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At least 775 records · Page 43
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Method for eliminating runout of braze filler metal during active brazing

Nanometers thick conformal coatings deposited by atomic-layer deposition (ALD) onto the metal surface of an active braze joint modifies the surface chemistry to eliminate excess braze filler metal flow. Unlike other means used to prevent braze filler metal runout, the thin ALD coating does not hinder next assembly processes, does not require post-braze cleaning, and does not alter the base material mechanical properties.

Goeke, Ronald S.↗
DOE OSTI2022

Methods for forming electrocatalyst structures and electrodes comprising same

Described herein are methods of forming an electrocatalyst structure on an electrode, comprising depositing a first layer on the electrode using atomic layer deposition (ALD), wherein the first layer comprises a plurality of discrete nanoparticles of a first electrocatalyst, and depositing one or more of a second layer on the first layer and the electrode using ALD, wherein the one or more second layer comprises a second electrocatalyst, wherein the first layer and the one or more second layers, collectively, form a multi-layer electrocatalyst structure on the electrode. Also described are electrodes having a multi-layer electrocatalyst structure. This abstract is intended as a scanning tool for purposes of searching in the particular art and is not intended to be limiting of the present disclosure.

Song, Xueyan↗
DOE OSTI2024

Metal fluoride passivation coatings prepared by atomic layer deposition for Li-ion batteries

The fabrication of robust interfaces between transition metal oxides and non-aqueous electrolytes is one of the great challenges of lithium ion batteries. Atomic layer deposition (ALD) of aluminum tungsten fluoride (AlWxFy) improves the electrochemical stability of LiCoO 2 . AlWxFy thin films were deposited by combining trimethylaluminum and tungsten hexafluoride. in-situ quartz crystal microbalance and transmission electron microscopy studies show that the films grow in a layer-by-layer fashion and are amorphous nature. Ultrathin AlWxFy coatings (<10 Å) on LiCoO 2 significantly enhance stability relative to bare LiCoO 2 when cycled to 4.4 V. The coated LiCoO 2 exhibited superior rate capability (up to 400 mA/g) and discharge capacities at a current of 400 mA/g were 51% and 92% of the first cycle capacities for the bare and AlWxFy coated materials. These results open new possibilities for designing ultrathin and electrochemically robust coatings of metal fluorides via ALD to enhance the stability of Li-ion electrodes.

Mane, Anil U.↗
DOE OSTI2018

Sinter-Resistant Platinum Catalyst Supported by Metal-Organic Framework

Installed on the zirconia nodes of a metal-organic framework (MOF) NU-1000 via targeted vapor-phase synthesis. The catalytic Pt clusters, site-isolated by organic linkers, are shown to exhibit high catalytic activity for ethylene hydrogenation while exhibiting resistance to sintering up to 200 degrees C. In situ IR spectroscopy reveals the presence of both single atoms and few-atom clusters that depend upon synthesis conditions. Operando X-ray absorption spectroscopy and Xray pair distribution analyses reveal unique changes in chemical bonding environment and cluster size stability while on stream. Density functional theory calculations elucidate a favorable reaction pathway for ethylene hydrogenation with the novel catalyst. Lastly, these results provide evidence that atomic layer deposition (ALD) in MOFs is a versatile approach to the rational synthesis of size-selected clusters, including noble metals, on a high surface area support.

36 MATERIALS SCIENCE↗
DOE OSTI2021

The effects of SMSI on m-Cresol Hydrodeoxygenation over Pt/Nb 2 O 5 and Pt/TiO 2

The hydrodeoxygenation (HDO) of m-cresol was studied on Pt/Nb 2 O 5 /MgAl 2 O 4 and Pt/TiO 2 /MgAl 2 O 4 catalysts to understand the effects of Strong Metal Support Interactions (SMSI). The Nb 2 O 5 and TiO 2 supports were prepared as 0.7-nm films on MgAl 2 O 4 by Atomic Layer Deposition (ALD) to ensure that the structures of the catalyst were the same. When reduced at 773 K to place Pt in the encapsulated state, Pt/Nb 2 O 5 /MgAl 2 O 4 was much less active than Pt/MgAl 2 O 4 at 573 K but much more active at 623 K. While Pt/MgAl 2 O 4 deactivated rapidly due to coking, Pt/Nb 2 O 5 /MgAl 2 O 4 showed significantly better coke tolerance and was almost 100% selective towards toluene production. Pt/Nb 2 O 5 /MgAl 2 O 4 reduced at lower temperatures exhibited intermediate catalytic properties. The effect of reduction temperature on Pt/TiO 2 /MgAl 2 O 4 was much less and this catalyst was more similar to Pt/MgAl 2 O 4 than its Nb 2 O 5 counterpart. Lastly, the implications of these results for understanding the nature of oxide promoters on HDO of m-cresol are discussed.

09 BIOMASS FUELS↗
DOE OSTI2017

Helium interactions with alumina formed by atomic layer deposition show potential for mitigating problems with excess helium in spent nuclear fuel

Helium gas accumulation from alpha decay during extended storage of spent fuel has potential to compromise the structural integrity the fuel. We report results obtained with surrogate nickel particles which suggest that alumina formed by atomic layer deposition can serve as a low volume-fraction, uniformly-distributed phase for retention of helium generated in fuel particles such as uranium oxide. Thin alumina layers may also form transport paths for helium in the fuel rod, which would otherwise be impermeable. Micron-scale nickel particles, representative of uranium oxide particles in their low helium solubility and compatibility with the alumina synthesis process, were homogeneously coated with alumina approximately 3–20 nm by particle atomic layer deposition (ALD) using a fluidized bed reactor. Particles were then loaded with helium at 800 °C in a tube furnace. Subsequent helium spectroscopy measurements showed that the alumina phase, or more likely a related nickel/alumina interface structure, retains helium at a density of at least 10 17 atoms/cm 3 . High resolution transmission electron microscopy revealed that the thermal treatment increased the alumina thickness and generated additional porosity. Results from Monte Carlo simulations on amorphous alumina predict the helium retention concentration at room temperature could reach 10 21 atoms/cm 3 at 400 MPa, a pressure predicted by others to be developed in uranium oxide without an alumina secondary phase. This concentration is sufficient to eliminate bubble formation in the nuclear fuel for long-term storage scenarios, for example. Finally, measurements by others of the diffusion coefficient in polycrystalline alumina indicate values several orders of magnitude higher than in uranium oxide, which then can also allow for helium transport out of the spent fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

Progress in durability of metal-supported solid oxide fuel cells with infiltrated electrodes

High power density and longevity are required to commercialize solid oxide fuel cells for vehicular applications. In this work, electrochemical durability of high-performance metal-supported solid oxide fuel cells (MS-SOFCs) with infiltrated catalysts is investigated. Durability screening of various cathode and anode compositions is conducted. The Pr 6 O 11 cathode and SDCN 40 (40 vol% Ni-60 vol% SDC) anode are selected due to preferential tradeoff between performance and durability. X-ray diffraction indicates the catalyst phases are stable after prolonged thermal annealing. Electrochemical impedance and scanning electron microscopy analyses show that the evolution of SDCN40 is minimal, and coarsening and Cr poisoning of the Pr 6 O 11 catalyst are the dominant degradation mechanisms. These degradation mechanisms are addressed by implementing three additional fabrication steps: (1) preoxidation of the metal support, (2) deposition of thin and protective atomic layer deposition (ALD) coatings throughout the cathode-side electrode and support, and (3) in situ pre-coarsening of the catalysts. A favorable tradeoff is achieved: the combination of the three fabrication steps reduces degradation rate at 0.7 V and 700 °C by two orders of magnitude to 2.3% kh -1 , while sacrificing 35% of initial power density. The catalyst pre-coarsening step is primarily responsible for the loss of performance.

25 ENERGY STORAGE↗
DOE OSTI2018

Improved Coking Resistance of “Intelligent” Ni Catalysts Prepared by Atomic Layer Deposition

Conformal CaTiO 3 films were deposited onto MgAl 2 O 4 by atomic layer deposition (ALD) and then examined as “intelligent” catalyst supports for Ni in the steam and CO 2 reforming of methane. CaTiO 3 films (1 nm) were characterized by scanning transmission electron microscopy and XRD and shown to be stable to at least 1073 K. Catalysts with 1 and 20 wt % Ni were studied, and it was found that, following calcination at 1073 K, the Ni-CaTiO 3 /MgAl 2 O 4 catalysts required high-temperature reduction to achieve activities comparable to that of their Ni/MgAl 2 O 4 counterparts. However, the Ni-CaTiO 3 /MgAl 2 O 4 catalysts exhibited dramatically improved tolerance toward carbon-whisker formation. The carbon content on the 1 wt % Ni catalyst on CaTiO 3 /MgAl 2 O 4 was small even after heating the catalyst in a dry, 10% CH 4 –90% He mixture at 1073 K for 12 h. As a result, possible mechanisms for the high carbon tolerance of the perovskite-containing catalysts are discussed.

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

Nanoscopic Plugs Block Hydrogen Crossover in Submicron Thick Proton-Conducting SiO 2 Membranes for Water Electrolysis

Zero-gap electrolyzers based on submicron thick proton-conducting oxide membranes (POMs) represent a promising approach to increasing the efficiency of H 2 production from water electrolysis while moving away from conventional perfluorosulfonic acid (PFSA) membranes. A critical barrier to the commercialization of such electrolyzers is that the ultrathin nature of POMs, which is necessary to achieve low cell resistance, makes them more susceptible to defects that can lead to unacceptably high rates of H 2 crossover. Herein, we demonstrate an approach to mitigate this problem through selective deposition of carbon-containing silicon oxide (SiO x C y ) “nanoplugs” into the defects of submicron thick SiO 2 membranes using a facile electrochemically mediated deposition process. Selective deposition of nanoplugs within the defects was verified by multiple characterization techniques, while scanning electrochemical microscopy (SECM) was used to confirm selective plugging of H 2 -crossover hotspots associated with defects at identical locations. Thanks to the use of nanoplugs, the H 2 permeance of 250 nm thick SiO 2 membranes was reduced by 5 to 6 orders of magnitude compared to the unmodified atomic layer deposition (ALD) SiO 2 membranes while having negligible impact on the ionic resistance of the membrane. These plug-modified membranes also enabled safe and stable operation of a zero-gap full cell electrolysis cell, in contrast to cells lacking nanoplugs that produced anode effluent streams having H 2 concentrations near or exceeding the lower flammability limit (LFL) of H 2 . Furthermore, beyond water electrolysis, this defect-sealing strategy has the potential to be broadly implemented in other applications, such as fuel cells and flow batteries, offering a versatile solution to mitigate crossover-related performance losses.

ALD SiO2↗
DOE OSTI2020

Epitaxial and Strong Support Interactions between Pt and LaFeO 3 Films Stabilize Pt Dispersion

The ability to stabilize very small Pt crystallites in supported-metal catalysts following harsh treatments is an important industrial problem. Herein, we demonstrate that Pt particles can be maintained in the 1- to 2-nm range following multiple oxidation and reduction cycles at 1073 K when the particles are supported on 0.5-nm LaFeO 3 films that have been deposited onto MgAl 2 O 4 using atomic layer deposition (ALD). Characterization by Scanning Transmission Electron Microscopy (STEM) suggest that, when the catalyst is oxidized at 1073 K, the Pt crystallites are oriented with respect to the underlying LaFeO 3 . X-Ray Absorption Spectroscopy (XAS) also shows evidence for changes in the Pt environment. CO-oxidation rates for the reduced catalyst remain unchanged after five redox cycles at 1073 K. Epitaxial growth of Pt clusters and the consequent strong metal-support interaction between Pt and LaFeO 3 are indicated to be prime reasons for the enhanced catalytic performances.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Nanoporous aluminum oxide membranes coated with atomic layer deposition-grown titanium dioxide for biomedical applications: An in vitro evaluation

The surface topographies of nanoporous anodic aluminum oxide (AAO) and titanium dioxide (TiO 2 ) membranes have been shown to modulate cell response in orthopedic and skin wound repair applications. In this study, we: (1) demonstrate an improved atomic layer deposition (ALD) method for coating the porous structures of 20, 100, and 200 nm pore diameter AAO with nanometer-thick layers of TiO 2 and (2) evaluate the effects of uncoated AAO and TiO 2 -coated AAO on cellular responses. The TiO 2 coatings were deposited on the AAO membranes without compromising the openings of the nanoscale pores. The 20 nm TiO 2 -coated membranes showed the highest amount of initial protein adsorption via the micro bicinchoninic acid (micro-BOA) assay; all of the TiO 2 -coated membranes showed slightly higher protein adsorption than the uncoated control materials. Cell viability, proliferation, and inflammatory responses on the TiO 2 -coated AAO membranes showed no adverse outcomes. For all of the tested surfaces, normal increases in proliferation (DNA content) of L929 fibroblasts were observed over from 4 hours to 72 hours. No increases in TNF-alpha production were seen in RAW 264.7 macrophages grown on TiO 2 -coated AAO membranes compared to uncoated AAO membranes and tissue culture polystyrene (TOPS) surfaces. Both uncoated AAO membranes and TiO 2 -coated AAO membranes showed no significant effects on cell growth and inflammatory responses. In conclusion, the results suggest that TiO 2 -coated AAO may serve as a reasonable prototype material for the development of nanostructured wound repair devices and orthopedic implants.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Transfer of Graphene with Protective Oxide Layers

Transfer of graphene, grown by chemical vapor deposition (CVD), to a substrate of choice, typically involves the deposition of a polymeric layer (for example, poly(methyl methacrylate) (PMMA), or polydimethylsiloxane, PDMS). These polymers are quite hard to remove without leaving some residues behind. One method to improve the graphene transfer is to coat the graphene with a thin protective oxide layer, followed by the deposition of a very thin polymer layer on top of the oxide layer (much thinner than the usual thickness), followed by a more aggressive polymeric removal method, thus leaving the graphene intact. At the same time, having an oxide layer on graphene may serve applications, such as channeled transistors or sensing devices. Here, we study the transfer of graphene with a protective thin oxide layer grown by atomic layer deposition (ALD). We follow the transfer process from the graphene growth stage through oxide deposition until completion. We report on the nucleation growth process of oxides on graphene, their resultant strain and their optical transmission.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Preparation of SBA-15-Supported Metals by Vapor-Phase Infiltration

A simple method is presented for incorporating various catalytic metals into the pores of SBA-15 using vapor-phase infiltration. The precursors used in Atomic Layer Deposition (ALD) for Pt, Pd, Rh, Ru, and Ni were exposed to an evacuated SBA-15, resulting in monolayer films of the adsorbed precursors inside the mesopores. The metal particles that formed after removal of the precursor ligands remained in the pores and had particle sizes ranging from 3.8 nm for Pt to 5.2 nm for Ni, as determined by Transmission Electron Microscopy (TEM), XRD, and CO chemisorption. Metal loadings for saturation exposures ranged from 5.1-wt% for Ni to 9.1-wt% for Pt; however, uniform deposition was demonstrated for lower loadings of Pd by decreasing the amount of precursor. To determine the effect of the surface composition of the mesopores, Pd particles were also added to SBA-15 that was coated with a 0.2-nm film of ZrO2.

Rh↗
DOE OSTI2019

“Intelligent” Pt Catalysts Based on Thin LaCoO3 Films Prepared by Atomic Layer Deposition

LaCoO3 films were deposited onto MgAl2O4 powders by atomic layer deposition (ALD) and then used as catalyst supports for Pt. X-ray diffraction (XRD) showed that the 0.5 nm films exhibited a perovskite structure after redox cycling at 1073 K, and scanning transmission electron microscopy and elemental mapping via energy-dispersive X-ray spectroscopy (STEM/EDS) data demonstrated that the films covered the substrate uniformly. Catalysts prepared with 3 wt % Pt showed that the Pt remained well dispersed on the perovskite film, even after repeated oxidations and reductions at 1073 K. Despite the high Pt dispersion, CO adsorption at room temperature was negligible. Compared with conventional Pt on MgAl2O4, the reduced forms of the LaCoO3-containing catalyst were highly active for the CO oxidation and water gas shift (WGS) reactions, while the oxidized catalysts showed much lower activities. Surprisingly, the reduced catalysts were much less active than the oxidized catalysts for toluene hydrogen. Catalysts prepared from thin films of Co3O4 or La2O3 exhibited properties more similar to Pt/MgAl2O4. Possible reasons for how LaCoO3 affects properties are discussed.

42 ENGINEERING↗
NASA NTRS2017

An Introduction to Atomic Layer Deposition

Atomic Layer Deposition has been instrumental in providing a deposition method for multiple space flight applications. It is well known that ALD is a cost effective nanoadditive-manufacturing technique that allows for the conformal coating of substrates with atomic control in a benign temperature and pressure environment. Through the introduction of paired precursor gases, thin films can be deposited on a myriad of substrates from flat surfaces to those with significant topography. By providing atomic layer control, where single layers of atoms can be deposited, the fabrication of metal transparent films, precise nano-laminates, and coatings of nano-channels, pores and particles is achievable. The feasibility of this technology for NASA line of business applications range from thermal systems, optics, sensors, to environmental protection. An overview of this technology will be presented.

ALD↗
DOE OSTI2016

Innovation Meets Performance Demands of Advanced Lithium-ion Batteries

Advancements in high capacity and low density battery technologies have led to a growing need for battery materials with greater charge capacity and therefore stability. NREL's developments in ALD and molecular layer MLD allow for thin film coatings to battery composite electrodes, which can improve battery lifespan, high charge capacity, and stability. Silicon, one of the best high-energy anode materials for Li-ion batteries, can experience capacity fade from volumetric expansion. Using MLD to examine how surface modification could stabilize silicon anode material in Li-ion batteries, researchers discovered a new reaction precursor that leads to a flexible surface coating that accommodates volumetric expansion of silicon electrodes.

25 ENERGY STORAGE↗
DOE OSTI2020

Visible-Light-Activated Photocatalytic Films toward Self-Cleaning Membranes

Membranes are among the most promising means of delivering increased supplies of fit-for-purpose water, but membrane fouling remains a critical issue restricting their widespread application. Coupling photocatalysis with membrane separation has been proposed as a potentially effective approach to reduce membrane fouling. However, commonly used materials in photocatalysis limit use of low-cost sources such as sunlight due to their large band gaps. There are few examples of in situ photocatalytic self-cleaning of membranes, with removal from the filtration system and ex situ illumination being more common. In this study, a visible-light-activated photocatalytic film prepared by nitrogen doping into the lattice of TiO 2 was deposited on commercial ceramic membranes via atomic layer deposition (ALD). The synergy between membrane separation and redox reactions between organic pollutants and reactive oxygen species (ROS) produced by the visible-light-activated layer offers a possibility for stable and sustainable membrane operation under in situ solar irradiation.

36 MATERIALS SCIENCE↗