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At least 667 records · Page 37

Ultrasonic Characterization of Spatially Varying Material Properties in Metal Components Fabricated by Additive Manufacturing

We investigated the sensitivity of ultrasonic measurements to changes in the operating conditions during additive fabrication for 316L stainless steel samples by selective laser melting. We found that the velocity of the ultrasound propagation positively correlates with the energy density used to melt layers of metal powder during the fabrication. In the range of the investigated conditions, the faster ultrasonic propagation, observed with the increase in the energy density, was shown to correspond to the improved hardness and the modulus of 316L stainless steel. Overall, our results indicate the feasibility of ultrasonic characterization of heterogeneities in the material properties of metal components produced by additive manufacturing.

Walton, Kenneth↗

Cs absorption capacity and selectivity of crystalline and amorphous Hf and Zr phosphates

Removal of radioactive Cs from sodium-rich solutions is a technical challenge that goes back to post World War II nuclear waste storage and treatment; and interest in this topic was reinvigorated by the Fukushima-Daiichi nuclear power plant disaster, 10 years ago. Since the 1960's there has been considerable focus on layered Zr phosphates as robust inorganic sorbents for separation of radionuclides such as Cs. Here we present synthesis and characterization, and direct comparison of Cs sorption capacity and selectivity of four related materials: 1) crystalline α-Zr phosphate and α-Hf phosphate, and 2) amorphous analogues of these. Powder X-ray diffraction, thermogravimetry, solid-state 31P magic angle spinning nuclear magnetic resonance (MAS-NMR) spectroscopy, and compositional analysis (inductively coupled plasma optical emission spectroscopy and mass spectroscopy, ICP OES and ICP MS) provided formulae; respectively M(HPO4)2∙1H2O and M(HPO4)2∙4H2O (M = Hf, Zr) for crystalline and amorphous analogues. Maximum Cs loading, competitive Cs-Na selectivity and maximum Cs-Na loading followed by the above characterizations plus 133Cs MAS-NMR spectroscopy revealed that amorphous analogues are considerably better Cs-sorbents (based on maximum Cs-loading and selectivity over Na) than the well-studied crystalline Zr-analogue. Additionally, crystalline α-Hf phosphate is better Cs-sorbent than crystalline α-Zr phosphate. All these studies consistently show that Hf phosphate is less crystallize than Zr phosphate, when obtained under similar or identical synthesis conditions. We attribute this to lower solubility of Hf phosphate compared to Zr phosphate, preventing ‘defect healing’ during the synthesis process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

X-ray diffraction under grazing incidence conditions

Material properties frequently relate to structures at or near surfaces, particularly in thin films. As a result, it is essential to understand these structures at the molecular and atomistic levels. The most accurate and widely used techniques for characterizing crystallographic order are based on X-ray diffraction. When dealing with thin films or interfaces, standard approaches, such as single crystal or powder diffraction, are not suitable. However, X-ray diffraction under grazing incidence conditions can provide the required information. Here, in this Primer, grazing incidence X-ray diffraction (GIXD) is comprehensively introduced, starting from basic considerations on X-ray diffraction at crystals with reduced dimensionality and the optical properties of X-rays, followed by a more in-depth description of an experimental performance, including X-ray sources, goniometers and detectors. Experimental errors, limitations and reproducibility are discussed. Various applications, from highly ordered inorganic single crystal surfaces to weakly ordered polymer thin films, are presented to illustrate the potential of GIXD. Data visualizations, representations and evaluation strategies are summarized, based on the example of anthracene thin films. The Primer compiles information relevant to perform high-quality GIXD experiments, evaluate data and interpret results, to extend knowledge about X-ray diffraction from surfaces, interfaces and thin films.

36 MATERIALS SCIENCE↗

Controlled release of losartan from acid- and heat-treated halloysite nanotubes

In this work, a simple method was used to sustained release of losartan (LOS) as a high blood pressure-controller drug using halloysites (HNT) as a carrier. The present work can be considered as an effective method because of using HNT as a natural source, which is available, inexpensive, safe with specific structure that led to release of drug, gradually. This carrier was improved by calcination and etching processes and their effect was investigated on loading amount and in vitro release of drug from HNT. The products were characterized by various analyses such as: BET (Brunauer–Emmett–Teller), TG (thermal gravimetry), TEM (transmission electron microscopy), and XRD (X-ray powder diffraction). According to the studies, two processes improving had no effect on structure and morphology of HNT and only increased the lumen size of them. It should be noted, removal water molecules through calcination had binary effect on halloysites: enlargement of lumen and decreasing the drug loading. Besides, release rate was investigated and it showed that maximum and minimum release rate of LOS are assigned to simple HNT and etched-HNT (EHNT), respectively. Kinetics studies confirmed that releasing the LOS molecules from HNT followed by diffusion process that is identified as Fickian diffusion.

60 APPLIED LIFE SCIENCES↗

Synthesis and characteristics of porous ceramic tubes: a comparison of centrifugal casting and cold isostatic pressing methods

Short porous ceramic tubes in small quantities are needed for membrane-related research and development efforts and can be synthesized by centrifugal casting (CC) or cold isostatic pressing (CIP) methods. Here, this work evaluates the characteristics of porous ceramic tubes prepared by both methods and provides a strategy for selecting the proper method for ceramic tube fabrication, depending on its application. Samarium-doped ceria (SDC) with an average crystallite size of 10 nm was synthesized by a citrate method and used to make porous SDC tubes by the CC and CIP methods under different conditions. Porous SDC tubes were prepared from an aqueous suspension of the SDC powder with polyvinyl alcohol (PVA) using a cylindrical metallic mold, centrifugated at 4000–6000 rpm, followed by sintering in 1200–1500 °C. SDC tubes were also made by the CIP method from the SDC powder placed inside a cylindrical rubber bag followed by isostatic compression at 1379 bar. The pore structure of the SDC tubes was characterized by helium permeation and liquid nitrogen Archimedes method. Due to high compression pressure giving a low porosity green tube, the CIP method with lower sintering temperature produces SDC tubes with much lower porosity and average pore size and similar tortuosity compared to the CC methods. The CIP method should be used to prepare low porosity or dense ceramic tubes, and the CC method should be used for preparing high-porosity ceramic tubes or tubes with pore gradient tube wall.

36 MATERIALS SCIENCE↗

Copper-containing ceramic precursor synthesis: Solid-state transformations and materials technology

Three copper systems with relevance to materials technology are discussed. In the first, a CuS precursor, Cu4S1O (4-methylpyridine)(sub 4)- (4-MePy), was prepared by three routes: reaction of Cu2S, reaction of CuBr-SMe2, and oxidation of copper powder with excess sulfur in 4-methylpyridine by sulfur. In the second, copper powder was found to react with excess thiourea (H2NC(S)NH2) in 4-methylpyridine to produce thiocyanate (NCS(-)) complexes. Three isolated and characterized compounds are: Cu(NCS)(4-MePy)(sub 2), a polymer, (4-MePy-H)(Cu(NCS)(sub 3)(4-MePy)(sub 2)), a salt, and t-Cu(NCS)(sub 2)(4-MePy)(sub 4). Finally, an attempt to produce a mixed-metal sulfide precursor of Cu and Ga in N-methylimidazole (N-MeIm) resulted in the synthesis of a Cu-containing polymer, Cu(SO4)(N-MeIm). The structures are presented; the chemistry will be briefly discussed in the context of preparation and processing of copper-containing materials for aerospace applications.

Hepp, Aloysius F.↗

Producing Zirconium Diboride Components with Complex, Near-Net Shape Geometries by Aqueous Room-Temperature Injection Molding

Room-temperature injection molding is proposed as a novel, low-cost and more energy efficient manufacturing process capable of forming complex-shaped zirconium diboride (ZrB2) parts. This innovative processing method utilized aqueous suspensions with high powder loading and a minimal amount (5 vol.) of water-soluble polyvinylpyrrolidone (PVP), which was used as a viscosity modifier. Rheological characterization was performed to evaluate the room-temperature flow properties of ZrB2-PVP suspensions. ZrB2 specimens were fabricated with high green body strength and were machinable prior to binder removal despite their low polymer content. After binder burnout and pressureless sintering, the bulk density and microstructure of specimens were characterized using Archimedes technique and scanning electron microscopy. X-Ray Diffraction was used to determine the phase compositions present in sintered specimens. Ultimate strength of sintered specimens will be determined using ASTM C1323-10 compressive C-ring test.

Near-Net Shape Forming↗

The Effect of Composition on Microstructure and Properties for Additively Manufactured Superalloy 718

Additive manufacturing (AM) represents an exciting new approach towards producing metallic aerospace components. The ability to make complex geometries that were impossible to create using conventional manufacturing methods has sparked interest from the aerospace community, including NASA. The use of AM components for crucial and human rated space missions necessitates a full characterization of the differences between AM and more conventional wrought and cast processes. For this study, sixteen different commercially available superalloy 718 powder feedstocks were obtained, built using laser powder bed fusion(L-PBF), and microstructurally and mechanically analyzed. These measurements revealed a wide range of build qualities and microstructures despite all powder lots falling within the 718chemical specification and being processed using the same prescribed build and heat treatment parameters. Statistical analysis found a strong correlation of the amount of carbon in the powder with the final grain size and strength of the heat-treated 718 part. Ultimately, this study highlights the need of a refined superalloy 718 chemical specification for powder lots to be used in AM.

Timothy M Smith↗

Laser Materials Processing for NASA's Aerospace Structural Materials

Lasers are useful for performing operations such as joining, machining, built-up freeform fabrication, and surface treatment. Due to the multifunctional nature of a single tool and the variety of materials that can be processed, these attributes are attractive in order to support long-term missions in space. However, current laser technology also has drawbacks for space-based applications. Specifically, size, power efficiency, lack of robustness, and problems processing highly reflective materials are all concerns. With the advent of recent breakthroughs in solidstate laser (e.g., diode-pumped lasers) and fiber optic technologies, the potential to perform multiple processing techniques in space has increased significantly. A review of the historical development of lasers from their infancy to the present will be used to show how these issues may be addressed. The review will also indicate where further development is necessary to realize a laser-based materials processing capability in space. The broad utility of laser beams in synthesizing various classes of engineering materials will be illustrated using state-of-the art processing maps for select lightweight alloys typically found on spacecraft. Both short- and long-term space missions will benefit from the development of a universal laser-based tool with low power consumption, improved process flexibility, compactness (e.g., miniaturization), robustness, and automation for maximum utility with a minimum of human interaction. The potential advantages of using lasers with suitable wavelength and beam properties for future space missions to the moon, Mars and beyond will be discussed. The laser processing experiments in the present report were performed using a diode pumped, pulsed/continuous wave Nd:YAG laser (50 W max average laser power), with a 1064 nm wavelength. The processed materials included Ti-6AI-4V, Al-2219 and Al-2090. For Phase I of this project, the laser process conditions were varied and optimized to see the effects on melt-quenching, cladding/alloying (using the pre-placed powder technique), and cutting. Key parameters such laser power, pulse repetition frequency, process speed, and shield gas flow and the observed process characteristics such as plasma formation during laser/material interaction, have been reported for all experimental runs. Preliminary materials characterization of select samples was carried out using various microscopy, diffraction, spectroscopy and microhardness test methods, and reported. Select nitridation results of Ti-6AI-4V using nitrogen assist gas indicated the successful formation of hard titanium nitrides with much higher hardness (2180 kg/sq mm). A cost-effective and simple powder delivery system has been successfully fabricated for the further experimentation in Phase H.

Nagarathnam, Karthik↗

High-Pressure Characterization of Two Stereoisomers of Tetranitroester Cyclobutane

The high-pressure behavior of two stereoisomeric cyclobutane nitric ester materials were studied at room temperature to near 25 GPa via Raman spectroscopy and powder X-ray diffraction. The materials investigated included [cis-trans-cis]- and [all-cis]-tetranitrate ester cyclobutanes. Over the course of these studies no evidence of polymorphism was observed, highlighting the stability of the ambient pressure crystal structures of the cyclobutanes to conditions near the detonation pressure of the material. Differences were observed between the bulk moduli of the two stereoisomers, suggesting potential tunability in materials response under dynamic conditions through the use of isomeric materials. Finally, such findings suggest that these high-performance materials can serve as TNT replacement in novel melt-castable energetic formulations without the concern of uncontrolled polymorphism that might otherwise affect the performance and safety of a munition.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

Fabrication and characterization of net-shaped iron nitride-amine-epoxy soft magnetic composites

Soft magnetic composites (SMCs) offer a promising alternative to electrical steels and soft ferrites in high performance motors and power electronics. They are ideal for incorporation into passive electronic components such as inductors and transformers, which require a non-permanent magnetic core to rapidly switch magnetization. As a result, there is a need for materials with the right combination of low coercivity, low magnetic remanence, high relative permeability, and high saturation magnetization to achieve these goals. Iron nitride is an attractive soft magnetic material for incorporation into an amine/epoxy resin matrix. This permits the synthesis of net-shaped SMCs using a “bottom-up” approach for overcoming the limitations of current state-of-the-art SMCs made via conventional powder metal processing techniques. In this work we present the fabrication of various net-shaped, iron nitride-based SMCs using two different amine/epoxy resin systems and their magnetic characterization. The maximum volume loading of iron nitride reached was ~77% via hot pressing, which produced SMCs with a saturation magnetic polarization (J s ) of ~0.9 T, roughly 2–3 times the J s of soft ferrites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Predicting Selective Laser Printing Print Quality of Polymer Powders through Melt Flow Index

Selective Laser Sintering (SLS) uses a precisely controlled laser to fuse polymer powder to build complex 3D shapes. While SLS covers a wide application space, the processing knowledge of polymer powder is limited, restricting the number of commercial powders available. This study serves to expand the processing knowledge of polypropylene and polyethylene in parallel with a “mature” SLS feedstock, nylon, through melt flow index (MFI) characterization. Differential Scanning Calorimetry (DSC) was used to explore the sintering window of the polymers. Polyethylene and polypropylene exhibited a relatively narrow sintering window between 4 – 5 °C, whereas the sintering window of nylon was much wider, between 23 – 24 °C. This suggests that the print quality between polyethylene and polypropylene would be similar; however, X-ray computed tomography revealed a higher volume of print defects, voids, and de lamination in polyethylene than in polypropylene. MFI analysis provided additional insight into the difference in print quality, as the MFI of polyethylene was 7.16 g/10 min, 9.95 g/10 min for polypropylene, and 17.23 g/10 min for nylon. MFI is inversely correlated to melt viscosity, and a low melt viscosity is desired for proper coalescing between the layers and particles. These results suggest that MFI is a promising tool, in conjunction with traditional thermal analysis, for screening candidate powder feedstocks for SLS and optimization of print parameters for novel powders.

36 MATERIALS SCIENCE↗

Characterization of aluminum/RP-1 gel propellant properties

Research efforts are being conducted by the NASA Lewis Research Center to formulate and characterize the properties of Al/RP-1 and RP-1 gelled propellants for rocket propulsion systems. Twenty four different compositions of gelled fuels were formulated with 5 and 16 micron, atomized aluminum powder in RP-1. The total solids concentration in the propellant varied from 5 to 60 wt percent. Tests were conducted to evaluate the stability and rheological characteristics of the fuels. Physical separation of the solids occurred in fuels with less than 50 wt percent solids concentration. The rheological characteristics of the Al/RP-1 fuels varied with solids concentration. Both thixotropic and rheopectic gel behavior were observed. The unmetallized RP-1 gels, which were formulated by a different technique than the Al/RP-1 gels, were highly viscoelastic. A history of research efforts which were conducted to formulate and characterize the properties of metallized propellants for various applications is also given.

Rapp, Douglas C.↗

Characterization of aluminum/RP-1 gel propellant properties

Research efforts are being conducted by the NASA Lewis Research Center to formulate and characterize the properties of Al/RP-1 and RP-1 gelled propellants for rocket propulsion systems. Twenty four different compositions of gelled fuels were formualted with 5 and 16 micron, atomized aluminum powder in RP-1. The total solids concentration in the propellant varied from 5 to 60 wt percent. Tests were conducted to evaluate the stability and rheological characteristics of the fuels. Physical separation of the solids occurred in fuels with less than 50 wt percent solids concentration. The rheological characteristics of the Al/RP-1 fuels varied with solids concentration. Both thixotropic and rheopectic gel behavior were observed. The unmetallized RP-1 gels, which were formulated by a different technique than the Al/RP-1 gels, were highly viscoelastic. A history of research efforts which were conducted to formulate and characterize the properties of metallized propellants for various applications is also given.

Rapp, Douglas C.↗

Evaluation of HCF strength of Alloy 625 with non-optimum additive manufacturing process parameters

An extensive experimental program was undertaken to generate the process-structure-HCF property data for additive-manufactured Alloy 625. Round tensile and flat dog-bone HCF specimens were fabricated using a laser powder bed fusion process. Several builds were fabricated with different processing parameters. The fatigue strengths were determined using a step-test method and fracture surfaces were characterized to identify the critical microstructure feature associated with the formation of the fatigue crack. Finally, a fracture mechanics-based methodology using fatigue crack growth data measured on a wrought alloy is shown to provide conservative estimates of the HCF lives for the additive-manufactured alloy.

36 MATERIALS SCIENCE↗

Laser-based ultrasound interrogation of surface and sub-surface features in advanced manufacturing materials

Abstract Structures formed by advanced manufacturing methods increasingly require nondestructive characterization to enable efficient fabrication and to ensure performance targets are met. This is especially important for aerospace, military, and high precision applications. Surface acoustic waves (SAW) generated by laser-based ultrasound can detect surface and sub-surface defects relevant for a broad range of advanced manufacturing processes, including laser powder bed fusion (LPBF). In particular, an all-optical SAW generation and detection configuration can effectively interrogate laser melt lines. Here we report on scattered acoustic energy from melt lines, voids, and surface features. Sub-surface voids are also characterized using X-ray Computed Tomography (CT). High resolution CT results are presented and compared with SAW measurements. Finite difference simulations inform experimental measurements and analysis.

36 MATERIALS SCIENCE↗