radar where they are on the order of 10 m and thicker. A SAR in orbit about Mars could use similar deep probing to reveal the nature of crater - and basin-related deposits.

Iridum crater↗

NASA NTRS1999

Autonomous Onboard Science Image Analysis for Future Mars Rover Missions

To explore high priority landing sites and to prepare for eventual human exploration, future Mars missions will involve rovers capable of traversing tens of kilometers. However, the current process by which scientists interact with a rover does not scale to such distances. Specifically, numerous command cycles are required to complete even simple tasks, such as, pointing the spectrometer at a variety of nearby rocks. In addition, the time required by scientists to interpret image data before new commands can be given and the limited amount of data that can be downlinked during a given command cycle constrain rover mobility and achievement of science goals. Experience with rover tests on Earth supports these concerns. As a result, traverses to science sites as identified in orbital images would require numerous science command cycles over a period of many weeks, months or even years, perhaps exceeding rover design life and other constraints. Autonomous onboard science analysis can address these problems in two ways. First, it will allow the rover to transmit only "interesting" images, defined as those likely to have higher science content. Second, the rover will be able to anticipate future commands. For example, a rover might autonomously acquire and return spectra of "interesting" rocks along with a high resolution image of those rocks in addition to returning the context images in which they were detected. Such approaches, coupled with appropriate navigational software, help to address both the data volume and command cycle bottlenecks that limit both rover mobility and science yield. We are developing fast, autonomous algorithms to enable such intelligent on-board decision making by spacecraft. Autonomous algorithms developed to date have the ability to identify rocks and layers in a scene, locate the horizon, and compress multi-spectral image data. Output from these algorithms could be used to autonomously obtain rock spectra, determine which images should be transmitted to the ground, or to aid in image compression. We will discuss these and other algorithms and demonstrate their performance during a recent rover field test.

Gulick, V. C.↗

DOE OSTI2025

Characterizing Stress Roughness at Utah FORGE Through Simulation of Hydraulic Fracture Growth During 16A Stage 3 Stimulation

In most geologic formations, the vertical gradient of the minimum horizontal stress (𝜎 h ) exceeds the hydrostatic gradient, often driving hydraulic fractures to propagate upward. However, observations indicate that the upward growth of real hydraulic fractures is less pronounced than theoretical predictions based on smoothly varying 𝜎 h fields. In fact, the layered structure of sedimentary rocks hinders fracture propagation across layers, partially explaining the limited height growth observed in practice (Zoback et al., 2022). While crystalline rocks lack the pervasive layered fabric of sedimentary formations, they still possess structural fabric formed over their geologic history, resulting in inherently "rough" in situ stress fields. Recent studies have identified another key factor: the "roughness" of in situ stress, characterized by temporal, relatively short-wavelength fluctuations superimposed on the overall stress gradient. This stress roughness leads to apparent toughness anisotropy, where the vertical toughness appears significantly larger than the horizontal toughness (P. Fu et al., 2019; Dontsov & Suarez-Rivera, 2021). Neglecting the effects of rock fabric and stress roughness can yield inaccurate predictions of hydraulic fracture geometry and growth rates at larger length scales.

58 GEOSCIENCES↗

DOE OSTI2020

Controlling Surface Phase Transition and Chemical Reactivity of O3-Layered Metal Oxide Cathodes for High-Performance Na-Ion Batteries

O3-layered metal oxides are promising cathode materials for high-energy Na-ion batteries (SIBs); however, they suffer from fast capacity fade. In this work, we develop a high-performance O3-NaNi 0.68 Mn 0.22 Co 0.10 O 2 cathode for SIBs toward practical applications by suppressing the formation of a rock salt layer at the cathode surface with an advanced electrolyte. The cathode can deliver a high specific capacity of ~196 mAh g –1 and demonstrates >80% capacity retention over 1000 cycles. NaNi 0.68 Mn 0.22 Co 0.10 O 2 –hard carbon full-cells with practical loading (>2.5 mAh cm –2 ) and lean electrolyte (~40 μL) demonstrate ~82% capacity retention after 450 cycles. A 60 mAh single-layer pouch cell has also been fabricated and demonstrated stable performance. This work represents a significant leap in SIB development and brings new insights to the development of advanced layered metal oxide cathodes for alkaline-ion batteries.

25 ENERGY STORAGE↗

NASA NTRS1999

Autonomous Image Analysis for Future Mars Missions

To explore high priority landing sites and to prepare for eventual human exploration, future Mars missions will involve rovers capable of traversing tens of kilometers. However, the current process by which scientists interact with a rover does not scale to such distances. Specifically, numerous command cycles are required to complete even simple tasks, such as, pointing the spectrometer at a variety of nearby rocks. In addition, the time required by scientists to interpret image data before new commands can be given and the limited amount of data that can be downlinked during a given command cycle constrain rover mobility and achievement of science goals. Experience with rover tests on Earth supports these concerns. As a result, traverses to science sites as identified in orbital images would require numerous science command cycles over a period of many weeks, months or even years, perhaps exceeding rover design life and other constraints. Autonomous onboard science analysis can address these problems in two ways. First, it will allow the rover to preferentially transmit "interesting" images, defined as those likely to have higher science content. Second, the rover will be able to anticipate future commands. For example, a rover might autonomously acquire and return spectra of "interesting" rocks along with a high-resolution image of those rocks in addition to returning the context images in which they were detected. Such approaches, coupled with appropriate navigational software, help to address both the data volume and command cycle bottlenecks that limit both rover mobility and science yield. We are developing fast, autonomous algorithms to enable such intelligent on-board decision making by spacecraft. Autonomous algorithms developed to date have the ability to identify rocks and layers in a scene, locate the horizon, and compress multi-spectral image data. We are currently investigating the possibility of reconstructing a 3D surface from a sequence of images acquired by a robotic arm camera. This would then allow the return of a single completely in focus image constructed only from those portions of individual images that lie within the camera's depth of field. Output from these algorithms could be used to autonomously obtain rock spectra, determine which images should be transmitted to the ground, or to aid in image compression. We will discuss these algorithms and their performance during a recent rover field test.

Gulick, V. C.↗

NASA NTRS1964

Packing properties of fine powders and the depth of the lunar dust layer

Previous experimental and theoretical studies by Hapke and Van Horn [1963] and Hapke [1963] of surfaces which reflect light like the moon support the hypothesis that the lunar surface is covered with a layer of fine rock dust. The material in this layer appears to be in an extremely unconsolidated state, having a bulk density of the order of one-eighth that of solid rock. Such photometric studies can give information concerning only the upper few millimeters of the lunar soil. However, analyses of radiofrequency observations indicate that extensive areas of the moon may be covered to depths of the order of a meter or greater by a substance which is also much less dense than solid rock. From the radar reflectivity of the lunar surface at meter wavelengths Evans [1962] infers a dielectric constant of K = 2.7; Troitsky [1962] estimates K = 1.6 on the basis of radio-thermal observations at centimeter wavelengths. Since the RF dielectric constants of stony meteorites and of terrestrial rocks range from about 4 to 45 [Fensler et al., 1962] it is clear that the density of the lunar soil is unusually low at least to depths to which RF radiation can penetrate; Troitsky estimates this depth to be of the order of 20 wavelengths or greater in the 3-cm-wavelength range.

Powder↗

NASA NTRS2012

The Gale Crater Mound in a Regional Geologic Setting

The Mars Science Laboratory Rover Curiosity is commencing a two-year investigation of Gale crater and Mt. Sharp, the crater s prominent central mound. Gale is a 155 km, late Noachian / early Hesperian impact crater located near the dichotomy boundary separating the southern highlands from the northern plains. The central mound is composed of layered sedimentary rock, with upper and lower mound units separated by a prominent erosional unconformity (Milliken et al., 2010). The lower mound is of particular interest, as it contains secondary minerals indicative of a striking shift from water-rich to water-poor conditions on early Mars. A key unknown in the history of Gale is the relationship between the sedimentary units in the mound and sedimentary sequences in the surrounding region. We employed orbital remote sensing data to determine if areas within a 1,000 km radius of Gale match the characteristics of sedimentary units in Mt. Sharp. Regions of interest were defined based on: the mound s inferred age (late Noachian to early Hesperian), altitude range (-4,600 m to +400 m), and THEMIS nighttime brightness (a proxy for thermal inertia). This combination of characteristics is matched by two extensive units, the late Noachian subdued cratered unit Npl2 and Noachian / Hesperian undivided material HNu (Greeley and Guest, 1987), located along the dichotomy. Geomorphic units have been mapped within the Gale mound by Thomson et al. (2011) based on albedo, layering and erosional characteristics. Using orbital CTX, MOC and HiRISE images we examined all areas within our regions of interest for analogous geomorphic units in the same altitude ranges as the corresponding units in Mt. Sharp. The most convincing geomorphic analogs to lower mound units, dominated by fine-scale layering and prominent yardangs, were located approximately 200 km northeast and southeast of Gale in late Noachian unit Npl2. The most convincing geomorphic analogs to upper mound layered units are located 250 900 km northwest of Gale in unit HNu, estimated to span the Noachian / Hesperian boundary.

Allen, Carlton C.↗

DOE OSTI2023

Constructing “Li-rich Ni-rich” oxide cathodes for high-energy-density Li-ion batteries

The current exploration of high-energy-density cathode materials for Li-ion batteries is mainly concentrated on either so-called “Li-rich” or “Ni-rich” oxides. However, both are suffering from formidable practical challenges. Here, we combine these two concepts to obtain “Li-rich Ni-rich” oxides in pursuit of more practical high-energy-density cathodes. As a proof of concept, we synthesized an array of Li 1+y Ni( 3-5y)/3 Mo 2y/3 O 2 oxides, whose structures were identified to be the coexistence of LiNiO 2 -rich and Li 4 MoO 5 -rich domains with the aid of XRD, TEM, and NMR techniques. Such an intergrowth structure of 5–20 nm size enables excellent mechanical and structural reversibility for the layered rock-salt LiNiO 2 -rich domain upon cycling thanks to the robust cubic rock-salt Li 4 MoO 5 -rich domain enabling an “epitaxial stabilization” effect. As a result, we achieved high capacities (>220 mA h g -1 ) with Ni contents as low as 80%; the Li 1.09 Ni 0.85 Mo 0.06 O 2 member (y = 0.09) shows much improved cycling performances (91% capacity retention for 100 cycles at C/10) compared with pure LiNiO 2 . Further, this work validates the feasibility of constructing Li-rich Ni-rich compounds in the form of intergrowing domains and hence unlocks vast possibilities for future cathode design.

25 ENERGY STORAGE↗

DOE OSTI2024

Densification of Cathode/Electrolyte Interphase to Enhance Reversibility of LiCoO 2 at 4.65 V

For LiCoO 2 (LCO) operated beyond 4.55 V (vs Li/Li + ), it usually suffers from severe surface degradation. Constructing a robust cathode/electrolyte interphase (CEI) is effective to alleviate the above issues, however, the correlated mechanisms still remain vague. Herein, a progressively reinforced CEI is realized via constructing Zr-O deposits (ZrO 2 and Li 2 ZrO 3 ) on LCO surface (i.e., Z-LCO). Upon cycle, these Zr-O deposits can promote the decomposition of LiPF6, and progressively convert to the highly dispersed Zr-O-F species. In particular, the chemical reaction between LiF and Zr-O-F species further leads to the densification of CEI, which greatly reinforces its toughness and conductivity. Further, combining the robust CEI and thin surface rock-salt layer of Z-LCO, several benefits are achieved, including stabilizing the surface lattice oxygen, facilitating the interface Li + transport kinetics, and enhancing the reversibility of O3/H1-3 phase transition, etc. As a result, the Z-LCO||Li cells exhibit a high capacity retention of 84.2% after 1000 cycles in 3–4.65 V, 80.9% after 1500 cycles in 3–4.6 V, and a high rate capacity of 160 mAh g -1 at 16 C (1 C = 200 mA g -1 ). This work provides a new insight for developing advanced LCO cathodes.

25 ENERGY STORAGE↗

DOE OSTI2026

Lattice-Oxygen-Driven Selective Oxidation Strategy for Stable Argyrodite Solid-State Lithium Metal Batteries

All-solid-state lithium metal batteries (ASSLMBs) with Li6PS5Cl argyrodite electrolytes and high-voltage LiNi0.8Mn0.1Co0.1O2 (NMC811) cathodes offer high energy density but suffer from rapid capacity fading due to the layered-to-rock-salt transition of NMC811 and structural degradation of Li6PS5Cl from parasitic interfacial reactions. Here, we demonstrate a catholyte engineering strategy using a Li2S scavenging additive to suppress interfacial reactivity and preserve the structural and electrochemical stability of both NMC811 and Li6PS5Cl. Incorporating 0.10 wt.% Li2S enables exceptional cycling stability, achieving 76% capacity retention after 550 cycles at C/10 and 88% retention after 800 cycles at C/3 at 60 degrees C, compared with rapid failure in pristine cells. Spectroscopic, electrochemical, and morphological analyses confirm that Li2S maintains electrode integrity by sustaining particle contact and suppressing phase decomposition. This work elucidates interfacial degradation pathways in NMC811/argyrodite systems and introduces a low-cost, scalable strategy to stabilize nickel-rich oxide cathodes in ASSLMBs, advancing their practical viability.

25 ENERGY STORAGE↗

DOE OSTI2022

Formation of Al 3 Sc in Al 0.8 Sc 0.2 thin films

We report the formation of Al 3 Sc, in 100 nm Al 0.8 Sc 0.2 films, is found to be driven by exposure to high temperature through higher deposition temperature or annealing. High film resistivity was observed in films with lower deposition temperature that exhibited a lack of crystallinity, which is anticipated to cause more electron scattering. An increase in deposition temperature allows for the nucleation and growth of crystalline Al 3 Sc regions that were verified by electron diffraction. The increase in crystallinity reduces electron scattering, which results in lower film resistivity. Annealing Al 0.8 Sc 0.2 films at 600 °C in an Ar vacuum environment also allows for the formation and recrystallization of Al 3 Sc and Al and yields saturated resistivity values between 9.58 and 10.5 μΩ-cm regardless of sputter conditions. Al 3 Sc was found to nucleate and grow in a random orientation when deposited on SiO 2 , and highly {111} textured when deposited on 100 nm Ti and AlN films that were used as template layers. The rocking curve of the Al 3 Sc 111 reflection for the as-deposited films on Ti and AlN at 450 °C was 1.79° and 1.68°, respectively. Annealing the film deposited on the AlN template reduced the rocking curve substantially to 1.01° due to recrystallization of Al 3 Sc and Al within the film.

36 MATERIALS SCIENCE↗

NASA NTRS1972

Craters formed in mineral dust by hypervelocity microparticles.

As a simulation of erosion processes on the lunar surface, impact craters were formed in dust targets by 2- to 5-micron-diameter polystyrene spheres with velocities between 2.5 and 12 km/sec. For weakly cohesive, thick targets of basalt dust with a maximum grain size comparable to the projectile diameter, the craters had an average projectile-to-diameter diameter ratio of 25, and the displaced mass was 3 orders of magnitude greater than the projectile mass. In a simulation of the effect of a dust covering on lunar rocks, a layer of cohesive, fine-grained basalt dust with a thickness nearly twice the projectile diameter protected a glass substrate from damage, but an area about 50 times the cross-sectional area of the projectile was cleared of all but a few grains. Impact damage was produced in glass under a thinner dust layer.

Vedder, J. F.↗

NASA NTRS1986

Organic S13C values vary slightly with salinity in microbial mats at Guerrero Negro, Baja California Sur, Mexico: Implications for stromatolite S13C values

Stromatolites, layered sedimentary rock structures produced by communities of microorganisms, constitute the most abundant early evidence of life on Earth. Microbial mats, which are found most frequently in hypersaline marine or hot spring environments, serve as useful modern analogs of stromatolitic communities. Biochemical studies of mats were conducted to assist in the interpretations of stromatolites. The data suggest that salinity effects are insufficient by themselves to cause the C-13 differences observed betwwen Precambrain stromatolites and modern microbial mats.

Desmarais, D. J.↗

NASA NTRS1992

The canyon system on Mars

Individual Martian equatorial troughs are described, and their stratigraphy, geomorphology and structure are discussed. Possible origins and the overall sequence of events are addressed. Wall rock, interior layered deposits, irregular floor deposits, fractured floor material, and surficial deposits are examined. Chasma walls, wall stability, pits and pit chains, tributary canyons, and the transition from troughs to channels are also discussed.

Lucchitta, B. K.↗