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Granular metals (GMs), consisting of metal nanoparticles separated by an insulating matrix, frequently serve as a platform for fundamental electron transport studies. However, few technologically mature devices incorporating GMs have been realized, in large part because intrinsic defects (e.g., electron trapping sites and metal/insulator interfacial defects) frequently impede electron transport, particularly in GMs that do not contain noble metals. Here, we demonstrate that such defects can be minimized in molybdenum–silicon nitride (Mo–SiNx) GMs via optimization of the sputter deposition atmosphere. For Mo–SiNx GMs deposited in a mixed Ar/N2 environment, x-ray photoemission spectroscopy shows a 40%–60% reduction of interfacial Mo-silicide defects compared to Mo–SiNx GMs sputtered in a pure Ar environment. Electron transport measurements confirm the reduced defect density; the dc conductivity improved (decreased) by 104–105 and the activation energy for variable-range hopping increased 10×. Since GMs are disordered materials, the GM nanostructure should, theoretically, support a universal power law (UPL) response; in practice, that response is generally overwhelmed by resistive (defective) transport. Here, the defect-minimized Mo–SiNx GMs display a superlinear UPL response, which we quantify as the ratio of the conductivity at 1 MHz to that at dc, Δ σ ω. Remarkably, these GMs display a Δ σ ω up to 107, a three-orders-of-magnitude improved response than previously reported for GMs. By enabling high-performance electric transport with a non-noble metal GM, this work represents an important step toward both new fundamental UPL research and scalable, mature GM device applications. [ABSTRACT FROM AUTHOR]

Multivalent rechargeable metal batteries offer a safer, more sustainable, and higher energy density alternative to lithium-ion batteries, though several challenges remain. Recent demonstrations of room-temperature reversible electrodeposition and dissolution of Ca metal indicate that it is possible to stabilize metallic Ca anodes with spontaneously formed solid electrolyte interphases (SEIs). However, further progress toward the goal of an energy-efficient, long cycle-life Ca anode requires correlating interphase identity with electrode performance. In this work, we demonstrate that the SEI formed from calcium borohydride solvated in tetrahydrofuran, an electrolyte that supports reversible Ca deposition, is a compositionally and structurally heterogeneous oxide, sufficiently thin to support Ca2+ cation transmission while stabilizing Ca from corrosive loss during long-term electrolyte contact. The significant advance demonstrated here is that ionically nonconductive materials, like calcium oxide, can form cation-transmissive interphases in which conductivity can be tailored through control of heterogeneity, providing an approach for stabilizing reactive metal electrodes.

Bimetallic, reactive multilayers are uniformly structured materials composed of alternating sputter-deposited layers that may be ignited to produce self-propagating mixing and formation reactions. These nanolaminates are most commonly used as rapid-release heat sources. The specific chemical composition at each metal/metal interface determines the rate of mass transport in a mixing and formation reaction. The inclusion of engineered diffusion barriers at each interface will not only inhibit solid-state mixing but also may impede the self-propagating reactions by introducing instabilities to wavefront morphology. This work examines the effect of adding diffusion barriers on the propagation of reaction waves in Co/Al multilayers. The Co/Al system has been shown to exhibit a reaction propagation instability that is dependent on the bilayer thickness, which allows for the occurrence of unstable modes in otherwise stable designs from the inclusion of diffusion barriers. Based on the known stability criteria in the Co/Al multilayer system, the way in which the inclusion of diffusion barriers changes a multilayer's heat of reaction, thermal conductivity, and material mixing mechanisms can be determined. These factors, in aggregate, lead to changes in the wavefront velocity and stability. [ABSTRACT FROM AUTHOR]

The Microscopy Society of America (MSA) has awarded several major awards for outstanding contributions to microscopy and microanalysis. The winners of the 2024 MSA major Society awards and MSA Fellows are highlighted in this article. The recipients include W. Gray "Jay" Jerome, J. Murray Gibson, Wu Zhou, Florian Schüder, Michael J. Zachman, Kathleen B. Reuter, Ilke Arslan, Lou Germinario, Adam Hitchcock, Yuichi Ikuhara, Ping Lu, K. Andre Mkhoyan, Velimir R. Radmilovic, David Tomlin, and Huolin Xin. Each individual has made significant contributions to the field of microscopy and microanalysis, with expertise ranging from lipid biology to AI-powered techniques for TEM. [Extracted from the article]

Nanothermite NiO–Al is a promising material system for low gas emission heat sources; yet, its reactive properties are highly dependent on material processing conditions. In the current study, sputter deposition is used to fabricate highly controlled nanolaminates comprised of alternating NiO and Al layers. Films having an overall stoichiometry of 2Al to 3NiO were produced with different bilayer thicknesses to investigate how ignition and self-sustained, high temperature reactions vary with changes to nanometer-scale periodicity and preheat conditions. Ignition studies were carried out with both hot plate and laser irradiation and compared to slow heating studies in hot-stage x-ray diffraction. Ignition behavior has bilayer thickness and heating rate dependencies. The 2Al/3NiO with λ ≤ 300 nm ignited via solid/solid diffusion mixing (activation energy, Ea = 49 ± 3 kJ/mole). Multilayers having λ≥ 500 nm required a more favorable mixing kinetics of solid/liquid dissolution into molten Al (Ea = 30 ± 4 kJ/mole). This solid/liquid dissolution Ea is a factor of 5 lower than that of the previously reported powder compacts due to the elimination of a passivating Al oxide layer present on the powder. The reactant mixing mechanism between 300 and 500 nm bilayer thicknesses was dependent on the ignition source's heating rate. The self-propagating reaction velocities of 2Al/3NiO multilayers varied from 0.4 to 2.5 m/s. Pre-heating nanolaminates to temperatures below the onset reaction temperatures associated with forming intermediate nickel aluminides at multilayer interfaces led to increased propagation velocities, whereas pre-heating samples above the onset temperatures inhibited subsequent attempts at laser ignition. [ABSTRACT FROM AUTHOR]

Ge2Sb2Te5 (GST-225) has been the most used active material in nonvolatile phase-change memory devices. Understanding the kinetics and dynamics involved in crystallization is critical for the optimization of materials and devices. A GST-225 thin film of 20 nm thickness was prepared by sputtering directly onto a Protochip and left uncapped and exposed to atmosphere for approximately 1 year. Early stages of crystallization and growth of the film have been studied inside the TEM from room temperature to 140 °C. The morphological and structural transformations have been studied by a Cs-corrected environmental TEM, and images have been recorded using a high-speed low electron dose camera (Gatan K3 IS). The amorphous to crystalline transformation has been observed at ∼35 °C. From the large field, high-resolution images obtained using the Gatan K3 IS camera early crystallization can be detected and nucleation rates and growth velocities can be obtained. [ABSTRACT FROM AUTHOR]

In this letter, we demonstrated stable nanoscale fracture in single-crystal silicon using an in-situ wedge-loaded double cantilever beam (DCB) specimen. The fracture toughness KIC was calculated directly from instrumented measurement of force and displacement via finite element analysis with frictional corrections. Measurements on multiple test specimens were used to show KIC = 0.72 ± 0.07 MPa m1/2 on {111} planes and observe the crack-growth resistance curve in <500 nm increments. The exquisite stability of crack growth, instrumented measurement of material response, and direct visual access to observe nanoscale fracture processes in an ideally brittle material differentiate this approach from prior DCB methods. In-situ fracture toughness experiments on single-crystal silicon revealed stable nanoscale fracture and identified the shape of the crack-growth resistance curve, role of fabrication-induced artifacts, and origin of fracture surface features. [ABSTRACT FROM AUTHOR]

The major focus of this study was to examine the feasibility of applying diamond-like nanocomposite (DLN) coatings on the sidewalls of Ni alloy parts fabricated using lithographie, galvanoformung and abformung (LIGA: a German acronym that means lithography, electroforming, and molding) for friction and wear control. Planar test coupons were employed to understand the friction mechanisms in regimes relevant to LIGA microsytems. Friction tests were conducted on planar test coupons as well as between LIGA-fabricated test structures in planar-sidewall and sidewall-sidewall configurations. Measurements were made in dry nitrogen and air with 50% relative humidity by enclosing the friction tester in an environmental chamber. In contrast to bare metal-metal contacts, minimal wear was exhibited for the DLN-coated LIGA NiMn alloy parts and test coupons. The low friction behavior of DLN was attributed to its ability to transfer to the rubbing counterface providing low interfacial shear at the sliding contact. The coating coverage and chemistry on the sidewalls and the substrate-coating interface integrity were examined by transmission electron microscopy, Automated eXpert Spectral Image Analysis, and electron backscatter diffraction on cross sections prepared by focused ion beam microscopy. The role of novel characterization techniques to evaluate the surface coatings for LIGA microsystems technology is highlighted. [2008-0007] Index Terms--Coatings, electron microscopy, friction.

High-Entropy Alloys (HEAs) are proposed as materials for a variety of extreme environments, including both fission and fusion radiation applications. To withstand these harsh environments, materials processing must be tailored to their given application, now achieved through additive manufacturing processes. However, radiation application opportunities remain limited due to an incomplete understanding of the effects of irradiation on HEA performance. In this letter, we investigate the response of additively manufactured refractory high-entropy alloys (RHEAs) to helium (He) ion bombardment. Through analytical microscopy studies, we show the interplay between the alloy composition and the He bubble size and density to demonstrate how increasing the compositional complexity can limit the He bubble effects, but care must be taken in selecting the appropriate constituent elements. [ABSTRACT FROM AUTHOR]

Buried resistors in low-temperature co-fired ceramics were studied to determine processing, microstructure, and electric properties.

We study the impact of irradiation on magnetic tunnel junction (MTJ) films with perpendicular magnetic anisotropy (PMA) and spin–orbit torque (SOT) switching using magneto-optical Kerr effect and transmission electron microscopy. Our results show that the thin-film stack is robust to gamma ionizing dose up to 1 Mrad(Si) and Ta1+ ion irradiation fluences up to 1012 ions/cm2, showing SOT PMA MTJs are radiation-hard. But, at very high Ta1+ ion irradiation between 1012 and 1014 ions/cm2, reduced coercivity and eventually greatly reduced PMA are observed, corresponding with an increase in intermixing of the CoFeB–MgO layers, particularly at the lower CoFeB–MgO interface. These results agree with displacement damage modeling that predicts higher damage in the layers closer to the bottom heavy metal and substrate. Compared to spin transfer torque and in-plane anisotropy MTJs, needing a top-pinned stack, a thicker heavy metal layer, and perpendicular anisotropy that is pinned out of plane by interfaces, all could make SOT PMA MTJs more susceptible to damage at high doses. [ABSTRACT FROM AUTHOR]

Airborne contaminants from fires containing nuclear waste represent significant health hazards and shape the design and operation of nuclear facilities. Much of the data used to formulate DOE-HDBK-3010-94, "Airborne Release Fractions/Rates and Respirable Fractions for Nonreactor Nuclear Facilities," from the U.S. Department of Energy, were taken over 40 years ago. The objectives of this study were to reproduce experiments from Pacific Northwest Laboratories conducted in June 1973 employing current aerosol measurement methods and instrumentation, develop an enhanced understanding of particulate formation and transport from fires containing nuclear waste, and provide modeling and experimental capabilities for updating current standards and practices in nuclear facilities. A special chamber was designed to conduct small fires containing 25 mL of flammable waste containing lutetium nitrate, ytterbium nitrate, or depleted uranium nitrate. Carbon soot aerosols showed aggregates of primary particles ranging from 20 to 60 nm in diameter. In scanning electron microscopy, ~200-nm spheroidal particles were also observed dispersed among the fractal aggregates. The 200-nm spherical particles were composed of metal phosphates. Airborne release fractions (ARFs) were characterized by leaching filter deposits and quantifying metal concentrations with mass spectrometry. The average mass-based ARF for 238U experiments was 1.0 × 10−3 with a standard deviation of 7.5 × 10−4. For the original experiments, DOE-HDBK-3010-94 states, "Uranium ARFs range from 2 × 10−4 to 3 × 10−3, an uncertainty of approximately an order of magnitude." Thus, current measurements were consistent with DOE-HDBK-3010-94 values. ARF values for lutetium and ytterbium were approximately one to two orders of magnitude lower than 238U. Metal nitrate solubility may have varied with elemental composition and temperature, thereby affecting ARF values for uranium surrogates (Yb and Lu). In addition to ARF data, solution boiling temperatures and evaporation rates can also be deduced from experimental data. [ABSTRACT FROM AUTHOR]