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At least 235 records · Page 13

All sources NASA NTRS DOE OSTI

DOE OSTI2014

Effects of helium implantation on the tensile properties and microstructure of Ni₇₃P₂₇ metallic glass nanostructures

We report fabrication and nanomechanical tension experiments on as-fabricated and helium-implanted ~130 nm diameter Ni₇₃P₂₇ metallic glass nano-cylinders. The nano-cylinders were fabricated by a templated electroplating process and implanted with He⁺ at energies of 50, 100, 150, and 200 keV to create a uniform helium concentration of ~3 at. % throughout the nano-cylinders. Transmission electron microscopy (TEM) imaging and through-focus analysis reveal that the specimens contained ~2 nm helium bubbles distributed uniformly throughout the nano-cylinder volume. In-situ tensile experiments indicate that helium-implanted specimens exhibit enhanced ductility as evidenced by a 2-fold increase in plastic strain over as-fabricated specimens, with no sacrifice in yield and ultimate tensile strengths. This improvement in mechanical properties suggests that metallic glasses may actually exhibit a favorable response to high levels of helium implantation.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Solubility-mediated sustained release enabling nitrate additive in carbonate electrolytes for stable lithium metal anode

Here, the physiochemical properties of the solid-electrolyte interphase, primarily governed by electrolyte composition, have a profound impact on the electrochemical cycling of metallic lithium. Herein, we discover that the effect of nitrate anions on regulating lithium deposition previously known in ether-based electrolytes can be extended to carbonate-based systems, which dramatically alters the nuclei from dendritic to spherical, albeit extremely limited solubility. This is attributed to the preferential reduction of nitrate during solid-electrolyte interphase formation, and the mechanisms behind which are investigated based on the structure, ion-transport properties, and charge transfer kinetics of the modified interfacial environment. To overcome the solubility barrier, a solubility-mediated sustained-release methodology is introduced, in which nitrate nanoparticles are encapsulated in porous polymer gel and can be steadily dissolved during battery operation to maintain a high concentration at the electroplating front. As such, effective dendrite suppression and remarkably enhanced cycling stability are achieved in corrosive carbonate electrolytes.

25 ENERGY STORAGE↗

DOE OSTI2020

Enabling “lithium-free” manufacturing of pure lithium metal solid-state batteries through in situ plating

Abstract The coupling of solid-state electrolytes with a Li-metal anode and state-of-the-art (SOA) cathode materials is a promising path to develop inherently safe batteries with high energy density (>1000 Wh L −1 ). However, integrating metallic Li with solid-electrolytes using scalable processes is not only challenging, but also adds extraneous volume since SOA cathodes are fully lithiated. Here we show the potential for “Li-free” battery manufacturing using the Li 7 La 3 Zr 2 O 12 (LLZO) electrolyte. We demonstrate that Li-metal anodes >20 μm can be electroplated onto a current collector in situ without LLZO degradation and we propose a model to relate electrochemical and nucleation behavior. A full cell consisting of in situ formed Li, LLZO, and NCA is demonstrated, which exhibits stable cycling over 50 cycles with high Coulombic efficiencies. These findings demonstrate the viability of “Li-free” configurations using LLZO which may guide the design and manufacturing of high energy density solid-state batteries.

25 ENERGY STORAGE↗

DOE OSTI2019

Hybrid dynamic windows using reversible metal electrodeposition and ion insertion

Dynamic windows with electronically controlled transmission reduce glare without obstructing views while increasing the energy efficiency of buildings and automobiles via lighting, heating and cooling savings. Electrochromic materials, which change colour with voltage, are widely explored for use in dynamic windows, but they have not been extensively commercialized due to problems associated with colour, cost, switching speed and durability. Here, we develop a class of dynamic windows that combines reversible metal electrodeposition with ion insertion chemistry. These devices function through the reversible electroplating of Bi and Cu at the working electrode and Li+ insertion in a nickel oxide counter electrode. In one minute, 100 cm 2 windows uniformly switch between a clear state with 75% transmission and a colour-neutral black state possessing 10% transmission, which represents a significant improvement over previous metal-based architectures. We demonstrate that these hybrid windows cycle at least 4,000 times without degradation and are compatible with flexible substrates. Finally, we discuss how this approach can be used to design practical large-scale windows.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Heterogeneous doping via nanoscale coating impacts the mechanics of Li intrusion in brittle solid electrolytes

Lithium dendrite intrusion in solid-state batteries limits fast charging and causes short-circuiting, yet the underlying regulating mechanisms are not well-understood. Here, in this work, we discover that heterogeneous Ag + doping dramatically affects lithium intrusion into Li 6.6 La 3 Zr 1.6 Ta 0.4 O 12 (LLZO), a brittle solid electrolyte. Nanoscale Ag + doping is achieved by thermally annealing a 3-nm-thick metallic coating on LLZO, inducing Ag–Li ion exchange and Ag diffusion into grains and grain boundaries. Density functional theory calculations and experimental characterization show negligible impact on the electronic properties and surface wettability from Ag + incorporation. Mechanically, nanoindentation experiments show a fivefold increase in the mechanical force required to fracture the surface Ag + -doped LLZO, indicating substantial doping-induced surface toughening. Operando microprobe scanning electron microscopy experiments show that the Ag + -doped LLZO surface exhibits improved lithium plating at >250 mA cm −2 and an electroplating diameter that is expanded by over fourfold, even under an extreme indentation stress of 3 GPa. This demonstrates enhanced defect tolerance in LLZO, rather than electronic or adhesion effects. Our study reveals a chemo-mechanical mechanism via surface heterogeneous doping, complementing present bulk design rules to minimize mechanical failures in solid-state batteries.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Design for reliability of BEoL and 3-D TSV structures – A joint effort of FEA and innovative experimental techniques

Copper-TSVs for 3D-IC-integration generate novel challenges for reliability analysis and prediction, e.g. the need to master multiple failure criteria for combined loading including residual stress, interface delamination, cracking and fatigue issues. So, the thermal expansion mismatch between copper and silicon leads to a stress situation in silicon surrounding the TSVs which is influencing the electron mobility and as a result the transient behavior of transistors. Furthermore, pumping and protrusion of copper is a challenge for Back-end of Line (BEoL) layers of advanced CMOS technologies already during manufacturing. These effects depend highly on the temperature dependent elastic-plastic behavior of the TSV-copper and the residual stresses determined by the electro deposition chemistry and annealing conditions. That’s why the authors pushed combined simulative/experimental approaches to extract the Young’s-modulus, initial yield stress and hardening coefficients in copper-TSVs from nanoindentation experiments, as well as the temperature dependent initial yield stress and hardening coefficients from bow measurements due to electroplated thin copper films on silicon under thermal cycling conditions. A FIB trench technique combined with digital image correlation is furthermore used to capture the residual stress state near the surface of TSVs. The extracted properties are discussed and used accordingly to investigate the pumping and protrusion of copper-TSVs during thermal cycling. Moreover, the cracking and delamination risks caused by the elevated temperature variation during BEoL ILD deposition are investigated with the help of fracture mechanics approaches.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Effect of a hard sublayer on contact interaction and wear behavior of electrodeposited gold-based coatings

The mechanical properties and wear of electroplated Au–Ni coatings deposited on beryllium bronze substrates with Ni or Ni–B intermediate layers were investigated. It was revealed that the sublayer material has no significant effect on the hardness and the elastic modulus of the coatings. At the same time, the harder sublayer favors localization of plastic deformation and, thus, strain hardening of coatings in the course of tribological tests. The Ni–B sublayer was shown to provide significant wear reduction of Au–Ni coatings as compared with the Ni sublayer.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

Physical mechanisms of copper-copper wafer bonding

The study of the physical mechanisms driving Cu-Cu wafer bonding allowed for reducing the bonding temperatures below 200 °C. Metal thermo-compression Cu-Cu wafer bonding results obtained at such low temperatures are very encouraging and suggest that the process is possible even at room temperature if some boundary conditions are fulfilled. Sputtered (PVD) and electroplated Cu thin layers were investigated, and the analysis of both metallization techniques demonstrated the importance of decreasing Cu surface roughness. For an equal surface roughness, the bonding temperature of PVD Cu wafers could be even further reduced due to the favorable microstructure. Their smaller grain size enhances the length of the grain boundaries (observed on the surface prior bonding), acting as efficient mass transfer channels across the interface, and hence the grains are able to grow over the initial bonding interface. Due to the higher concentration of random high-angle grain boundaries, this effect is intensified. The model presented is explaining the microstructural changes based on atomic migration, taking into account that the reduction of the grain boundary area is the major driving force to reduce the Gibbs free energy, and predicts the subsequent microstructure evolution (grain growth) during thermal annealing.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Eliminating the non-Gaussian spectral response of X-ray absorbers for transition-edge sensors

Transition-edge sensors (TESs) as microcalorimeters for high-energy-resolution X-ray spectroscopy are often fabricated with an absorber made of materials with high Z (for X-ray stopping power) and low heat capacity (for high resolving power). Bismuth represents one of the most compelling options. TESs with evaporated bismuth absorbers have shown spectra with undesirable and unexplained low-energy tails. We have developed TESs with electroplated bismuth absorbers over a gold layer that are not afflicted by this problem and that retain the other positive aspects of this material. To better understand these phenomena, we have studied a series of TESs with gold, gold/evaporated bismuth, and gold/electroplated bismuth absorbers, fabricated on the same die with identical thermal coupling. Lastly, we show that the bismuth morphology is linked to the spectral response of X-ray TES microcalorimeters.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Isotopic targets with graphene backing

Many of the isotopes cannot be made as free-standing targets and require thin film backing. Low-Z backing materials, such as amorphous carbon and thin polymer films are materials of choice for some experiments. However, the limitations of these backing materials are poor thermal and mechanical stability. All-carbon graphene films would be an excellent choice as a backing material due to their high thermal conductivity, high temperature tolerance (3550ºC melting point), low outgassing, mechanical integrity, and ease of handling. We fabricated a variety of targets using graphene material as a backing or a host matrix. Using PVD sputtering deposition of boron-11 carbide, we fabricated 11 B target with a 0.5 mg/cm 2 on graphene film. The 11 B isotope is of interest due to aneutronic proton–boron fusion reaction 1 p + 11 B → 3 4 He + 8.7 MeV suitable for clean energy production1. We also prepared a neutron rich natCr target on graphene backing by electroplating Cr in an aqueous chromium (III) oxide bath. The chromium target can be used for production of positron emitting Mn radioisotope2 in the reaction 52 Cr (p,n) 52 Mn. One of the unique advantages of the graphene film fabrication process is the capability to embed target materials, including refractory metals, in the nanoparticle form into a host graphene matrix during target preparation. Finally, we fabricated nat Ir, nat Re, nat WO3, and nat HfO 2 nanoparticle-loaded graphene targets that can be used in nuclear physics research.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Thin-film X-ray filters on microstructured substrates and their thermophysical properties

It is shown that structured substrates having micron- or submicron-sized through holes and coated with an ultrathin organic film can be used for the fabrication of thin-film X-ray filters via direct growth of functional layers on a substrate by sputter deposition, without additional complex processing steps. An optimised process is considered for the fabrication of X-ray filters on support structures in the form of electroplated fine nickel grids and on track-etched polymer membranes with micron- and submicron-diameter through pores. ‘Optimisation’ is here taken to mean matching the sputter deposition conditions with the properties of substrates so as to avoid overheating. The filters in question are intended for both imaging and single-channel detectors operating in the soft X-ray and vacuum UV spectral regions, at wavelengths from 10 to 60 nm. Thermal calculations are presented for the heating of ultrathin layers of organic films and thin-film support substrates during the sputter deposition of aluminium or other functional materials. The paper discusses approaches for cooling thin-film composites during the sputter deposition process and the service of the filters in experiments and gives a brief overview of the works that utilised filters produced by the described technique on microstructured substrates, including orbital solar X-ray research in the framework of the CORONAS programme and laboratory laser plasma experiments. (invited paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2017

The Design and Use of Tungsten Coated TZM Molybdenum Tile Inserts in the DIII-D Tokamak Divertor

Future tokamak devices are envisioned to utilize a high-Z metal divertor with tungsten as theleading candidate. However, tokamak experiments with tungsten divertors have seen significantdetrimental effects on plasma performance. The DIII-D tokamak presently has carbon as theplasma facing surface but to study the effect of tungsten on the plasma and its migration aroundthe vessel, two toroidal rows of carbon tiles in the divertor region were modified with high-Zmetal inserts, composed of a molybdenum alloy (TZM) coated with tungsten. A dedicated twoweek experimental campaign was run with the high-Z metal inserts. One row was coated withtungsten containing naturally occurring levels of isotopes. The second row was coated withtungsten where the isotope 182W was enhanced from the natural level of 26% up to greater than90%. The different isotopic concentrations enabled the experiment to differentiate between thetwo different sources of metal migration from the divertor. Various coating methods wereexplored for the deposition of the tungsten coating, including chemical vapor deposition,electroplating, vacuum plasma spray, and electron beam physical vapor deposition. The coatingswere tested to see if they were robust enough to act as a divertor target for the experiment. Testsincluded cyclic thermal heating using a high power laser and high-fluence deuterium plasmabombardment. The issues associate with the design of the inserts (tile installation, thermal stress,arcing, leading edges, surface preparation, etc.), are reviewed. The results of the tests used toselect the coating method and preliminary experimental observations are presented.

Holtrop, Kurt↗

DOE OSTI2017

Process Developments in the Fabrication of Depleted Uranium Hohlraums

Research at General Atomics and Lawrence Livermore National Laboratory has been focused on evaluating depleted uranium (DU) hohlraum fabrication over the past 10 years to improve the yield, thereby increasing the availability of DU hohlruams required to support the increased shot rate at the National Ignition Facility. The more straightforward gold (Au) hohlraum fabrication involves four basic steps: mandrel fabrication, electroplating, back machining and milling, and leaching. For Au, the overall fabrication yield of this process approaches 98%. Depleted uranium lined hohlraum fabrication, however, requires deposition of a multilayer of thin films after the mandrel fabrication step. These thin film deposition processes have historically proven difficult to execute on a complex cylindrical geometry of a hohlraum, resulting in unacceptable stress-driven delamination, with net yields ranging 20% to 35%. Recent hohlraum design and fabrication process changes, as well as material selections implemented between 2014 and 2016, have improved the fabrication yield to over 60%. Additionally, these changes are discussed here as well as plans for future improvements.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2020

Multi-metallic conduction cooled superconducting radio-frequency cavity with high thermal stability

Superconducting radio-frequency cavities are commonly used in modern particle accelerators for applied and fundamental research. Such cavities are typically made of high-purity, bulk Nb and with cooling by a liquid helium bath at a temperature of ~2 K. The size, cost and complexity of operating a particle accelerator with a liquid helium refrigerator make the current cavity technology not favorable for use in industrial-type accelerators. We have developed a multi-metallic 1.495 GHz elliptical cavity conductively cooled by a cryocooler. The cavity has a ~2 µm thick layer of Nb 3 Sn on the inner surface, exposed to the rf field, deposited on a ~3 mm thick bulk Nb shell and a bulk Cu shell, of thickness $\geqslant\! 5$ mm deposited on the outer surface by electroplating. A bolt-on Cu plate 1.27 cm thick was used to thermally connect the cavity equator to the second stage of a Gifford-McMahon cryocooler with a nominal capacity of 2 W at 4.2 K. The cavity was tested initially in liquid helium at 4.3 K and reached a peak surface magnetic field of ~36 mT with a quality factor of 2 × 10 9 . The cavity cooled by the cryocooler achieved a peak surface magnetic field of ~29 mT, equivalent to an accelerating gradient of 6.5 MV m –1 . The conduction-cooled cavity could be operated in continuous-wave with as high as 5 W dissipation in the cavity for 1 h without any thermal breakdown, because of the Cu outer layer with high thermal conductivity. This result represents a paradigm shift in the technology of superconducting accelerator cavities.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2024

An experimental study to investigate magnetic field and winding force-dependent contact resistance of NI REBCO coil

Abstract This paper reports the magnetic field and winding force-dependent contact resistance, also known as characteristic resistance, of no-insulation (NI) REBCO coil. Three NI coils were wound with different winding forces ( < 1 kgf, 3 kgf, and 5 kgf) using the same REBCO-coated conductor, and they were tested at 4.2 K in a background field of 0, 5, 10, and 14 T. The contact resistance of each coil is measured at each field. As a result of the measurements, we draw two conclusions. First, a quadratic function for magnetic field intensity reasonably reproduces the measurement results of each NI test coil’s magnetic field-dependent contact resistance, where the practical fit function’s coefficients are determined depending on the winding force. Second, the contact resistance of each coil is partially inconsistent with the magnetoresistance of the electroplated material, i.e. copper, of the REBCO-coated conductor. This paper will present the measurement results in detail, discuss them with Kohler’s rule, and formulate the contact resistance using winding force and magnetic field terms.

Bang, Jeseok (ORCID:0000000247616334)↗

DOE OSTI2026

Effects of stabilizer strength on the delamination strength of ReBCO coated conductors

Delamination strengths (DSs) of ReBCO tapes were evaluated using a transverse tensile anvil test. This study first demonstrated that the electromechanical DS is nearly equivalent to the purely mechanical DS for ReBCO tapes exhibiting abrupt delamination behavior. Mechanical DS was then examined for tapes with and without stabilizer edges to assess the influence of stabilizer strength. Scanning electron microscopy/energy-dispersive x-ray spectroscopy analysis revealed the delamination sites and crack propagation in ReBCO tapes. Further investigation revealed that the DS of ReBCO tapes is primarily determined by two factors: (1) interfacial bonding strength between the layers and (2) mechanical strength of the stabilizer edges. These findings point to a potential approach to enhancing DS by increasing the strength of the stabilizer (e.g. by optimizing the Cu electroplating process).

Cu stabilizer↗

DOE OSTI2020

A Digital Twin Approach to Study Additive Manufacturing Processing Using Embedded Optical Fiber Sensors and Numerical Modeling

One of the major challenges for metal-powder-based additive manufacturing is measuring and mitigating residual strain induced during the manufacturing processes. This article reports distributed fiber optic sensors embedded in Inconel alloy components as experimental means to validate numerical models of additive manufacturing process. Electroplating was used to deposit a metal protective jacket onto standard telecom single-mode fibers for strain measurements, Fiber sensors were embedded in an Inconel alloy substrate using the laser engineered net shaping (LENS) process. Here by using a Rayleigh-scattering optical frequency domain reflectometer (OFDR), temperature changes, and residual strain in the metal substrate were monitored with 5 mm spatial resolution during the LENS process. Using finite element analysis, temperature and strain profiles induced by the LENS deposition processes were also numerically studied. Discrepancies between the simulated temperature and strain profiles and those measured directly were less than 10%. Results presented in this article demonstrates a digital twin approach to fuse modeling results with distributed fiber sensor measurement data to study additive manufacturing process toward design and fabrication process optimization.

36 MATERIALS SCIENCE↗

DOE OSTI2018

III–V Solar Cells Grown on Unpolished and Reusable Spalled Ge Substrates

Substrate reuse offers a promising route toward enabling high-efficiency III-V solar cells to become cost-competitive for one-sun terrestrial applications. In this study, Ge films were spalled using an electroplated Ni stressor layer, and the fracture surface was characterized. Initial heteroepitaxial GaAs films grown on spalled Ge substrates by hydride vapor phase epitaxy were found to be single crystal with nearly equivalent growth rates between growth on epi-ready and unpolished spalled Ge substrates. We show the first demonstration of III-V solar cells (GaInAsP, E g ~ 1.7 eV) grown on unpolished spalled Ge substrates to assess the viability of substrate reuse. We demonstrate equivalent performance for a solar cell grown on spalled Ge and on a coloaded epi-ready Ge substrate, despite the residual roughness on the spalled Ge substrate and the lack of any substrate surface preparation. This initial demonstration of combining substrate reuse with the ability to grow III-V solar cells using a high growth rate and high throughput deposition process is a promising step toward low-cost III-V photovoltaics.

14 SOLAR ENERGY↗