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DOE OSTI2021

Thermal Processing Conditions for the Synthesis of Near Theoretical Density Li 5 La 3 Ta 2 O 12 Ceramics for Ceramic Dual-Mode Detectors

A family of Li-containing garnet compounds, extensively investigated for Li-ion solid electrolyte applications, show great potential to be developed into transparent ceramic dual-mode scintillators. In particular, Li 5 La 3 Ta 2 O 12 (LLTaO) shows promise as an efficient dual-mode scintillator due to its high Li content, high density, non-hygroscopicity, and high effective-Z. Often the synthesis of LLTaO ceramics involves solid state processing techniques starting with oxide and carbonate powders, calcining, sintering for the removal of residual porosity, and post-processing. This study focuses on two objectives: (1) establishing thermal processing boundary conditions for a flexible alkoxide-based sol-gel method for synthesizing fine-grained powders; and (2), consolidating powders via hot-pressing to form high-density ceramics. In this study, near single-phase ceramics were achieved by hot-pressing sol-gel powders with varying amounts of excess Li. Rietveld refinements were used to analyze X-ray diffraction data and provide a quantitative evaluation of the phases present in the hot pressed ceramics. Some of the diffraction data showed large low angle peak asymmetry, suggesting the presence of two cubic Li 5 La 3 Ta 2 O 12 garnet phases with different lattice parameters. Depending on the synthesis and processing conditions, the refinement revealed ~ 90 wt% concentration of a phase with a ≈ 12.8 Å and ~ 10 wt% concentration of a phase with a ≈ 12.9 Å, indicating a remaining excess of Li in the hot pressed ceramics in the large lattice parameter phase. These synthesis experiments allowed for the determination of a baseline for Li loss during hot-pressing. X-ray excited radioluminescence and photoluminescence excitation and emission spectra were obtained from the hot pressed ceramics. In conclusion, the measured emission spectra featured broad tantalate emission and line emissions likely from a rare-earth impurity.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Self-terminating etching processes for post-processing of 3D printed metal alloys

A process is provided to remove a selective amount of material from a metal part fabricated by additive manufacturing in a self-terminating manner. The process can be used to remove support structures and trapped powder from a metal part as well as to smooth surfaces of a 3D printed metal part. In one embodiment, selected surfaces of the metal part are treated to make the selected surfaces at least one of mechanically and chemically unstable. The unstable portion of the metal support can then be removed chemically, electrochemically, with a pressure differential, and/or through vapor-phase etching. In one embodiment, the metal part may comprise one or more of an aluminum alloy, a titanium alloy, and a copper alloy. The process can be used to modify any fluid or vapor-accessible regions and surfaces of a 3D printed metal part.

Hildreth, Owen J.↗

DOE OSTI2024

A Simulated Evaluation of Powder Flowability Through a Partially Obstructed Consumable in Blown Powder Directed Energy Deposition Systems

Abstract In the interest of continued industrialization of metal additive manufacturing in modern production environments, cost is often referenced as a primary deterrent to new adopters. Conventional economic models for additive systems, processes, and supply chains often focus on specific process applications with little generalizability, or they neglect significant costs associated with production such as machine maintenance and consumable part replacement. Compounding the latter issue are substantial knowledge gaps in consumable part wear characterization for additive and other convergent manufacturing systems. In coaxial blown powder directed energy deposition systems, gas atomized metal powder is wasted during material deposition at a rate that is partly dependent on present wear phenomena in a consumable nozzle housed in the cladding head assembly. The price and lead time required to replace the nozzle incentivizes its reuse even when visibly worn. Often this initiates a process quality decline in the form of underbuilt geometry and internal defects due to losses in powder catchment efficiency. While depositing H13 steel using a hybrid manufacturing machine tool equipped with such a deposition system, a unique partial clog with a bridge-like structure formed at the consumable nozzle exit when supporting argon gas flows failed mid-process. To further understand coaxial multi-phase powder flow in the event of support gas failure, a computational fluid dynamics simulation is tailored to relevant process parameters, H13 powder material profile, and machine operator observations collected after the incident. The resulting differences in powder flow compared to control gas flow parameters is presented and discussed. The powder flowability and performance of the clogged nozzle is then assessed by using an optical profilometer to extract the profile of the clog and recreate the clog geometry within the simulation environment. In past work this simulation has been experimentally validated for a 316L steel powder material profile and used specifically for analyzing powder stream geometry and catchment efficiency. After the initial powder flow characterization, the clog is removed, and the nozzle is reprofiled. After removing the obstructing clog, the newly unobstructed nozzle geometry, the original off the shelf nozzle geometry, and additional nozzle profiles exploring different consumable refurbishment strategies are reevaluated in the simulation. Powder catchment efficiency for all variant nozzle geometries and relevant flow variables are compared and discussed, along with potential mitigation strategies for optimizing powder flowability with worn consumables. This work expands on the known morphology of blown powder obstructions and wear defects present in consumable coaxial nozzles while discussing pragmatic simulation driven responses to unanticipated subsystem failure in hybrid manufacturing machining platforms.

DeWitte, Lisa↗

NASA NTRS2017

Cleaning and Cleanliness Measurement of Additive Manufactured Parts

Additive Manufacturing processes allow for the manufacture of complex three dimensional components that otherwise could not be manufactured. Post treatment processes require the removal of any remnant bulk powder that may become entrapped within small cavities and channels within a component. This project focuses on several gross cleaning methods and the verification metrics associated with additive manufactured parts for oxygen propulsion usage.

Mitchell, Mark A.↗

DOE OSTI2026

Filament Extension Atomization for High Solids Loading in Energy Efficient Spray Drying Systems

We demonstrate that we could scale FEA to reach outputs needed by industrial production, while increasing solids loading of the sprayed product by at least 30% and maintaining equal or better spray powder. After testing a wide range of products, in collaboration with industry partners we decided on our primary spray products of dry whey and WPC-80, two common materials processed and sold by US manufacturers with different parameters. We sprayed these with FEA at solids loadings of 70% for dry whey and 45% for WPC-80 with a spray output with particle sizes similar to industrial particles sizes and reduced variation in particle size. We simultaneously scaled up FEA first with a multi-nip with 6 nips surrounding a central roller with parallel axis of rotation and eventually with a tapered design that solved problems we encountered with our initial design. We were able to achieve output from a single array from our first design of up to 4.7 liters per minute (L/min) and from an array of our second multi-nip of 8 L/min exceeding expectations. This demonstrates that FEA technology can indeed be scaled up to meet the needs of industrial production. More arrays can be added as necessary to meet a wide range of spray dryer designs. We also tested FEA to create dried powders from a small scale (10 L/hour of water removal) spray dryer. Though we were not able to produce large quantities of powder from FEA due to challenges in integration, the powder we produced was higher quality and produced from higher solids loading materials. From our technoeconomic analysis we for a typically sized spray dryer, we estimate a 27% cost reduction and 41% energy and carbon reduction for WPC-80 and a 39-57% cost reduction and 52-76% energy reduction for sweet dry whey (depending on the exact product).

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

NASA NTRS1972

Stopping rate of negative cosmic-ray muons near sea level.

A relatively simple method for measuring with high sensitivity the rate of stopped negative muons is described. A process in which Ar-37 is obtained from K-39 in connection with the stopping of a negative muon was used in the experiments. The Ar-37 activity can be measured in small proportional counters with extremely low backgrounds. It is possible to remove Ar-37 from potassium acetate powder at room temperature with almost 100 per cent efficiency merely by trapping the gas from the storage container with a charcoal trap at the liquid nitrogen temperature.

Spannagel, G.↗

DOE OSTI2024

System and method for atomic layer deposition of rare-earth oxides on optical grade materials for laser gain media

A method is disclosed for doping a quantity of powder particles. A container having a central chamber is initially charged with a quantity of powder particles. A quantity of precursor is sublimed to form a heated precursor. A quantity of carrier gas is mixed with the precursor to form a mixture of heated precursor/carrier gas. The central chamber is charged with the heated precursor/carrier gas and then moved to cause interaction of the powder particles with the heated precursor/carrier gas to form a first monolayer coating on the powder particles. The heated precursor/carrier gas is then removed from the central chamber and the central chamber is charged with a O2/O3 gas under a plasma. The central chamber is then further moved to produce interaction of the O2/O3 gas with the first monolayer coating on the powder particles to modify the first monolayer coating to create a different, single monolayer coating forming an oxide coating on the powder particles.

Miller, John S.↗

DOE OSTI2022

Effect of Remnant Carbon and Etching of Particles on Pyrolysis Bonded Silicon Carbide (PBSC)

Silicon carbide (SiC) formed through pyrolysis of preceramic polymers loaded with SiC particles has gained significant attention for applications such as coatings, composite matrix modifications, and most importantly additive manufacturing. This work presents combined synchrotron XRD, Raman spectroscopy, scanning electron microscopy, nano-indentation, and Vickers indentation of pyrolysis bonded SiC to shed light on the changes of composition and mechanical properties of these materials. Characterization was performed on samples that were heat treated ranging from the synthesis 850 °C up to 1500 °C. Pre-treatments of the powders prior to pellet synthesis, such as heat treatment and etching using a hydrofluoric acid (HF), were investigated. It is shown that the degradation of mechanical properties when exposed to higher temperatures is due to the burnout of amorphous carbon clusters remnant of the pyrolysis process of the preceramic polymer. Furthermore, prior HF etching and removal of the native oxide layer of the powders showed improved density and hardness values in the final pellets. The average Vickers hardness of the control samples were 4.59 GPa and later 3.74 GPa when exposed to 1500 °C, while the samples synthesized using powders that were etched with HF had an average hardness value of 9.37 GPa and later 6.86 GPa when exposed to 1500 °C.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2022

All-Inorganic Open-Framework Chalcogenides, A 3 Ga 5 S 9 · x H 2 O ( A = Rb and Cs), Exhibiting Ultrafast Uranyl Remediation and Illustrating a Novel Post-Synthetic Preparation of Open-Framework Oxychalcogenides

Fast and effective uranyl sequestration is of interest to the nuclear industry. Recently layered chalcogenide materials have demonstrated fast, selective, and efficient sorption properties towards uranyl cations and the development and investigation of new types of chalcogenide materials continues to be of interest and represents an intriguing option for uranyl remediation. Three new all-inorganic A 3 Ga 5 S 9 ·xH 2 O (A = Rb, Rb/Cs, and Cs) open-framework chalcogenides were obtained via an in-situ alkali carbonate to alkali sulfide conversion process achieved under mild hydrothermal conditions. The structures of the all-inorganic open framework chalcogenides consist of a 2-fold interpenetrated diamond-like 3D framework containing pseudo-T 3 [Ga 10 S 20 ] 10– supertetrahedra. 48% of the structural volume is occupied by A + cations and water species, as established by single-crystal X-ray diffraction (SCXRD), infrared (IR) and energy-dispersive (EDS) spectroscopies. The dynamic nature of the A + cations and water molecules within the pores was investigated via single crystal X-ray diffraction as well as by IR spectroscopy monitored H 2 O to D 2 O exchange experiments. Framework stability was probed with post-synthetic treatment of A 3 Ga 5 S 9 ·xH 2 O (A = Rb and Cs) samples in acidic solutions that resulted in the formation of the oxysulfide (A/H) 3 Ga 5 S 9–y O y ·xH 2 O (A = Rb and Cs; y = 0–1), as shown by SCXRD and IR. Ion-exchange studies on A 3 Ga 5 S 9 ·xH 2 O (A = Rb and Cs) samples were carried out utilizing a uranyl acetate solution. The presence of the UO 2 2+ species in the ion-exchanged product was supported by IR and EDS spectroscopies. Batch method ion-exchange experiments on Cs 3 Ga 5 S 9 ·xH 2 O powder demonstrated fast kinetics with 95% uranyl removal from the uranyl acetate solution during the first minute, a maximum uranyl uptake capacity of 15mg/g, and the subsequent elution of uranyl species with KCl solution. Furthermore, the porous and dynamic nature of the A 3 Ga 5 S 9 ·xH 2 O framework coupled with effective UO 2 2+ ···S 2– bonding interactions makes it a good potential sorbent for uranyl remediation from aqueous media.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1974

Improved toughness of refractory compounds

The concept of grain-boundary-engineering through elimination of the grain-boundary silicate phase in silicon nitride was developed. The process involved removal of the silica from the nitride powder via a thermal treatment coupled with the use of nitride additives to compensate the remaining oxygen. Magnesium and aluminum nitrides are found to be the most effective additive for use as oxygen compensators. Strength decreases at elevated temperatures are not observed in the alumina containing material. The creep rate of a dual additive sialon composition was two orders of magnitude lower at 1400 C than commercial silicon nitride. A cursory analysis of the creep mechanism indicate that grain-boundary sliding is avoided through elimination of the grain-boundary silicate phase.

Wright, T. R.↗

NASA NTRS1990

One step HIP canning of powder metallurgy composites

A single step is relied on in the canning process for hot isostatic pressing (HIP) powder metallurgy composites. The binders are totally removed while the HIP can of compatible refractory metal is sealed at high vacuum and temperature. This eliminates outgassing during hot isostatic pressing.

John J Juhas↗

NASA NTRS2000

Gear Durability Shown To Be Improved by Superfinishing

Gears, bearings, and similar mechanical elements transmit loads through contacting surfaces. At the NASA Glenn Research Center at Lewis Field, we postulated that the fatigue lives of gears could be improved by providing smoother tooth surfaces. A superfinishing process was applied to a set of conventionally ground, aerospace-quality gears. This process produced a highly polished, mirrorlike surface as shown in the preceding photograph. The surface fatigue lives of both superfinished and conventionally ground gears were measured by experiments. The superfinished gears survived about four times longer than the conventionally ground gears. These superfinished gears were produced from conventionally ground, aerospace-quality gears whose geometry had been inspected. The gears were superfinished by placing them in a vibrating bath consisting of water, detergent, abrasive powder, and small pieces of zinc. Upon removal from the bath, the surfaces were highly polished, as depicted in the preceding photograph. The gears were again inspected, and dimensional measurements made before and after the superfinishing operation were compared. Superfinishing removed the peaks of the grinding marks and left a much smoother surface. Profile and spacing checks proved that the overall gear tooth shape was not affected in any harmful way. Superfinishing uniformly removed approximately 2.5 microns from each surface.

Krautz, Timothy L.↗

NASA NTRS1983

Technique for removing resin from a molded object

Resin is removed from a molded object in such a way that no cracks or expansion occurs in the casting. The resin is first mixed with a ceramics powder or metal powder. This mixture is then molded and the resin is removed by heat. The molded object is then placed into a container which is sealed and large enough to allow the gas from the resin to be controlled by heat from the resin. The gas pressure at the surface of the object is increased by the gas pressure generated from the resin and the resin removed. The increase in gas pressure from the surface of the molded object is 1.5 atm to 3 atm at 350 C to 400 C.

Hemmi, I.↗

NASA NTRS1967

Isostatic compression process converts polyaromatics into structural material

Isostatic compression process compacts certain powdered aromatic polymers into homogeneous materials that can be machined to form useful components, such as bearings. It provides for complete removal of air in the interstitial spaces surrounding the granules of the powdered polymer before the powder is subjected to isostatic compression.

Ingham, J. D.↗

NASA NTRS2005

Net-Shape HIP Powder Metallurgy Components for Rocket Engines

True net shape consolidation of powder metal (PM) by hot isostatic pressing (HIP) provides opportunities for many cost, performance and life benefits over conventional fabrication processes for large rocket engine structures. Various forms of selectively net-shape PM have been around for thirty years or so. However, it is only recently that major applications have been pursued for rocket engine hardware fabricated in the United States. The method employs sacrificial metallic tooling (HIP capsule and shaped inserts), which is removed from the part after HIP consolidation of the powder, by selective acid dissolution. Full exploitation of net-shape PM requires innovative approaches in both component design and materials and processing details. The benefits include: uniform and homogeneous microstructure with no porosity, irrespective of component shape and size; elimination of welds and the associated quality and life limitations; removal of traditional producibility constraints on design freedom, such as forgeability and machinability, and scale-up to very large, monolithic parts, limited only by the size of existing HIP furnaces. Net-shape PM HIP also enables fabrication of complex configurations providing additional, unique functionalities. The progress made in these areas will be described. Then critical aspects of the technology that still require significant further development and maturation will be discussed from the perspective of an engine systems builder and end-user of the technology.

Bampton, Cliff↗

DOE OSTI2026

Hybrid Additive Manufacturing and Electric Field-Assisted Sintering of High-temperature Heat Exchangers via Sacrificial Channel Molds

A hybrid manufacturing approach, integrating additive manufacturing (AM) with powder methodology via electric field-assisted sintering (EFAS), was developed for the fabrication of high-temperature compact heat exchangers (CHX) from refractory metals. The methodology employed additively manufactured sacrificial channel molds (SCMs) as shapeholders for CHX channels, which were embedded in metal powders using EFAS. Following embedding, the SCMs were chemically dissolved to form the internal channel network. SCMs were fabricated using both digital light processing (DLP) and direct ink writing (DIW) from chemically reactive, calcium-based ceramic feedstocks with varying ratios of Al2O3 reinforcement. The microstructure, phase composition, and dissolution behavior of both as-printed and embedded SCMs were investigated. The shrinkage behavior of the SCMs embedded in refractory metals, as well as the interfacial characteristics between the SCMs and metal matrix, were studied. The results showed that the SCMs containing sufficient chemical reactive ceramics dissolved effectively before and after embedding. The as-printed SCMs retained the phase composition of their feedstocks, but the embedded SCMs containing calcium-based ceramics and Al2O3 exhibited the formation of calcium aluminates due to high temperature exposure during embedding. Most SCMs exhibited a cellular Al2O3 network filled with Ca-rich ceramics. Shrinkage after embedding was strongly dependent on SCM density, with lower density SCMs exhibiting greater shrinkage. A thin SCM-affected zone was observed at the metal matrix surface, characterized by increased porosity compared to the bulk matrix. This effect was attributed to infiltration of the SCM materials into powder particle boundaries under pressure, followed by their removal during dissolution. This study demonstrates the feasibility of manufacturing CHXs from hard-to-process refractory metals for use in harsh environments.

36 - MATERIALS SCIENCE↗

DOE OSTI2024

Persistence of Methionine Side Chain Mobility at Low Temperatures in a Nine‐Residue Low Complexity Peptide, as Probed by 2 H Solid‐State NMR

Abstract Methionine side chains are flexible entities which play important roles in defining hydrophobic interfaces. We utilize deuterium static solid‐state NMR to assess rotameric inter‐conversions and other dynamic modes of the methionine in the context of a nine‐residue random‐coil peptide (RC9) with the low‐complexity sequence GGKGMGFGL. The measurements in the temperature range of 313 to 161 K demonstrate that the rotameric interconversions in the hydrated solid powder state persist to temperatures below 200 K. Removal of solvation significantly reduces the rate of the rotameric motions. We employed 2 H NMR line shape analysis, longitudinal and rotation frame relaxation, and chemical exchange saturation transfer methods and found that the combination of multiple techniques creates a significantly more refined model in comparison with a single technique. Further, we compare the most essential features of the dynamics in RC9 to two different methionine‐containing systems, characterized previously. Namely, the M35 of hydrated amyloid‐β 1–40 in the three‐fold symmetric polymorph as well as Fluorenylmethyloxycarbonyl (FMOC)‐methionine amino acid with the bulky hydrophobic group. The comparison suggests that the driving force for the enhanced methionine side chain mobility in RC9 is the thermodynamic factor stemming from distributions of rotameric populations, rather than the increase in the rate constant.

Vugmeyster, Liliya↗

NASA NTRS2010

Reducing Seal Adhesion in Low Impact Docking Systems

Silicone elastomers, used in seals for airlocks or other sealing surfaces in space, are sticky in their as-received condition. Because of the sticking, a greater force may be needed to separate the mating surfaces. If the adhesion is sufficiently high, a sudden unpredicted movement of the spacecraft during undocking, vibration, or uneven release could pull off the seal, resulting in a damage that would have to be repaired before another docking. The damaged seal can result in significant gas leakage and possibly in a catastrophic mishap impacting the safety of the crew. It is also possible that a compromised seal could result in a delayed but sudden gas leak that could put the crew at unexpected risk. This is especially of concern for androgynous seals, which have identical mating surfaces on both sides for interchangeability and redundancy. Such seals typically have elastomer-on-elastomer sealing surfaces. To reduce sticking, one could use release agents such as powders and lubricants, but these can be easily removed and transferred to other surfaces, causing uneven sealing and contamination. Modification of the elastomer surface to make a more slippery and less sticky surface that is integral with the bulk elastomer would be more desirable.

Banks, Bruce A.↗