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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.

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At least 883 records · Page 49
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Materials Signatures of Metallic Phases (Final Report)

This report summarizes key accomplishments from a 2 year Laboratory Directed Research and Development (LDRD) project focused on advancing nanoscale characterization of metallic particulates and synthesis of laboratory-scale analogs. We successfully developed and refined nanoscale crystallography techniques with significantly improved spatial resolution and throughput compared to traditional transmission electron microscopy. We also established nanotomography capabilities for 3D particle reconstruction and began optimizing throughput for broader application. Additionally, we demonstrated the ability to relocate and characterize individual particles using atomic force microscopy (AFM), providing insights into hardness, conductivity, and magnetic behavior. On the synthesis front, we leveraged controlled and combustion-based methods to investigate annealing effects and rapid oxidation behavior of U–Fe–Ni compounds. These efforts collectively enhance our ability to characterize and interpret particulate formation and transformation under relevant conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Effect of Propagating Dopant Reactivity on Lattice Oxygen Loss in LLZO Solid Electrolyte Contacted with Lithium Metal

Lithium lanthanum zirconium oxide (LLZO) is widely known as the most stable solid electrolyte against lithium metal electrodes. This thermodynamic stability can be lost by the presence of dopants which are required to stabilize the cubic phase of LLZO and can be reduced by lithium metal. However, the role of oxygen in such reactions is taken for granted. In this work, the reduction of Nb-substituted LLZO (Nb-LLZO) is explored by Li metal and shows that interfacial reactions propagate and lead to the decomposition with substantial Nb 5+ reduction deep into the bulk electrolyte. Scanning Transmission Electron Microscopy with Energy Dispersive X-ray Spectroscopy and thermogravimetric analyses show much of the reduction is due to oxygen vacancies formed, leading to increased electronic conductivity mapped with conductive Atomic Force Microscopy. Density functional theory calculations indicate oxygen release is favored by increased excess lithiation of Nb-LLZO. Electrochemical impedance of polycrystalline Nb-LLZO shows the continuous evolution of ionically resistive interphases near the lithium metal interface with Nb-LLZO while single crystals show little reactivity at room temperature and self-limiting reduction at 60°C. This work underlines the role of grain boundaries in propagating destructive solid electrolyte reactions and highlights previously unseen mechanisms involving lattice oxygen in LLZO.

Li metal, solid-state electrolytes↗
DOE OSTI2024

De novo design of pH-responsive self-assembling helical protein filaments

Abstract Biological evolution has led to precise and dynamic nanostructures that reconfigure in response to pH and other environmental conditions. However, designing micrometre-scale protein nanostructures that are environmentally responsive remains a challenge. Here we describe the de novo design of pH-responsive protein filaments built from subunits containing six or nine buried histidine residues that assemble into micrometre-scale, well-ordered fibres at neutral pH. The cryogenic electron microscopy structure of an optimized design is nearly identical to the computational design model for both the subunit internal geometry and the subunit packing into the fibre. Electron, fluorescent and atomic force microscopy characterization reveal a sharp and reversible transition from assembled to disassembled fibres over 0.3 pH units, and rapid fibre disassembly in less than 1 s following a drop in pH. The midpoint of the transition can be tuned by modulating buried histidine-containing hydrogen bond networks. Computational protein design thus provides a route to creating unbound nanomaterials that rapidly respond to small pH changes.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Facile MoS 2 Growth on Reduced Graphene-Oxide via Liquid Phase Method

Single and few-layers MoS 2 were uniformly grown on the surface of chemically reduced graphene oxide (r-GO), via a facile liquid phase approach. The method is based on a simple functionalization of r-GO with oleyl amine which seems to affect significantly the MoS 2 way of growth. Scanning-transmission-electron microscopy (STEM) analysis revealed the presence of single-layer MoS 2 on the surface of a few-layers r-GO. This result was also confirmed by atomic-force microscopy (AFM) images. X-ray photoemission spectroscopy (XPS) and Raman spectroscopy were used for in-depth structural characterization. Furthermore, we have successfully applied the method to synthesize MoS 2 nanocomposites with multi wall carbon nanotubes (CN) and carbon nanofibers (CNF). The results demonstrate clearly the selective MoS 2 growth on both carbon-based supports.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Solutions Are the Problem: Ordered Two-Dimensional Covalent Organic Framework Films by Chemical Vapor Deposition

Covalent organic frameworks (COFs) are a promising class of crystalline polymer networks that are useful due to their high porosity, versatile functionality, and tunable architecture. Conventional solution-based methods of producing COFs are marred by slow reactions that produce powders that are difficult to process into adaptable form factors for functional applications, and there is a need for facile and fast synthesis techniques for making crystalline and ordered covalent organic framework (COF) thin films. In this work, we report a chemical vapor deposition (CVD) approach utilizing co-evaporation of two monomers onto a heated substrate to produce highly crystalline, defect-free COF films and coatings with hydrazone, imine, and ketoenamine COF linkages. Further, this all-in-one synthesis technique produces highly crystalline, 40 nm–1 μm-thick COF films on Si/SiO2 substrates in less than 30 min. Crystallinity and alignment were proven by using a combination of grazing-incidence wide-angle X-ray scattering (GIWAXS) and transmission electron microscopy (TEM), and successful conversion of the monomers to produce the target COF was supported by Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and UV–vis measurements. Additionally, we used atomic force microscopy (AFM) to investigate the growth mechanisms of these films, showing the coalescence of triangular crystallites into a smooth film. To show the wide applicability and scope of the CVD process, we also prepared crystalline ordered COF films with imine and ketoenamine linkages. These films show potential as high-quality size exclusion membranes, catalytic platforms, and organic transistors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Electrostatic imaging of encapsulated graphene

Devices made from two-dimensional (2D) materials such as graphene and transition metal dichalcogenides exhibit remarkable electronic properties of interest to many subdisciplines of nanoscience. Owing to their 2D nature, their quality is highly susceptible to contamination and degradation when exposed to the ambient environment. Protecting the 2D layers by encapsulation between hexagonal boron nitride (hBN) layers significantly improves their quality. Locating these samples within the encapsulant and assessing their integrity prior to further processing then becomes challenging. Here we show that conductive scanning probe techniques such as electrostatic force and Kelvin force microscopy make it possible to visualize the encapsulated layers, their charge environment and local defects on the sub-micrometer scale. Our techniques are employed without requiring electrical contact to the embedded layer, providing valuable feedback on the device's local electronic quality prior to any device etching or electrode deposition. We show that these measurement modes, which are simple extensions of atomic force microscopy, are perfectly suited for imaging encapsulated conductors and their local charge environments.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Topographic Evolution of Heat-Treated Nb Upon Electropolishing for SRF Applications

Surface finish plays an essential role in the performance of superconducting radio frequency cavities. Several surface treatments have been developed to reduce surface resistance at a moderate accelerating gradient. We investigated the effects of sequential electropolishing on samples vacuum heat-treated at 300 and 600 °C and N-doped Nb samples using atomic force microscopy. The N-doping process precipitates niobium nitrides within grains and, most notably, continuously and deeply along some grain boundaries. Upon electropolishing, the nitrides are preferentially removed leaving behind a topographically imperfect surface marked by relatively deep holes and grooves with low radius of curvature edges. The progression of magnetic field enhancement and superheating field suppression factors upon electropolishing were investigated using atomic force micrographs. While minor changes in magnetic field enhancement and superheating field suppression factors are observed for the 300 and 600 °C heat-treated Nb, substantial improvements are observed for N-doped Nb. In this system, the most severe topographic defects are the grain boundary grooves which substantially suppress the superheating field. We find that the severity of topographic defects is related to the N-doping process.

Lechner, Eric↗
DOE OSTI2021

Breaking a dative bond with mechanical forces

Bond breaking and forming are essential components of chemical reactions. Recently, the structure and formation of covalent bonds in single molecules have been studied by non-contact atomic force microscopy (AFM). Here, we report the details of a single dative bond breaking process using non-contact AFM. The dative bond between carbon monoxide and ferrous phthalocyanine was ruptured via mechanical forces applied by atomic force microscope tips; the process was quantitatively measured and characterized both experimentally and via quantum-based simulations. Our results show that the bond can be ruptured either by applying an attractive force of ~150 pN or by a repulsive force of ~220 pN with a significant contribution of shear forces, accompanied by changes of the spin state of the system. Our combined experimental and computational studies provide a deeper understanding of the chemical bond breaking process.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Low earth simulation and materials characterization

Oxygen plasma ashers and an electron cyclotron resonance (ECR) sources are currently being used for low Earth orbit (LEO) simulation. The suitability of each of these simulation techniques is considered. Thin film coatings are characterized by optical techniques, including variable-angle spectroscopic ellipsometry, optical spectrophotometry, and laser light scatterometry. Atomic force microscopy (AFM) has been used to characterize the surface morphology of thin aluminum films as a function of substrate temperature during deposition. Results on diamondlike carbon (DLC) films show that DLC degrades with simulated atomic oxygen (AO) exposure at a rate comparable to Kapton polyimide. Since DLC is not as susceptible as Kapton to environmental factors such as moisture absorption, it could potentially provide more accurate measurements of AO fluence on short space flights.

Synowicki, R. A.↗
DOE OSTI2025

Metal-organic chemical vapor deposition of MgGeN2 films on GaN and sapphire

MgGeN2 films were synthesized using metal-organic chemical vapor deposition on GaN/c-sapphire templates and c-plane sapphire substrates. Energy-dispersive x-ray spectroscopy was used to estimate the cation composition ratios. To mitigate magnesium evaporation, the films were grown at pyrometer temperature 745 °C with a wafer rotation speed of 1000 rpm. Growth rates were determined by fitting energy-dispersive x-ray spectroscopy spectra to film thicknesses using NIST DTSA-II software. The thickness estimates determined by this method were consistent with scanning transmission electron microscopy measurements done for selected samples. Scanning electron microscopy images revealed faceted surfaces indicative of a tendency toward three-dimensional growth. X-ray diffraction spectra confirmed that the films were highly crystalline and exhibited preferential orientation in alignment with the substrate. Atomic force microscopy measurements show that film thicknesses are consistent across samples grown on both GaN templates and sapphire substrates, with typical roughnesses around 10 nm. Transmittance spectra of films grown on double-side-polished sapphire substrates yielded band gaps of 4.28 ± 0.06 eV for samples exhibiting close-to-ideal stoichiometry. Comparison of the measured spectra with ab initio calculations are in good agreement both near the bandgap and at higher energies where excitation is into higher-lying bands. These findings provide insight into the growth and characterization of MgGeN2, contributing to the development of this material for potential applications in optoelectronics and power electronics.

Hu, Chenxi (ORCID:0000000236299660)↗
DOE OSTI2016

Visualising the molecular alteration of the calcite (104) – water interface by sodium nitrate

The reactivity of calcite, one of the most abundant minerals in the earth’s crust, is determined by the molecular details of its interface with the contacting solution. Recently, it has been found that trace concentrations of NaNO 3 severely affect calcite’s (104) surface and its reactivity. Here we combine molecular dynamics (MD) simulations, X-ray reflectivity (XR) and in situ atomic force microscopy (AFM) to probe the calcite (104) – water interface in the presence of NaNO 3 . Simulations reveal density profiles of different ions near calcite’s surface, with NO 3 – able to reach closer to the surface than CO 3 2– and in higher concentrations. Reflectivity measurements show a structural destabilisation of the (104) surfaces’ topmost atomic layers in NaNO 3 bearing solution, with distorted rotation angles of the carbonate groups and substantial displacement of the lattice ions. Nanoscale AFM results confirm the alteration of crystallographic characteristics, and the ability of dissolved NaNO 3 to modify the structure of interfacial water was observed by AFM force spectroscopy. Our experiments and simulations consistently evidence a dramatic deterioration of the crystals’ surface, with potentially important implications for geological and industrial processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Molecular-Level Control over Ionic Conduction and Ionic Current Direction by Designing Macrocycle-Based Ionomers

Poor ionic conductivity of the catalyst-binding, submicrometer- thick ionomer layers in energy conversion and storage devices is a huge challenge. However, ionomers are rarely designed keeping in mind the specific issues associated with nanoconfinement. Here, we designed nature-inspired ionomers (calix-2) having hollow, macrocyclic, calix[4]arene-based repeat units with precise, sub-nanometer diameter. In ≤100 nm-thick films, the in-plane proton conductivity of calix-2 was up to 8 times higher than the current benchmark ionomer Nafion at 85% relative humidity (RH), while it was 1-2 orders of magnitude higher than Nafion at 20-25% RH. Confocal laser scanning microscopy and other synthetic techniques allowed us to demonstrate the role of macrocyclic cavities in boosting the proton conductivity. The systematic self-assembly of calix-2 chains into ellipsoids in thin films was evidenced from atomic force microscopy and grazing incidence small-angle X-ray scattering measurements. Moreover, the likelihood of alignment and stacking of macrocyclic units, the presence of one-dimensional water wires across this macrocycle stacks, and thus the formation of long-range proton conduction pathways were suggested by atomistic simulations. We not only did see an unprecedented improvement in thin-film proton conductivity but also saw an improvement in proton conductivity of bulk membranes when calix-2 was added to the Nafion matrices. Nafion-calix-2 composite membranes also took advantage of the asymmetric charge distribution across calix[4]arene repeat units collectively and exhibited voltage-gating behavior. The inclusion of molecular macrocyclic cavities into the ionomer chemical structure can thus emerge as a promising design concept for highly efficient ion-conducting and ion-permselective materials for sustainable energy applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Supramolecular Nanosheets Assembled from Poly(ethylene glycol)- b -poly( N -(2-phenylethyl)glycine) Diblock Copolymer Containing Crystallizable Hydrophobic Polypeptoid: Crystallization Driven Assembly Transition from Filaments to Nanosheets

Supramolecular two-dimensional (2D) nanomaterials from block copolymers have received great interest for their unique structure and properties. In this work, we report the formation of ultrathin nanosheets from self-assembly of amphiphilic poly(ethylene glycol)- b -poly( N -(2-phenylethyl)glycine) (PEG- b -PNPE) diblock copolymers, which contain rigid crystallizable polypeptoid segment. The PEG- b -PNPE copolymers were synthesized via ring opening polymerization (ROP). The obtained PEG- b -PNPE diblock copolymers can spontaneously form highly ordered structures in PEG selective solvents such as water and methanol. The copolymers with short PNPE segment can directly form nanosheets in water, and the obtained 2D nanosheets have a uniform thickness of 4-5 nm. In contrast, the copolymers with relatively long PNPE segment can only assemble into nanosheets with the assistance of methanol. It is anticpated that the crystallization and π-π stacking of PNPE blocks play critical roles in the formation of the nanosheet as suggested by grazing incidence wide-angle X-ray scattering (GIWAXS). During the process of adding water into copolymer methanol solution, the nanosheets were observed to evolve from individual nanofibers, to parallel aligning nanofibers, and eventually to the nanosheet structures verified by transmission electron microscopy (TEM) and cryo-TEM characterizations. We demonstrated that the preassembled filament behave as a fundamental packing motif to align laterally and further fuse into platelet-like structures. The assembly structure evolution process was tracked by TEM, atomic force microscopy, and cryo-TEM techniques. The understandings of supramolecular 2D nanosheet formation offer a new opportunity to make hierarchical nanostructures from polypeptoids containing copolymers.

36 MATERIALS SCIENCE↗
DOE OSTI2017

A Mesocrystal‐Like Morphology Formed by Classical Polymer‐Mediated Crystal Growth

Abstract Growth by oriented assembly of nanoparticles is a widely reported phenomenon for many crystal systems. While often deduced through morphological analyses, direct evidence for this assembly behavior is limited and, in the calcium carbonate (CaCO 3 ) system, has recently been disputed. However, in the absence of a particle‐based pathway, the mechanism responsible for the creation of the striking morphologies that appear to consist of subparticles is unclear. Therefore, in situ atomic force microscopy is used to investigate the growth of calcite crystals in solutions containing a polymer additive known for its ability to generate crystal morphologies associated with mesocrystal formation. It is shown that classical growth processes that begin with impurity pinning of atomic steps, leading to stabilization of new step directions, creation of pseudo‐facets, and extreme surface roughening, can produce a microscale morphology previously attributed to nonclassical processes of crystal growth by particle assembly.

Smeets, Paul J. M.↗
NASA NTRS2018

Light Microscopy Module Biophysics - 4 (LMM-B4)

Compare incorporation of protein aggregates into growing protein crystals on ISS (International Space Station) and on Earth. Measure growth rates in 1g (1 gravity) versus microgravity (micro-g) for different size aggregates of proteins. Compare the defect density and crystal quality via fluorescent-based atomic force microscopy and X-ray diffraction quality of crystals grown at different rates in a 1g environment.

Penn, Benjamin G.↗
DOE OSTI2020

Squeezing Noise in Microscopy with Quantum Light

Quantum-enhanced microscopes capable of probing classically inaccessible material properties have drawn increasing interest, but most proof-of-principle quantum microscopes have not surpassed classical limits. Here, we discuss the promise and obstacles associated with the use of quantum light with reduced noise (‘squeezed’ light) for quantum-enhanced atomic force microscopy, bioimaging, magneto-optical measurements, and Raman spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Temperature controlled transformations of giant unilamellar vesicles of amphiphilic triblock copolymers synthesized via microfluidic mixing

We report on a simple approach for synthesis of temperature-responsive giant unilamellar vesicles (GUVs) from poly(N-vinylcaprolactam) 15 -block-poly(dimethylsiloxane) 65 -block-poly(N-vinylcaprolactam) 15 (PVCL 15 -PDMS65-PVCL 15 ) triblock copolymer and non-temperature responsive small and giant vesicles from novel poly(N-vinylpyrrolidone)-block-poly(dimethylsiloxane)-block-poly(N-vinylpyrrolidone) (PVPON 15 -PDMS 65 -PVPON 15 and PVPON 6- PDMS 30- PVPON 6 ) triblock copolymers using microfluidic mixing at 25 °C. We show that temperature-responsive PVCL 15 -PDMS 65- PVCL 15 GUVs with the average diameter of 1.4 ± 0.2 µm while being stable at room temperature for at least 14 days, transformed irreversibly into small vesicles of 168 ± 40 nm after incubation of their aqueous solution at 42 °C for 24 h. We hypothesized that this transformation is induced by local compressive stresses of the vesicle membrane due to the collapse of PVCL blocks above the copolymer lower critical solution temperature (LCST) leading to the decrease of the vesicle membrane thickness. Consequently, we found that the temperature-induced size transformation of the PVCL-based GUVs at 42°C can be suppressed by substituting PVCL with its hydrophilic homologue PVPON, or by suppressing the PVCL's LCST behavior through hydrogen-bonding with tannic acid molecules. In the former case, novel PVPON n -PDMS m -PVPON n triblock copolymers (n = 15, m = 65 and n = 6, m = 30) assemble into vesicles stable from 25 °C to 55 °C as confirmed by optical and electron microscopy, dynamic light scattering (DLS) and small-angle neutron scattering (SANS). In the latter, hydrogen bonding interactions of PVCL with the polyphenol tannic acid (TA) at room temperature resulted in stable PVCL-based GUVs at 42°C as confirmed by optical, electron, and atomic force microscopies. We also found that physical crosslinking of the PVCL corona through hydrogen bonding with TA in PVCL 15- PDMS 65- PVCL 15 GUVs will delay their low pH-induced degradation at 37°C by 48 h compared to non-modified GUVs. Our findings open opportunities for the development of temperature-regulated stable micro-vehicles that would change their structural characteristics in the physiologically relevant temperature range from 25 to 42°C and can be utilized for cell mimicking studies. The developed GUVs also have potential in theranostic drug delivery as substitutes for polymer microcapsules and lipid microbubbles as well as for stimuli-triggered sensing, protection, and rapid response in an aqueous environment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗