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At least 1,243 records · Page 69
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

The Effect of Membrane Structure Prepared from Carboxymethyl Cellulose and Cellulose Nanofibrils for Cationic Dye Removal

Water-stable and eco-friendly membranes were fabricated from carboxymethyl cellulose (CMC) acting as anionic adsorbent and cellulose nanofibrils (CNFs) as strengthening filler by solvent- and unidirectional freeze-casting processes, both supported with simultaneous citric acid (CA) mediated cross-linking. Spectroscopic, thermogravimetric and potentiometric titration techniques were applied to evaluate the efficacy of the cross-linking as well as to quantify the processing-dependant surface charge. In addition, the CMC/CNF assembling and membrane porosity were identified microscopically as the combinatorial effect of components ratio and the applied fabrication technique. Finally, the membrane’s cationic dyes adsorption capacity and kinetic were evaluated depending on the dyes ionization constants, solution pH, and the contact time using batch equilibrium experiment, and further evaluated for filtration performance at optimal pH. The resulting, freeze-casted membranes demonstrate anisotropic to isotropic and highly (> 90%) porous structures with gradient pore sizes (from few nm up to 200 µm range). This provides relatively high and stable flux rates (150–190 kL/m{sup 2} h MPa) with ~ 100% cationic dye adsorption, fast dynamic (8.536–5.446 kg/g min) and capacity (1828–1398 g/kg), which highlight their potential in dead-end filtration technologies without need for additional separation step. The similar dye adsorption capacity was assessed for denser and nano-porous (< 50 nm) solvent-casted membranes, however, with much lower and time-declining flux rates (100–10 L/m{sup 2} h MPa), demonstrating their potential usage in spiral wound-cross-flow modules. Both types of membranes anyhow showed high dye removal capacity (≥ 90%) even after 4th (solvent-casted) and 50th (freeze-casted) reusing cycle, present a high-value alternative to commercial activated carbons or other bio-nano-absorbents.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Relationships Between Solidification Parameters in A319 Aluminum Alloy

The design of high-performance materials depends on a comprehensive understanding of the alloy-specific relationships between solidification and properties. However, the inconsistent use of a particular solidification parameter for presenting materials characterization in the literature impedes inter-study comparability and the interpretation of findings. Therefore, there is a need for accurate expressions relating the solidification parameters for each alloy. In this study, A319 aluminum alloy castings were produced in a permanent mold with various preheating temperatures in order to control metal cooling. Analysis of the cooling curve for each casting enabled the identification of its liquidus, Al-Si eutectic, and solidus temperatures and times. These values led to the calculation of the primary solidification rate, total solidification rate, primary solidification time, and local solidification time for each casting, which were related to each other as well as to the average casting SDAS and material hardness. Expressions for each of their correlations have been presented with high coefficients of determination, which will aid in microstructural prediction and casting design.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Change in Porosity of A356 by Holding Time and Its Effect on Mechanical Properties

In most of the practical casting operations, it is important to be able to cast large number of part with one single melt. Therefore, when quantity of the charge and melting crucible is increased, during casting process, the liquid is led to settle for a long period of time. In this work, 10 kg charge of A356 was melted at 750 °C and held for 240 min. A sand mold with different thickness was cast at 30, 60, 120, and 240 min of holding time of the liquid, before and after degassing conditions. Melt quality was measured by reduced pressure test, and pore size and number were measured at each cast part. A correlation between bifilm index and tensile properties was established. It was found that melt quality was decreased with increased holding time and pore formation was enhanced linearly. Additionally, mechanical properties of the alloy were decreased with decreased melt quality and increased pore formation due to holding time of the liquid.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructural Transition of (CuFeMnNi){sub 1−x}Cr{sub x} (x = 0-0.25) High-Entropy Alloys

The influence of Cr on the microstructure and hardness of the cast and annealed (CuFeMnNi){sub 1−x}Cr{sub x} (x = 0, 0.05, 0.1, 0.15, 0.2 and 0.25) high-entropy alloys were investigated systematically. The results revealed that the microstructures of (CuFeMnNi){sub 1−x}Cr{sub x} (x = 0, 0.05 and 0.1) alloys were composed of (Fe, Ni and Cr)-rich FCC1 and (Cu, Mn)-rich FCC2 phases. No obvious change in the dendritic size was detected between cast and related annealed alloys, indicating the excellent thermal structure stability of the studied alloys. The microstructures of the cast (CuFeMnNi){sub 1−x}Cr{sub x} (x = 0.15, 0.2 and 0.25) alloys contained FCC1, FCC2 and (Cr, Fe)-rich BCC phases, while those of the annealed alloys were composed of FCC1, FCC2 and ρ phases. The significant transition from BCC phase to ρ phase was detected. Moreover, the hardness of both cast and annealed (CuFeMnNi){sub 1−x}Cr{sub x} alloys increased with the increasing Cr content. The hardness of annealed (CuFeMnNi){sub 1−x}Cr{sub x} (x = 0, 0.05 and 0.10) alloys reduced slightly as compared to corresponding cast alloys, whereas the hardness of the annealed (CuFeMnNi){sub 1−x}Cr{sub x} (x = 0.15, 0.2 and 0.25) alloys increased.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Chemical interaction and compatibility of uranium mononitride and alumina forming austenitic stainless steel

Uranium mononitride (UN) and alumina forming austenitic (AFA) stainless steel are a potential fuel-cladding combination for the lead-cooled fast reactor (LFR). Chemical compatibility between UN and AFA steel needs to be verified before implementation in a nuclear reactor. Diffusion couple experiments at 823 K and 1023 K were conducted for nonirradiated UN samples in contact with as-cast (no thermally grown Al 2 O 3 ) and preoxidized (with thermally grown Al 2 O 3 ) AFA for 500 and 1000 h in an inert environment. Preoxidized AFA exhibited little to no interaction with all UN samples tested at both 823 K and 1023 K, displaying the stability and capability of the Al 2 O 3 layer to prevent chemical interaction and inter-diffusion with UN. Chemical interaction occurs between UN and as-cast AFA. At 1023 K, an aluminum and nitrogen rich phase (likely AlN) formed along the interface of as-cast AFA and UN samples. At 823 K the AlN phase was not prominently observed due to the reduced diffusivity of aluminum through AFA. The aluminum and nitrogen-enriched phase was also observed in a high temperature pressure-assisted test sample of UN and as-cast AFA thermally treated at 1373 K. Finally, in UN samples doped with a low weight percent of UO 2 (< 3 wt%), AlN was not detected along the interface at either temperatures, and an Al 2 O 3 layer likely formed along the interface and prevented further chemical interaction between UN and as-cast AFA.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructure and mechanical properties of hypoeutectic Al–6Ce–3Ni-0.7Fe (wt.%) alloy

Here, a hypoeutectic, Fe-modified Al–Ce–Ni alloy (Al–6Ce–3Ni-0.7Fe, wt.%) is studied in terms of microstructure, thermal stability, ambient temperature strengthening, and creep resistance. The as-cast microstructure consists of primary Al dendrites and interdendritic binary eutectic regions (Al–Al11Ce3 and/or Al–Al9(Fe,Ni)2), with micron/submicron lamellar spacing, depending on the location along the height of the ingot. The cast alloy exhibits excellent coarsening resistance at 400 °C, with mostly unchanged microstructure and microhardness after 6 weeks of aging, indicating good thermal stability of Al11Ce3 and Al9(Fe,Ni)2. Orowan strengthening and load transfer are identified as strengthening mechanisms at ambient and elevated temperature. A high volume fraction of the intermetallic phases (providing load transfer) and relatively coarse eutectic spacing (for modest Orowan strengthening) result in a moderate as-cast microhardness of 566 ± 32 MPa. Creep resistance at 300 and 350 °C is similar to a binary Al-12.5Ce eutectic alloy (with twice the Ce content) because of two countering effects: Al–6Ce–3Ni-0.7Fe shows a higher volume fraction of strengthening intermetallic phases, but it also exhibits a large fraction of primary Al dendrites which weaken the alloy. By contrast, the alloy, when laser-remelted at the surface, has a fully eutectic microstructure without primary aluminum dendrites achieved by high undercooling on solidification, with a refined network of eutectic phases that doubles the microhardness as compared to the cast alloy. Whereas coarsening is faster due to the shorter diffusion distances between the eutectic phases, hardness remains ~30% higher than the as-cast alloy after ~6 weeks aging at 400 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Tissue factor pathway inhibitor prevents airway obstruction, respiratory failure and death due to sulfur mustard analog inhalation

Sulfur mustard (SM) inhalation causes airway injury, with enhanced vascular permeability, coagulation, and airway obstruction. The objective of this study was to determine whether recombinant tissue factor pathway inhibitor (TFPI) could inhibit this pathogenic sequence. Methods: Rats were exposed to the SM analog 2-chloroethyl ethyl sulfide (CEES) via nose-only aerosol inhalation. One hour later, TFPI (1.5 mg/kg) in vehicle, or vehicle alone, was instilled into the trachea. Arterial O{sub 2} saturation was monitored using pulse oximetry. Twelve hours after exposure, animals were euthanized and bronchoalveolar lavage fluid (BALF) and plasma were analyzed for prothrombin, thrombin–antithrombin complex (TAT), active plasminogen activator inhibitor-1 (PAI-1) levels, and fluid fibrinolytic capacity. Lung steady-state PAI-1 mRNA was measured by RT-PCR analysis. Airway-capillary leak was estimated by BALF protein and IgM, and by pleural fluid measurement. In additional animals, airway cast formation was assessed by microdissection and immunohistochemical detection of airway fibrin. Results: Airway obstruction in the form of fibrin-containing casts was evident in central conducting airways of rats receiving CEES. TFPI decreased cast formation, and limited severe hypoxemia. Findings of reduced prothrombin consumption, and lower TAT complexes in BALF, demonstrated that TFPI acted to limit thrombin activation in airways. TFPI, however, did not appreciably affect CEES-induced airway protein leak, PAI-1 mRNA induction, or inhibition of the fibrinolytic activity present in airway surface liquid. Conclusions: Intratracheal administration of TFPI limits airway obstruction, improves gas exchange, and prevents mortality in rats with sulfur mustard-analog-induced acute lung injury. - Highlights: • TFPI administration to rats after mustard inhalation reduces airway cast formation. • Inhibition of thrombin activation is the likely mechanism for limiting casts. • Rats given TFPI had improved tissue oxygenation, and mortality was prevented.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2023

Earthworms Exposed to Polyethylene and Biodegradable Microplastics in Soil: Microplastic Characterization and Microbial Community Analysis

While much is known about microplastics in aquatic environments, only few studies have focused on how microplastics interact with terrestrial organisms. The objective of our study was to investigate the interactions of earthworms with microplastics in a natural environment with environmentally realistic plastic concentrations. Here we investigated whether earthworms would ingest microplastics and incorporate them into their bodies and cast, and whether microplastics would alter the intestinal and soil microbiome. Lumbricus terrestris was exposed to two types of mi croplastics, biodegradable polybutylene adipate terephthalate (PBAT) and low-density polyethylene (LDPE) in mesocosoms filled with natural soil. Microplastics were mixed with poplar leaves and earthworms were allowed to forage for food for 20 days. Surface and bulk soil, earthworm cast, and earthworms themselves were sampled and analyzed for plastic content and microbial communities. Earthworms did not show macroscopic health deterioration (weight loss, vitality). We observed microplastics particles in earthworm casts and guts. Raman spectroscopy indicated that PBAT in guts and cast had degraded to some extent; however, LDPE remained unchanged among the different samples. Microbial analysis showed that soil and casts has similar microbial communities; however, they were signicantly different from the guts samples. Microplastic treatments did not result in a statistically signicant change in bacterial richness, diversity or community composition compared to controls. Taken together, our results suggest that, at environmentally realistic concentrations and short exposure times, PBAT and LDPE microplastics do not have adverse effects on Lumbricus terrestris earthworms.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Processing-Dependent Structure and Poroelasticity of Nafion in Liquid Water

Ionomers act as the solid polymer electrolyte membrane in many modern electrochemical devices, yet the role of their nanostructure in modulating the poroelastic response remains poorly understood, especially in liquid water, where few techniques can measure simultaneous transport-mechanical properties. Poroelastic Relaxation Indentation (PRI) is uniquely suited for measuring time-dependent transport-mechanical properties of porous solids, specifically hydraulic diffusivity, elastic modulus, Poisson’s ratio, and intrinsic permeability, for porous solids. While ionomers such as Nafion are not porous in the typical sense, Nafion has a nanophase-segregated structure that, when fully swollen in liquid water, behaves as a poroelastic solid with a coupled mechanical-transport response. Using a poroelastic framework, we investigate how casting and pretreatment of Nafion membranes alter their poroelastic response in liquid environments. We characterize both extruded and dispersion-cast Nafion membranes pretreated in water at 25 or 100 °C and relate the mechanical-transport properties to the ionomer structure via hydrophilic and intercrystalline domain spacing measured using Small-Angle X-ray Scattering (SAXS). At 25 °C, dispersion-cast membranes exhibit distinctly lower hydraulic diffusivity and intrinsic permeability than extruded membranes but with comparable mechanical properties. Pretreatment at 100 °C increases hydrophilic domain spacing, improving transport but at the expense of mechanical stiffness. Dispersion-cast membranes respond more strongly to pretreatment than extruded membranes. Using the Carman-Kozeny pore network model and the hydrophilic domain-spacing, we estimate the pore radius and tortuosity to show how pretreatment reduces structure-related tortuosity differences between dispersion-cast and extruded membranes. Here, in this work, we show that nanophase-segregated materials such as Nafion can be rigorously characterized using poroelasticity, resulting in physically meaningful transport-mechanical properties. Coupling PRI with SAXS provides insights into the nanostructural features that govern the coupled mechanical-transport response. By establishing PRI for a nanophase-segregated material, this approach opens avenues for this technique’s application in other hydrated polymeric materials not typically considered to be poroelastic.

Shen, Margaret [University of California, Berkeley↗
DOE OSTI2021

Development of high B s Fe–Ni-based metal amorphous nanocomposite by optimization of glass-forming ability

Thermocalc simulations identified compositions with good glass-forming ability (GFA) by locating minima in liquidus temperature, and solidification range in (Fe 70 Ni 30 ) x (B-Si-Nb) 100-x alloys with x = 82% and x = 85%, increased compared to previously developed x = 80% alloys. 3 compositions in the x = 82% system and 1 in the x = 85% system were successfully cast as amorphous magnetic ribbon. Magnetic properties of as-cast alloys showed improvements in Curie temperature and saturation induction, especially for the 85% alloy. Crystallization behavior in the 85% alloy was determined to occur as a 2-step process. Annealing studies showed (Fe 70 Ni 30 ) 82 Nb 2 Si 0 B 16 and (Fe 70 Ni 30 ) 82 Nb 3 Si 0 B 15 alloys to exhibit low coercivity and high B s with annealing. TEM results show significant crystallization in as-cast ribbon. The (Fe 70 Ni 30 ) 85 Nb 0.5 Si 0 B 14.5 alloy as-cast has small, uniformly distributed grains, allowing a useful nanocrystalline alloy to be produced as cast. Lastly, the parameter ΔT xg , the temperature range in which the material can be thermomechanically processed, was in the range of 12–23 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Poly(p-Phenylene Sulfonic Acids). PEMs with frozen-in free volume

Early work with rigid rod aromatic polyelectrolytes implied that steric hindrance in packing of the rigid rods left unoccupied volumes that could absorb and hold water molecules strongly. We called this “frozen in free volume). It is illustrated and contrasted with the packing of flexible backbone polyelectrolytes (Reference 5 of this report). This was quantified for poly(biphenylene disulfonic acid) (PBDSA) and poly(phenylene disulfonic acid) (PPDSA). We found that PPDSA held three water molecules per acid group down to 11% relative humidity (RH) and had very high conductivity even at these low RHs. (Reference 1 of report.) The frozen-in free volume was calculated to be equivalent to a λ of 3.5. The work reported below concentrated on studying these polymers and their copolymers with biphenylene disulfonic acid. As expected, the polyelectrolytes are water soluble. Several approaches towards making water stable films were studied. Grafting alkyl benzene substituents on sulfonic acid groups had worked for PBPDSA (1) so it was tried with PPDSA and a 20%/80% copolymer of BPDSA and PDSA (B20P80). T-butyl, n-octyl and n-dodecyl benzene were grafted. Good films could be made. Water absorption and conductivity were studied as a function of RH and temperature (Reference 2). When less than 20% of the sulfonic acid groups were grafted, conductivity was much higher than that of Nafion NR212 at all RHs. At low graft levels, conductivity was ten times higher. Mechanical properties and swelling were acceptable below 90% RH. However, all the films were unstable in water and slowly disintegrated. The proposed explanation was that the molecules formed nano-aggregates in solution held together by hydrophobic bonding. Their cast films disintegrated when placed in water since hydrophobic bonding between the nano-aggregates was poor. We then shifted to crosslinking as a method to produce water stable films (References 3 and 4). Biphenyl could easily be reacted with the polymer, generating biphenyl sulfone grafts. Films were cast and then crosslinked by heating to 210°C for at least one hour. There was no loss of acid groups even after heating at 225°C for two hours. PPDSA and B20P80 polymers were grafted and crosslinked. Conductivity and water absorption were measured on polymers with grafting degrees from 3 to 16%. As before they all had much higher conductivity than Nafion NR212. One sample was tested as a fuel cell membrane. Unfortunately it tore; the tear was mended with a 3M ionomer. There was some hydrogen leakage. However, the current at a given voltage was about 95% that of a Nafion NR212 membrane over the whole useful range. Considering that this was the first test for such a system, this is remarkable performance. A mechanically better membrane was tested at the end of the grant period. This did not have tears or micro cracks (Reference 5). Testing confirmed earlier data (Sergio Granados-Focil, Ph. D. Thesis, CWRU. 2006) that such very polar membranes were excellent barriers to hydrogen diffusion. Standard measurements showed no hydrogen leakage. This was confirmed by open circuit voltage measurements. They were higher than those of the Nafion NR212 cells. Again the single cell performance was about 95% that of the Nafion SR212 cell over the whole range. These films show great promise. They are very stable and perform very well at very low humidity. They should be able to outperform the present cells with relatively little further development. A second project is reported fully in the final report since it was not published. Its goal was to make membranes with high conductivity and good mechanical strength that would have a constant volume at all RHs. We made large planar 2-D polymers containing 1.5 nm holes lined with sulfonic acid groups. These should hold water very strongly. The largest made was calculated to have a number average diameter of 29 nm. It was expected that when they were cast, they would aggregate and create channels for proton conduction. However, they were so large that they aggregated in solution during preparation. Measurements showed that the aggregates developed long channels. This was demonstrated and is reported. Unfortunately, the aggregates could not be cast with the channels perpendicular to the film plane. If methods are developed to keep the molecules in solution until they are cast, their planes should be parallel and the channels perpendicular to the film direction. They could be very interesting and perhaps important materials.

25 ENERGY STORAGE↗
DOE OSTI2014

Influence of Homogenization on the Mechanical Properties and Microstructure of the U-10Mo Alloy

In Phase 1 of this study, the mechanical properties of as-cast, depleted uranium alloyed with 10 weight percent molybdenum alloy (U-10Mo) samples were evaluated by high-temperature compression testing. Compression testing was conducted at three strain rates over a temperature range of 400 to 800°C. The results indicated that with increasing test temperature, the material flow stress decreases and the material becomes more sensitive to strain rate. In addition, above the eutectoid transformation temperature (~ 550°C), the drop in material flow stress is prominent and shows a strain-softening behavior, especially at lower strain rates. In the second part of this research, we studied the effect that homogenization heat treatment had on the high temperature mechanical properties and microstructure of the cast U-10Mo alloy. Various homogenization times and temperatures were studied ranging between 800 and 1000°C for 4 to 48 hours. Based on the microstructural response in this homogenization study, a heat treatment cycle of 800°C for 24 hours and another at 1000°C for 16 hours were selected as the times at temperature to achieve a fully homogenized sample. Samples from these conditions were then compression tested at a variety of temperatures ranging from 500 to 800°C. The microstructure of these samples were compared to the as-cast samples and to a baseline sample homogenized at 1000°C for 16 hours. The results indicate that below the eutectoid temperature (~ 550°C) all three samples showed strain hardening and followed similar trends. Above the eutectoid temperature, the yield strength of the material decreased linearly. For the as-cast sample and the sample homogenized at 800°C for 24 hours, the n-values were negative, whereas for the samples homogenized at 1000°C for 16 hours the material exhibited a perfectly plastic behavior. The as-cast sample, heat treated at 800°C for 24 hours, showed significant lamellar structure transformation that seems to have precipitated along the grain boundaries in the molybdenum-lean regions. In similar samples, homogenized at 800°C for 24 hours and tested at 650°C, the backscattered-electron scanning electron microscopy images revealed a composite structure of lamellar phase and nano-scale molybdenum-rich and -lean phases along the grain boundaries. These phases may have been responsible for the lowering of the flow stress in the material observed in the Phase 1 work. For comparison, the samples homogenized at 1000°C for 16 hours showed no such transformations.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Cost-effective, Thin-film SOFCs for Reliable Power Generation (Final Report)

The project was aimed at developing and demonstrating an advanced solid-oxide fuel cell (SOFC) technology to cost-effectively and reliably generate electricity directly from hydrocarbon fuels (e.g., natural gas and coal-derived syngas) for distributed and central generation applications. The studied technology was built on a planar, porous metal-supported SOFC (MS-SOFC) with a unique thin-film structure having its anode intimately supported on a metal substrate. The porous metal support with graded porosity was fabricated from a low-cost scalable phase-inversion tape casting method. Anode, thin-film electrolyte, and cathode were sequentially deposited on the porous metal substrate using atmospheric plasma spray (APS). In this study, it was shown that the composition of the casting slurry could significantly influence the morphology of the metal support fabricated using the phase-inversion tape-casting method. Increasing the solid loading in the slurry favored the formation and growth of finger-like pores to a point, but the presence of excessive solid loading increased the viscosity of the casting slurry, restraining the growth of finger-like pores. With the increase in the amount of the binder polyethersulfone (PESf) in the slurry, well grown finger-like pores and a thin sponge-like layer were formed. Since the parameters of the APS process have a significant effect on the microstructure of coatings, which in turn affects or determines the SOFC cell performance, a series of metal-supported solid oxide fuel cells with a four-layer cell configuration of 430L/Ni-ScSZ/ScSZ/LSCF have been fabricated by a combination of phase inversion tape casting and APS techniques. Electrochemical testing of the cells fabricated from different deposition APS conditions revealed significant differences in cell performance.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2021

Solid Phase Gradient Alloying Method via ShAPE

Alloying has been used to confer desirable properties to various metallic systems since the bronze age. For example, Ni, Mn, and Cr are alloyed into an Fe matrix to make steel, which has improved strength and corrosion resistance (as displayed in Fig. 1). In addition to the type of alloying elements, the amount of alloying elements added into a matrix is also very critical for a material’s mechanical property, physical property, machinability, and cost. Conventionally, new alloys are discovered by combining alloy precursors and elemental constituents into a mixture and melting them together. The solidified product or ingot represents a usually non-homogeneous combination of the chemistry with a microstructure dictated by the physics of solidification. It is time and energy intensive to optimize the alloying amounts via the casting process and hence, economically not conducive to rapid alloy discovery. In addition, the cast microstructure seen in the as-cast ingot is often not the ideal, nor even desired structure for optimized performance. Cast materials often need further processing such as homogenization, annealing, and deformation work put in through rolling, forging, extruding, etc. to have favorable microstructures and properties. A faster method to discover new alloy combinations and evaluate them in their worked or processed form is needed. Recently, Laser Engineered Net Shaping was applied to fabricate gradient compositional material for alloy designing. However, the mechanical properties of this gradient alloy were poor due to the existence of impurities, oxidation and cracks that are inherent in the melt-solidification process. Because of these limitations, we propose to use a solid-phase process (ShAPE) to create bulk materials (extrudates) that vary in composition from one end of the extruded solid to the other. Various manufacturing methods for alloy design including conventional casting method, laser based combinatorial method and current solid phase gradient alloying method are displayed and compared in Fig. 2. ShAPE machine and a schematic of ShAPE process are displayed in Fig. 3. Starting material is processed by a rotating and plunging die to form an extrudate. We are proposing through this methodology to invent a new, bulk-scale combinatorial technique. With this novel technique, alloying element can be dissolved into the matrix with a continued gradient without bulk melting. Formation of inter-metallics and defects originating from melt processing can be avoided. In addition, the ShAPE process creates the mixed alloy chemistry, and meanwhile subjects the material to severe plastic strain, which induces the favorable “worked” microstructure. Products from the ShAPE process can be tested in hardness directly providing a path to rapid evaluation of mechanical properties. The ability to create graded structures using friction stir processing (FSP) has been demonstrated, however using the ShAPE process we believe will lead to much faster and higher fidelity results. When combined with high throughput screening methods of physical, mechanical and microstructural property characterization, efficiency and accuracy of alloy design can be significantly improved.

36 MATERIALS SCIENCE↗
NASA NTRS1975

Preliminary study of oxide-dispersion-strengthened B-1900 prepared by mechanical alloys

An experimental oxide dispersion strengthened (ODS) alloy based on the B-1900 composition was produced by the mechanical alloying process. Without optimization of the processing for the alloy or the alloy for the processing, recrystallization of the extruded product to large elongated grains was achieved. Materials having grain length-width ratios of 3 and 5.5 were tested in tension and stress-rupture. The ODS B-1900 exhibited tensile strength similar to that of cast B-1900. Its stress-rupture life was lower than that of cast B-1900 at 760 C. At 1095 C the ODS B-1900 with the higher grain length-width ratio (5.5) had stress-rupture life superior to that of cast B-1900. It was concluded that, with optimization, oxide dispersion strengthening of B-1900 and other complex cast nickel-base alloys has potential for improving high temperature properties over those of the cast alloy counterparts.

Glasgow, T. K.↗
NASA NTRS1984

Low-cost single-crystal turbine blades, volume 2

The overall objectives of Project 3 were to develop the exothermic casting process to produce uncooled single-crystal (SC) HP turbine blades in MAR-M 247 and higher strength derivative alloys and to validate the materials process and components through extensive mechanical property testing, rig testing, and 200 hours of endurance engine testing. These Program objectives were achieved. The exothermic casting process was successfully developed into a low-cost nonproperietary method for producing single-crystal castings. Single-crystal MAR-M 247 and two derivatives DS alloys developed during this project, NASAIR 100 and SC Alloy 3, were fully characterized through mechanical property testing. SC MAR-M 247 shows no significant improvement in strength over directionally solidified (DS) MAR-M 247, but the derivative alloys, NASAIR 100 and Alloy 3, show significant tensile and fatigue improvements. Firtree testing, holography, and strain-gauge rig testing were used to determine the effects of the anisotropic characteristics of single-crystal materials. No undesirable characteristics were found. In general, the single-crystal material behaved similarly to DS MAR-M 247. Two complete engine sets of SC HP turbine blades were cast using the exothermic casting process and fully machined. These blades were successfully engine-tested.

Strangman, T. E.↗
NASA NTRS1987

Mechanical properties of high gradient and hot isostatically pressed PWA 1480

This program has been designed to evaluate the potential benefits to alloy 1480 material properties due to high thermal gradient casting, hot isostatic pressing, and alternative heat treatment. Alloy 1480 castings have been obtained from vendors representing the extremes of commercial casting thermal gradients. Quantitative characterization of the dendrite arm spacing (DAS) and pore distributions has been conducted. A hot isostatic pressing (HIP) schedule, which avoids the many pitfalls of single crystal HIP has been devised for alloy 1480. In addition, an alternate heat treatment for alloy 1480 has been devised which provides benefits in mechanical properties. The standard gradient cast test material is being evaluated in the standard heat treat condition as a baseline and in the HIP plus alternate heat treated condition. The fhigh gradient cast material is being evaluated in alternate heat treat and HIP plus alternate heat treated conditions. Evaluations focus on demonstration of the benefits due to the applied processes, especially in the area of cyclic life.

Fritzemeier, L. G.↗
NASA NTRS1987

Crystallization behavior of a melt-spun Fe-Ni based steel

Whether Fe-Ni-based alloys solidify with a bcc or fcc structure has been observed by many investigators to be a stronger function of kinetics and undercooling than strictly free-energy minimization. Such behavior has been observed in an Fe(52.8)Ni(28.7)Al(3.4)Ti(6.1)B(9.0) alloy. The alloy was cast as ribbons about 45 microns thick using a dual free-jet variation of chillbock melt spinning against a Cu wheel. Optical, X-ray, and electron analyses of the as-cast and annealed ribbons were performed. A microstructure of at least four layers containing combinations of ecc, bcc, and amorphous phases in differing proportions was observed in the as-cast ribbon. The midthickness layer had the most unusual features, containing fcc grains about 75 nm in size encompassing spherulitic regions as large as 15 microns comprised of fcc grains about 25 nm in size. The crystallization sequence responsible for the as-cast microstructure is discussed in terms of the competition between the formation of bcc and fcc phases as influenced by undercooling, recalescence, and variations in cooling rate experienced by the as-cast ribbon.

Michal, G. M.↗