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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Brittle-to-Ductile Transition Temperature Decreases at the Microscale in Muscovite Mica

Characterizing the structural and chemical transitions of muscovite mica across various scales and thermal profiles is essential for ensuring the reliability of high-voltage power insulation, aerospace thermal barriers, and nanoscale semiconductor substrates under extreme operational stress. Here, we investigate notch fracture toughness $K^{n}_{Ic}$ of muscovite mica as a function of feature size w and temperature T with microscale shear testing. $K^{n}_{Ic}$ decreased and then stayed constant as w increased, likely from fabrication-induced changes to the microstructure and roughness. Moreover, $K^{n}_{Ic}$ initially decreased and then increased as temperature T increased, with the reversal in trend indicative of a brittle-to-ductile transition. Complementary Raman spectroscopy and molecular dynamics showed that the observed trends were due to an increase in bond lengths and a decrease in critical stresses/strains. In comparing the microscale results to macroscale counterparts, it was surmised that the decrease in brittle-to-ductile transition temperature was due to an increase in the dehydroxylation rate.

DelRio, Frank W. [Sandia National Laboratories (SN↗
NASA NTRS1997

Au Colloids Formed by Ion Implantation in Muscovite Mica Studied by Vibrational and Electronic Spectroscopes and Atomic Force Microscopy

Au was implanted into the (001) surface of Muscovite mica at an energy of 1.1 MeV and at doses of 1, 3, 6, and 10 x 10(exp 16) ions/cu cm. Optical spectra of the as-implanted samples revealed a peak at 2.28 eV (545 nm) which is attributed to the surface plasmon absorption of Au colloids. The infrared reflectance measurements show a decreasing reflectivity with increasing ion dose in the Si-O stretching region (900-1200 /cm). A new peak observed at 967 /cm increases with the ion dose and is assigned to an Si-O dangling bond. Atomic force microscopy images of freshly cleaved samples implanted with 6 and 10 x 10(exp 16) ions/sq cm indicated metal colloids with diameters between 0.9- 1.5 nm. AFM images of the annealed samples showed irregularly shaped structures with a topology that results from the fusion of smaller colloids.

Tung, Y. S.↗
DOE OSTI2025

Distribution of nickel(II) ions adsorbed at the muscovite mica (001)-water interface determined by in-situ resonant anomalous X-ray reflectivity

Mineral-water interfaces mediate adsorption, ion exchange, and secondary mineral formation that control element mobility in natural and engineered systems. Reliable prediction and control of these processes require a fundamental understanding of the interfacial structure that links adsorbed ion speciation to macroscopic sorption capacity and strength. Here, we determine atomic-scale changes in hydration and distribution of Ni(II) at the muscovite mica (001)-water interface using in situ high-resolution X-ray reflectivity (XR) and resonant anomalous X-ray reflectivity (RAXR) at 1 mM NiCl2 and pH 5.7. XR reveals reorganization of the primary hydration structure relative to that in deionized water: the water layer adsorbed in the cavity sites at a height of ~1.3 Å disappears, while distinct solution layers emerge at ~2.3, ~4.1, and ~5.6 Å above the basal oxygen plane. RAXR resolves three interfacial Ni(II) species: a dominant outer-sphere complex at 3.65 Å (~80% of the total coverage), a minor inner-sphere complex at 0.75 Å, and a low-coverage, more distant outer-sphere species at 5.63 Å. These three adsorbed Ni(II) species account for a total Ni(II) coverage of 0.54 ± 0.02 ion per unit cell area that compensates for the surface charge. These results highlight the role of interfacial hydration in controlling the speciation and stability of adsorbate cations on the negatively charged mica surface, providing quantitative insight into predicting the geochemical behavior of divalent metal cations in the aqueous environments.

Lee, Sang Soo↗
DOE OSTI2024

Insights into the structure and dynamics of K + ions at the muscovite–water interface from machine learning potential simulations

The surfaces of many minerals are covered by naturally occurring cations that become partially hydrated and can be replaced by hydronium or other cations when the surface is exposed to water or an aqueous solution. These ion exchange processes are relevant to various chemical and transport phenomena, yet elucidating their microscopic details is challenging for both experiments and simulations. Here, in this work, we make a first step in this direction by investigating the behavior of the native K + ions at the interface between neat water and the muscovite mica (001) surface with ab-initio -based machine learning molecular dynamics and enhanced sampling simulations. Our results show that the desorption of the surface K + ions in pure ion-free water has a significant free energy barrier irrespective of their local surface arrangement. In contrast, facile K + diffusion between mica’s ditrigonal cavities characterized by different Al/Si orderings is observed. This behavior suggests that the K + ions may favor a dynamic disordered surface arrangement rather than complete desorption when exposed to deionized water.

Ab-initio molecular dynamics↗
DOE OSTI2020

Nonclassical Behavior in Competitive Ion Adsorption at a Charged Solid–Water Interface

Ion adsorption at solid-water interfaces is commonly described by interactions between specific surface sites and adsorbed ions in classical models. However, energetic contributions from non-site-specific ion-ion interactions have not been explored systematically. Here, we report non-classical behaviors observed during competitive adsorption between Sr 2+ and Na + /Rb + at the negatively-charged muscovite mica (001)-water interface, revealing apparent controls of adsorbed ion speciation over the interfacial reactivity. In the absence of competing cations, Sr 2+ adsorbs in approximately equivalent proportions of inner-sphere and outer-sphere complexes, whereas it adsorbs predominantly as an outer-sphere complex in the presence of Na + /Rb + . This transformation of adsorbed Sr 2+ speciation significantly decreases its adsorption strength, as indicated by ~15-fold shift in the Sr 2+ adsorption edge concentration, compared to that calculated from a classical Langmuir isotherm model developed based on site-specific interactions. Finally, these observations highlight the importance of non-site-specific interactions in controlling the energetics of chemical reactions at the charged interface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

The Anisotropic Adsorption of De Novo Allosteric Two‐Component Protein Fibers on Mica Surfaces

Protein adsorption at solid–liquid interfaces underlies many biomedical and materials applications, yet the mechanisms governing adsorption of proteins and their assemblies remain poorly understood. Here we investigate de novo–designed proteins that self-assemble into three fibrillar morphologies — small (S), large (L), and helical (H)—on muscovite mica. S-fibers are metastable, forming first but diminishing as L- and H-fibers develop and deposit. Adsorption of both fibers and monomers depends on fiber morphology and solvent environment, which is modulated by the substrate. The anisotropic surface features of the fiber types—long axis of S- and L-fibers and helical grooves of H-fibers—correlate with specific crystallographic directions on mica (001). S- and L-fibers align along the unique lattice axis, while the substrate-facing groove of H-fibers preferentially aligns along the remaining symmetry-related directions. Increasing potassium chloride (KCl) concentrations to molar levels alters adsorption, decreasing monomer coverage relative to fibers. These observations, interpreted through the effect of interfacial interface, indicate that ion-mediated modulation of hydration layers governs electrostatic interactions and alignment. This study reveals how coupling between protein topography, substrate crystallography, and hydration structure dictates selective adsorption and orientation of protein assemblies, offering insights for rational biomolecular material design.

AFM↗
DOE OSTI2022

Chemomechanical weakening of muscovite quantified with in situ liquid nanoindentation

Abstract Chemomechanical weakening of layered phyllosilicate muscovite mica was studied as a function of chemical environment via in situ liquid-nanoindentation under four conditions (dry, deionized water, and two NaCl solutions of different pH). While traditional indentation analyses of layered materials with extreme mechanical anisotropy have been limited due to displacement bursts (pop-ins), here the bursts were used as proxies for delamination, fracture, and spalling events. Since displacement bursts during an indent represent a stochastic process, 120 indents were conducted for each condition to generate statistically significant amounts of data. In total, over 9000 bursts were assessed using a load–displacement threshold criterion, classifying this as a high-throughput nanoscale fracture technique. For each burst, initiation load, initiation displacement, plastic zone volume at initiation, and energy dissipation were analyzed. A power-law relationship between the burst load and burst energy was noted which separated the bursts into two continuous distributions: (1) bursts due only to the mechanics of the indent and (2) bursts due to both the mechanics of the indent and the environment. By using a cumulative probability distribution, it was found that the NaCl solutions decreased the minimum plastic zone volume necessary to initiate a displacement burst by an order of magnitude relative to the dry condition. Finally, the underlying mechanisms explaining the trends in initiation volume as a function of environment were discussed, with a focus on the chemomechanical degradation processes via chemical attack and cation exchange.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Room-Temperature Ferroelectric Epitaxial Nanowire Arrays with Photoluminescence

The development of large-scale, high-quality ferroelectric semiconductor nanowire arrays with interesting light-emitting properties can address limitations in traditional wide-bandgap ferroelectrics, thus serving as building blocks for innovative device architectures and next-generation high-density optoelectronics. Here, we investigate the optical properties of ferroelectric CsGeX 3 (X = Br, I) halide perovskite nanowires that are epitaxially grown on muscovite mica substrates by vapor phase deposition. Detailed structural characterizations reveal an incommensurate heteroepitaxial relationship with the mica substrate. Furthermore, photoluminescence that can be tuned from yellow-green to red emissions by varying the halide composition demonstrates that these nanowire networks can serve as platforms for future optoelectronic applications. In addition, the room-temperature ferroelectricity and ferroelectric domain structures of these nanowires are characterized using second harmonic generation (SHG) polarimetry. Finally, the combination of room-temperature ferroelectricity with photoluminescence in these nanowire arrays unlocks new avenues for the design of novel multifunctional materials.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2020

Wide bandwidth frequency-domain thermoreflectance: Volumetric heat capacity, anisotropic thermal conductivity, and thickness measurements

A frequency-domain thermoreflectance (FDTR) system with a frequency range of 1 Hz to 75 MHz is presented. The wide bandwidth of pump modulation frequency enables enhanced simultaneous thermophysical property characterization of bulk and thin-film materials. The wide bandwidth FDTR system is demonstrated with simultaneous measurements of in-plane and cross-plane thermal conductivities of sapphire and muscovite mica, thickness and thermal conductivity of gold/titanium thin films, and isotropic thermal conductivity and volumetric heat capacity of lithium niobate and silicon. Thermophysical properties measured with FDTR are compared to literature values or independent measurements for verification. Finally, at low frequencies, a negligible error was achieved in the numerical integration of the heat diffusion equation with a Gauss–Legendre quadrature method solved with 400 integration points and an upper integration limit of 16weff, where weff is the effective pump–probe 1/e2 radius.

Ziade, Elbara (ORCID:0000000249020497)↗
DOE OSTI2022

Rotational Dynamics and Transition Mechanisms of Surface-Adsorbed Proteins

Assembly of biomolecules at solid-water interfaces requires molecules to traverse complex orientation-dependent energy landscapes through processes that are poorly understood, largely due to the dearth of in-situ single molecule measurements and statistical analyses of the rotational dynamics that define directional selection. Emerging capabilities in high-speed atomic force microscopy and machine learning have allowed us to directly determine the orientational energy landscape and observe and quantify the rotational dynamics for protein nanorods on the surface of muscovite mica under a variety of conditions. Comparisons with kinetic Monte Carlo simulations show that the transition rates between adjacent orientation-specific energetic minima can largely be understood through traditional models of in-plane Brownian rotation across a biased energy landscape, with resulting transition rates that are exponential in the energy-barriers between states. However, transitions between more distant angular states are decoupled from barrier height, with jump-size distributions showing a power-law decay that is characteristic of a non-classical Levy-flight random walk, indicating that large jumps are enabled by alternative modes of motion via activated states. The findings provide new insights into the dynamics of biomolecules at solid-liquid interfaces that lead to self-assembly, epitaxial matching and other orientationally anisotropic outcomes and define a general procedure for exploring such dynamics with implications for hybrid biomolecular-inorganic materials design.

Orientational energy landscapes, Rotational dynami↗
NASA NTRS1974

Techniques for carrying out radiative transfer calculations for the Martian atmospheric dust

A description is given of the modification of a theory on the reflectance of particulate media so as to apply it to analysis of the infrared spectra obtained by the IRIS instrument on Mariner 9. With the aid of this theory and the optical constants of muscovite mica, quartz, andesite, anorthosite, diopside pyroxenite, and dunite, modeling calculations were made to refine previous estimates of the mineralogical composition of the Martian dust particles. These calculations suggest that a feldspar rich mixture is a very likely composition for the dust particles. The optical constants used for anorthosite and diopside pyroxenite were derived during this program from reflectance measurements. Those for the mica were derived from literature reflectance data. Finally, a computer program was written to invert the measured radiance data so as to obtain the absorption coefficient spectrum which should then be independent of the temperature profile and gaseous component effects.

Aronson, J. R.↗
NASA NTRS1975

Optical constants of minerals and rocks

Lorentz line parameters (and estimates of their standard deviations) have been empirically derived from measured reflectance data for muscovite mica, an anorthosite, a diopsidic pyroxenite, an almandite-pyrope garnet, and a soda lime glass. These parameters provide a useful starting point for computer calculations requiring optical constants as a function and are therefore given here. A novel method of fitting the reflectance data by least squares is described in detail, as is the statistical procedure for estimating the standard deviations of the parameters found.

Aronson, J. R.↗
NASA NTRS1995

Fission foil detector calibrations with high energy protons

Fission foil detectors (FFD's) are passive devices composed of heavy metal foils in contact with muscovite mica films. The heavy metal nuclei have significant cross sections for fission when irradiated with neutrons and protons. Each isotope is characterized by threshold energies for the fission reactions and particular energy-dependent cross sections. In the FFD's, fission fragments produced by the reactions are emitted from the foils and create latent particle tracks in the adjacent mica films. When the films are processed surface tracks are formed which can be optically counted. The track densities are indications of the fluences and spectra of neutrons and/or protons. In the past, detection efficiencies have been calculated using the low energy neutron calibrated dosimeters and published fission cross sections for neutrons and protons. The problem is that the addition of a large kinetic energy to the (n,nucleus) or (p,nucleus) reaction could increase the energies and ranges of emitted fission fragments and increase the detector sensitivity as compared with lower energy neutron calibrations. High energy calibrations are the only method of resolving the uncertainties in detector efficiencies. At high energies, either proton or neutron calibrations are sufficient since the cross section data show that the proton and neutron fission cross sections are approximately equal. High energy proton beams have been utilized (1.8 and 4.9 GeV, 80 and 140 MeV) for measuring the tracks of fission fragments emitted backward and forward.

Benton, E. V.↗