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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Towards directed energy deposition of metals using polymer-based supports: porosity of 316L stainless steel deposited on carbon-fiber-reinforced ABS

Directed energy deposition (DED) is increasingly valuable to many industries because of its high deposition rates relative to other metal additive manufacturing processes, but the design space of DED is limited. For instance, steep overhangs are difficult or impossible to manufacture. Polymer-based support structures could help address this challenge. The viability of DED on polymer composite substrates has begun to be explored, specifically with 316L stainless steel on carbon-fiber-reinforced ABS substrates. Monolithic metal components can be deposited on the polymer, but it was found that gas release during polymer degradation causes porosity due to gas entrapment in the metal. An interlayer cooling time was introduced to reduce polymer degradation and decrease the porosity due to gas entrapment, but this led to porosity from lack of fusion. The results of this work provide insight into process parameter selection and scan strategy development to enable the use of polymer support structures in blown-powder DED.

Kurfess, Rebecca↗
DOE OSTI2026

Co-sputter deposition of Nb₃Sn layer into SRF cavity using Nb-Sn composite target

Nb₃Sn, with its superior superconducting critical temperature (Tc ~18.3 K) and superheating field (Hsh ~400 mT), is considered a promising material for superconducting radiofrequency (SRF) cavities, offering enhanced cryogenic performance compared to bulk niobium cavities. A Nb₃Sn coating technique has been developed for Nb SRF cavities using co-sputtering of Nb-Sn composite target in a DC cylindrical magnetron sputtering system. The composite target configuration and discharge conditions for co-sputtering were optimized to deposit Nb-Sn films on flat Nb substrates, followed by annealing to form Nb₃Sn. Multiple strategies have been explored to improve the surface homogeneity of the Nb₃Sn coating, including optimizing a two-step annealing process, annealing in Sn vapor, and a light Sn recoating process. A 1.5 µm Nb-Sn co-sputtered film was deposited on the interior of a 2.6 GHz Nb SRF cavity and annealed at 600 °C for 6 h, followed by 950 °C for 1 h. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, confirming the formation of Nb₃Sn. Then, the annealed cavity underwent a light recoating treatment and attained a quality factor (Q0) of 8.5E+08 at 2.0 K.

Accelerator Physics↗
DOE OSTI2020

Continuous polymer films deposited on top of porous substrates using plasma-enhanced atomic layer deposition and molecular layer deposition

Molecular layer deposition (MLD) is able to produce ultrathin polymer films with control over thickness, cross-linking, and chemical composition. With these capabilities, MLD should be useful in the fabrication of novel polymer membranes on porous supports. However, confining a continuous MLD film to the surface of porous substrates is difficult because of MLD film growth in the pores. The deposition in the pores lowers the conductance of the porous support. This paper presents a method to deposit continuous polymer films on top of porous substrates. In this method, Al2O3 plasma-enhanced atomic layer deposition (PE-ALD) using trimethylaluminum and oxygen plasma as the reactants was first used to cap the pores of the substrate. Subsequently, a polyamide MLD film was deposited on the Al2O3 PE-ALD capping layer using m-phenylenediamine and trimesoyl chloride as the reactants. The Al2O3 pore caps were then removed from the porous substrate by etching from the backside using a timed exposure to a dilute sodium hydroxide solution. This method was demonstrated using anodic aluminum oxide (AAO) and polyethersulfone (PES) porous substrates. Al2O3 PE-ALD film growth was limited to the top of the porous substrate, resulting in rapid surface recombination or high sticking coefficients for the reactive plasma species within the pores. Gas permeance measurements confirmed the pore capping of the AAO substrates. The reopening of the pores by dissolving the Al2O3 pore caps with a sodium hydroxide solution was monitored using gas permeance versus etch time. The removal of the Al2O3 pore caps from the PES substrates could also dissolve the Al2O3 layer underneath the MLD film. The loss of this Al2O3 layer led to the detachment of the MLD film from the PES substrate. However, the MLD film could be anchored to the PES support at fractures located in the Al2O3 film prior to the MLD. The Al2O3 film fracture allowed the MLD film to anchor firmly to the PES substrate by MLD in the pores of the PES porous substrate. The distance between the anchor points was a function of fracture density. This distance could be controlled by applying a tensile stress to the Al2O3 PE-ALD film to fracture the film through sample bending. This method produced firmly anchored polymer MLD films on top of the PES porous substrates.

Welch, Brian C. (ORCID:000000029747045X)↗
DOE OSTI2023

Effect of Blown Powder Directed Energy Deposition Angle On Overspray Contamination

Abstract Blown powder directed energy deposition (DED) hybrid machine tools are particularly beneficial when the net shape of a component is to be manufactured in an additive and machined interleaved fashion. This investigation seeks to analyze the effect of the additive head lean angle relative to the part on blown powder DED surface contamination due to overspray. These hybrid DED platforms are commonly installed on multi-axis machining systems where the lean of the deposition head relative to the component surface can be controlled by tilting the component. The blown powder DED process has a 10–50% lower catchment efficiency as compared to wire fed DED systems. This excess powder is still fed towards the deposition location where the particles are heated by the laser and rebound off the melt pool. Some of these heated particles impact the previously machined thin-wall surface. While the deposition process and tool path planning process has been evaluated, the effect of the overspray due to lean angle of the deposition head on the previously thin-wall machined surface is not yet fully understood. This investigation found that minimum lean angle coincides with minimal overspray effect with nearly no contamination. If a lean angle is required, the maximum lean angle possible should be implemented for the smallest effected overspray area on the machined surface which was found to decrease the affect zone by half compared to intermediate lean angles. A diameter divergence was also noticed as the deposition angle was increased. In this study, a thorough analysis of the surface and geometric effects when depositing thin-walled components at varying angles is completed. It has been shown that part quality can be significantly affected by lean angle and thus must be incorporated as an additional design consideration in the manufacturing process.

Heinrich, Lauren↗
DOE OSTI2022

Investigating Deposition Sequence During Synthesis of Pd/Al2O3 Catalysts Modified with Organic Monolayers

Modification of supported metal catalysts with self-assembled monolayers (SAMs) has been shown to improve selectivity and turnover frequencies (TOFs) for many catalytic reactions. However, these benefits are often accompanied by a decrease in overall mass activity due to partial blocking of active sites by the monolayers. Therefore, a potential method for increasing site accessibility is to deposit the active metal (e.g., Pd) after deposition of a SAM modifier on the support material. In this work, Pd/Al2O3 catalysts were synthesized using both a conventional, "metal-first" sequence in which the phosphonic acid (PA) SAM was deposited on Pd/Al2O3 and a "SAM-first" technique in which the ligands were deposited onto the support prior to deposition of the metal. Although metal-first catalysts showed a significant increase in TOF during benzyl alcohol HDO, they exhibited only a modest increase in overall mass activity due to a decrease in the number of active sites. Meanwhile, SAM-first catalysts showed similar improvements in TOF and toluene selectivity but exhibited significantly improved HDO rates compared to metal-first catalysts. The rate increase was attributed to reduced site blocking as evidenced by CO chemisorption measurements. Additionally, analysis of catalysts having high Pd loadings using transmission electron microscopy (TEM) showed that SAM-first catalysts generally resulted in lower average particle sizes than traditionally modified and unmodified catalysts, suggesting that precoating the support surface with PAs changes the way that Pd is deposited during incipient wetness, leading here to improved activity.

catalytic reactions↗
DOE OSTI2019

Characterizations of Binary FeCr (AISI 430) Thin Films Deposited from a Single Magnetron Sputtering Under Easy Controllable Deposition Parameters

A series of 50-nm binary FeCr martensitic thin films were sputtered from a single source made of commercial AISI 430 ferritic stainless steel under the deposition rates gradually increased from 0.03 to 0.11 nm/s with 0.02 nm/s steps at stationary condition. And, under 0.09 nm/s deposition rate, a second series of the films were also deposited under the rotation speed of their substrates which was chosen at 0, 25, and 45 rpm. As far as we are concerned, this study is the first investigation of properties of the thin films produced from AISI 430. The atomic Fe content in the films increased from 79.3 to 98.6% while atomic Cr content decreased from 20.5 to 1.2% with the increase of deposition rate from 0.03 to 0.11 nm/s. According to compositional analysis, the Fe content increased while Cr content decreased with increasing deposition rate. The reason for this may be attributed to the relatively different bond energy/melting point of metals which have different contents sputtered from source material since this physical parameter is very significant for the sputtering process. And, the Fe content in the films decreased from 84.9 to 79.2 at. % while the Cr content increased from 14.9 to 20.6 at. % when the increase of rotation speed of substrate. The crystal structure of all films was observed to have a body-centered tetragonal phase and the intensity of (110) peak varied with the atomic Fe content. The surface observations of films performed by a scanning electron microscope exposed that the number of surface grains increased with the increase of deposition rate and decreased with the increase of rotation speed. According to surface roughness analysis done by an atomic force microscope, the roughness of the film surfaces increased as the deposition rate increased. And, the roughness of the film surfaces decreased as the rotation speed increased. This has been consistent with the grain size and roughness parameters. Thus, increasing deposition rate and decreasing rotation speed of the substrate caused an increase in grain size and roughness parameters. The magnetic measurements of the films achieved, by a vibrating sample magnetometer at room temperature, displayed that the saturation magnetization, M{sub s}, values increased from 820.1 to 1700.4 emu/cm{sup 3}, the remanence magnetization, M{sub r}, values increased from 293 to 817 emu/cm{sup 3}, and the coercivity, H{sub c}, value also increased from 38 to 107 Oe with the increasing of deposition rate. It is also seen that the magnetic easy axis are in the film plane due to the shape anisotropy. With the increase rotation speed, the values of M{sub s} and M{sub r} increased and the H{sub c} decreased. It was seen that variation of Fe content in the films influences the M{sub s} values and the H{sub c} values are consistent with the surface properties. It was concluded that the deposition rate and the rotation speed of the substrate play a considerable role on the structural and related magnetic properties of the sputtered FeCr thin films, and the properties of the films can be easily controlled by changing production parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Dry Deposition of Atmospheric Aerosols: Approaches, Observations, and Mechanisms

Aerosols are liquid or solid particles suspended in the atmosphere, typically with diameters on the order of nanometers to microns. These particles impact air quality and the radiative balance of the planet. Dry deposition is a key process for the removal of aerosols from the atmosphere and plays an important role in controlling the lifetime of atmospheric aerosols. Dry deposition is driven by turbulence and shows a strong dependence on particle size. This review summarizes the mechanisms behind aerosol dry deposition, including measurement approaches, field observations, and modeling studies. We identify several gaps in the literature, including deposition over the cryosphere (i.e., snow and ice surfaces) and the ocean; in addition, we highlight new techniques to measure black carbon fluxes. While recent advances in aerosol instrumentation have enhanced our understanding of aerosol sources and chemistry, dry deposition and other loss processes remain poorly investigated.

Chemistry↗
DOE OSTI2019

Accelerated Springtime Melt of Snow on Tundra Downwind from Northern Alaska River Systems Resulting from Niveo-aeolian Deposition Events

It is well known that light-absorbing particulate matter (PM) enhances absorption of sunlight when deposited on ice and snow. Such increased absorption is due to a reduction in surface albedo, resulting in accelerated melt of frozen surfaces. In isolation, earlier melt enhances Arctic warming since dark surfaces underlying snow and ice are exposed and absorb additional solar energy. Here, we combine various observational tools to demonstrate that aeolian deposition of PM along fluvial features on the North Slope of Alaska resulted in a notable reduction of surface albedo in the spring of 2016, from values typical for snow (~0.8) to around 0.35 on average. This reduction resulted in accelerated snow and ice melt by up to three weeks compared to unaffected areas. This phenomenon was observed to some degree in 12 other years dating back to 2003. Deposition generally was found to occur near particular sections of the rivers, with several areas affected by events in multiple years. In all years, the deposition is attributed to high wind events. The extreme case in 2016 is linked to unusually strong and extraordinarily persistent winds during April. The deposited material is thought to be the natural sediment carried by the rivers, resulting in a seasonally replenished source of PM. These findings indicate a previously unreported impact of both fluvial and atmospheric processes on the seasonal melt of northern Alaska rivers.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Modeling of deposit formation in mesoporous substrates via atomic layer deposition: Insights from pore‐scale simulation

Atomic layer deposition (ALD) has been a promising technique in fabricating membranes and tuning their properties with a precision at the atomic level. Fabrication of zeolitic imidazolate framework (ZIF) membranes using the ligand-induced permselectivation (LIPS) method starts with the formation of an oxide in a mesoporous substrate by ALD and is followed by the transformation of this oxide to ZIF using imidazolate vapor treatment. The objective of the ALD step is to block the mesopores with a thin deposit, that is, one with small penetration depth and small thickness on the top surface of the substrate. Unlike typical ALD on nonporous substrates, where all available sites react per ALD cycle, thin deposit formation in a mesoporous substrate requires that only a small fraction of the available deposition sites (i.e., close to the substrate surface) is subjected to ALD. Consequently, reactant dosing and duration of pulses are important process variables which, together with diffusion and reaction kinetics determine the deposit structure. Quantitative understanding of the interplay of these variables and phenomena can enable the rational design of ALD within mesoporous substrates. Here, we extend our earlier modeling effort considering the coexistence of ALD both inside the pores and on the external surface of the substrate. Finite-volume based models were developed and validated to simulate the two distinct modes of deposition cycle by cycle. The total mass uptake of the substrate with ALD cycles can be predicted using the combined surface deposition and pore reaction–diffusion models as affirmed by in situ quartz crystal microbalance experimental data. The ALD reactor model combined with the deposition model can accurately capture the number of ALD cycles needed to block the pores of the substrate. Based on the model, we designed a modified ALD process and examined the performance of the corresponding LIPS membranes. Furthermore, the present modeling work provides a new understanding of the deposit formation via ALD within mesoporous substrates for a variety of membrane applications.

atomic layer deposition↗
DOE OSTI2019

Easy Controlled Properties of Quaternary FeNiCrCd Thin Films Deposited from a Single dc Magnetron Sputtering Under the Influence of Deposition Rate

The quaternary FeNiCrCd thin films were produced from a single FeNiCrCr source on a commercial flexible polymer substrate using one dc magnetron sputtering technique. For that, a series of the films with a thickness of 50 nm were produced at different deposition rates of 0.02, 0.04, 0.06, and 0.08 nm/s, separately. In this study, as far as concerned, this was the first time that structural and magnetic properties of FeNiCrCd thin films were investigated. According to compositional analysis, the Fe and Cr contents slightly decreased with increasing deposition rate while Ni was almost constant, whereas those of the amount of Cd atoms increased. However, the atomic amounts of Fe and Cd in the films are quite different from those of the source material. The change of the atomic contents in the films from the source may be attributed to the relatively different bond energy/melting point of metals which have different contents sputtered from source material since this physical parameter is very significant for the sputtering process. For crystal structural analysis, a combination of hexagonal close-packed (hcp) and body-centered cubic (bcc) were observed. The peak intensity of the bcc-dominated planes decreased while the hcp-dominant plane increased since the change in peak intensities is compatible with the compositional analysis with increasing deposition rate. And, the grain sizes decreased gradually from 40.1 to 23.4 nm, with increasing deposition rate from 0.02, to 0.08 nm/s. Also, the film surfaces transformed from a rough to smooth surfaces with decreasing grain sizes as deposition rate increased. For magnetic analysis, the saturation magnetization M{sub s} values decreased as 1030, 773, 730, and 217 emu/cm{sup 3} with increasing deposition rate as 0.02, 0.04, 0.06, and 0.08 nm/s, respectively. In the same manner, the coercivity H{sub c} values were found as 11, 7, 6, and 2 Oe with the deposition rate of 0.02, 0.04, 0.06, and 0.08 nm/s, respectively. The decrease of the H{sub c} may have primarily come from the transformation of rough to smooth surface of the films. It may also be said that the films showed soft magnetic properties due to their low H{sub c} values with increasing deposition rate. Thus, the magnetic properties of the quaternary FeNiCrCd alloy films were seen to be easily improved with the deposition rate parameter for potential use in different industrial applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Residual stresses in Cu matrix composite surface deposits after laser melt injection

Abstract Tungsten carbide particles reinforced metal matrix composite (MMC) coatings can significantly improve surface wear resistance owing to their increased surface hardness. However, the presence of macro‐ and micro‐residual stresses in MMC coatings can have detrimental effects, such as reducing service life. In this study, neutron diffraction was used to determine the residual stresses in spherical fused tungsten carbide (sFTC) reinforced Cu matrix composite surface deposits after laser melt injection. We also developed a thermo‐mechanical coupled finite element model to predict residual stresses. Our findings reveal that sFTC/Cu composite deposits produced with a preheating temperature of 400°C have low residual stresses, with a maximum tensile residual stress of 98 MPa in the Cu matrix on the top surface. In contrast, the sFTC/bronze (CuAl10Ni5Fe4) composite deposit exhibits very high residual stresses, with a maximum tensile residual stress in the Cu matrix on the top surface reaching 651 MPa. These results provide a better understanding of the magnitudes and distributions of residual stresses in sFTC‐reinforced Cu matrix composite surface deposits manufactured via laser melt injection.

Zhang, Xingxing↗
DOE OSTI2026

Deposition Height Prediction in Directed Energy Deposition

Using 316L stainless steel as a model material, reduced-order models are developed to predict capture efficiency, deposition height, and site-specific hardness in directed energy deposition. Capture efficiency is predicted over a 15 to 55 pct range using a dimensionless number derived from processing conditions and thermophysical properties. Deposition height is predicted over a 0.3 to 1.3 mm range without in situ sensing or prior training data, using two models based on the same mass and energy-balance principles. Predictions are compared with machine learning approaches. A quantitative relationship links deposition height, primary dendrite arm spacing (PDAS), and hardness: heights of 0.3 to 1.1 mm correspond to PDAS values of 2.7 to 5.1 µm and Vickers hardness (HV) of 160 to 219. Thinner layers cool more rapidly, producing finer microstructures and higher hardness. Samples fabricated with in situ variations in deposition height exhibited up to 55 HV differences between thick and thin regions, demonstrating that local control of deposition height enables predictive, site-specific hardness within a single build. These results establish deposition height prediction as a pathway for a priori process design and property control in directed energy deposition for 316L stainless steel.

Kunkel, William [Univ. of Wisconsin, Madison, WI (↗
DOE OSTI2020

Wet and dry plastic deposition data for western US National Atmospheric Deposition Program sites (2017-2019)

Raw plastic counts and calculated plastic deposition rates for 11 National Atmospheric Deposition Program (NADP) sites in the western USA recorded from 2017-2019. Samples were collected to determine plastic deposition rates in remote locations and identify the potential sources of plastic to the atmosphere. Samples were collected using an Aerochem Metrics Wet and Dry sampler. Wet deposition refers to the material retained on a 0.45-micron filter. Dry deposition refers to the dry only deposition collected using a Dry Side Insert (DSI) (Brahney et al. 2020). Plastics are identified as either fibers or particles (includes small colored films). Wet deposition rates are recorded weekly and dry plastic deposition rates are based on monthly sampling intervals. Sites included are Grand Canyon National Park (AZ03), Joshua Tree National Park (CA67), Rocky Mountain National Park (CO98), Niwot Ridge (CO02), Ashley National Forest (UT95), East River SFA (CO10)), Craters of the Moon National Park (ID03), Great Basin National Park (NV05), Canyonlands National Park (UT09), Bryce Canyon Nationa Park (UT99), and Wind River Range (WY06). Data collection is being published in collaboration with the Department of Energy's research project, "Constraining physical understanding of aerosol loading, biogeochemistry, and snowmelt hydrology from hillslope to watershed scale in the East River Scientific Focus Areas.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2019

Vapor-Deposited Glass Structure Determined by Deposition Rate–Substrate Temperature Superposition Principle

In this article, we show that deposition rate substantially affects the anisotropic structure of thin glassy films produced by physical vapor deposition. Itraconazole, a glass-forming liquid crystal, was deposited at rates spanning 3 orders of magnitude over a 25 K range of substrate temperatures, and structure was characterized by ellipsometry and X-ray scattering. Both the molecular orientation and the spacing of the smectic layers obey deposition rate–substrate temperature superposition, such that lowering the deposition rate is equivalent to raising the substrate temperature. We identify two different surface relaxations that are responsible for structural order in the vapor-deposited glasses and find that the process controlling molecular orientation is accelerated by more than 3 orders of magnitude at the surface relative to the bulk. Finally, the identification of distinct surface processes responsible for anisotropic structural features in vapor-deposited glasses will enable more precise control over the structure of glassy materials used in organic electronics.

36 MATERIALS SCIENCE↗
DOE OSTI2020

High‐Performance Zinc Tin Oxide TFTs with Active Layers Deposited by Atomic Layer Deposition

Abstract New deposition techniques for amorphous oxide semiconductors compatible with silicon back end of line manufacturing are needed for 3D monolithic integration of thin‐film electronics. Here, three atomic layer deposition (ALD) processes are compared for the fabrication of amorphous zinc tin oxide (ZTO) channels in bottom‐gate, top‐contact n‐channel transistors. As‐deposited ZTO films, made by ALD at 150–200 °C, exhibit semiconducting, enhancement‐mode behavior with electron mobility as high as 13 cm 2 V −1 s −1 , due to a low density of oxygen‐related defects. ZTO deposited at 200 °C using a hybrid thermal‐plasma ALD process with an optimal tin composition of 21%, post‐annealed at 400 °C, shows excellent performance with a record high mobility of 22.1 cm 2 V –1 s –1 and a subthreshold slope of 0.29 V dec –1 . Increasing the deposition temperature and performing post‐deposition anneals at 300–500 °C lead to an increased density of the X‐ray amorphous ZTO film, improving its electrical properties. By optimizing the ZTO active layer thickness and using a high‐ k gate insulator (ALD Al 2 O 3 ), the transistor switching voltage is lowered, enabling electrical compatibility with silicon integrated circuits. This work opens the possibility of monolithic integration of ALD ZTO‐based thin‐film electronics with silicon integrated circuits or onto large‐area flexible substrates.

Allemang, Christopher R.↗
DOE OSTI2025

Highly Active Hydrogen Evolution Reaction (HER) Catalysts Formed by Energetic Pt n Cluster Deposition: Deposition Dynamics and the HER Mechanism

Mass-selected Pt n + (n ≤ 7) were deposited at variable energies on highly oriented pyrolytic graphite (HOPG), creating highly active hydrogen evolution reaction (HER) electrocatalysts. HER mass activities were ~2 to >10 times higher than those for the surface atoms in bulk Pt and for Pt n deposited on several other supports. Thus, high activity reflects the Pt-C structures formed by energetic Pt n -HOPG impacts, in addition to high Pt surface availability. The Pt n /HOPG electrodes were probed by X-ray photoelectron spectroscopy, low energy ion scattering, and electron microscopy. Born-Oppenheimer molecular dynamics (BOMD) was used to simulate Pt n - HOPG impacts, revealing the types of structures formed at different energies, then DFT was used to probe their most important HER pathways. For low deposition energies, the Pt n deposit onto the HOPG surface with sub-unit sticking probability, aggregating at defects. With increasing deposition energy, the sticking probability initially decreases, then rises to unity as subplantation and defect creation allow formation of strongly bonded platinum-carbon structures. Barriers for HER on these structures were found to be low and weakly dependent on Pt n size, consistent with experiment. The activities were highest for small covalently-bonded Pt-C structures created at high deposition energies. The larger aggregated structures formed at low energies were less active, but still substantially better than the bulk Pt surface monolayer. The catalysts were stable in repeated potential cycling at reducing potentials, but electrodes containing subplanted Pt became more active when scanned to oxidizing potentials, due to emergence of subplanted Pt onto the surface.

08 HYDROGEN↗