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At least 19 records

Powder Characterization Inter-Comparison

We performed qualitative and quantitative image analysis on SEM images for 5 uranium samples. Qualitative assessment was completed using the lexicon of Tamasi et al. 2017 on a subset of images from each sample to provide an overall morphological profile of each material. Quantitative analysis of the particles was done using the Morphological Analysis for Materials Attribution, or MAMA, software. We performed particle analysis primarily on samples labeled U Mo, U Si, and UO 2 . Samples labeled ADU and DU Ox were not prioritized for quantitative analysis due to staffing and time it took to segment these images. Two lab analysts worked on this effort, one focusing on the qualitative assessment and the other focusing on the quantitative assessment.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructural Characterization of Laser Powder Bed Fusion (L-PBF) Additively Manufactured Inconel 718 for Aerospace Application

Alloy 718 (Inconel 718) is used for aerospace applications because of its excellent corrosion resistance and mechanical properties. This alloy is particularly applicable in manufacturing components subjected to high temperatures in rocket engines, aero-engines, and gas turbines. Properties for this alloy when processing on systems from similar and different Laser Powder Bed Fusion (L-PBF) machines provide subtle differences due to process parameters, feedstock, and machine configurations. A series of sixteen L-PBF AM Inconel 718 geometric feature build plates have been evaluated for microstructure using optical microscopy. This study presents the details of the microstructure analysis concerning geometry and different machine platforms. Microstructural investigations of these samples included average grain width measurement for all the X-Y and Y-Z build layers and are accompanied by process parameters and powder characterization. The present work concludes with a discussion on the importance of captured differences among builds to understand the practical limitations among AM platforms.

Additive Manufacturing↗

Iridium Atoms Bonded to Crystalline Powder MgO: Characterization by Imaging and Spectroscopy

Samples with low loadings of metals on well-defined supports provide some of the best opportunities to determine the metal–support structure and bonding. We illustrate methods for characterizing atomically dispersed heavy metals on metal oxide supports by aberration-corrected scanning transmission electron microscopy (STEM) complemented by fluorescence detection extended X-ray absorption fine structure and infrared spectroscopies. STEM images of Ir atoms derived from Ir(C 2 H 4 ) 2 (acac) (acac = acetylacetonato) on high-surface-area MgO powder were obtained with minimized electron beam damage by quickly recording images near where the focus had been established. The images show that iridium at a loading of 1.0 wt % on MgO calcined at 1073 K was atomically dispersed, populating much of the surface of the MgO particles, which had irregular shapes—consequently the Ir atoms were bonded at various sites to two or three surface O atoms. In contrast, MgO calcined at 1273 K consisted of almost perfectly cubic crystals, and Ir atoms at a loading of only 0.01 wt % on this nearly ideal support were anchored preferentially at edges and corners of the (100) faces and bonded to three surface O atoms. The latter results indicate a path forward for the determination of precise structures of atomically dispersed metals on crystalline metal oxide supports.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Standardization Gaps in Powder Feedstock Characterization and Establishing Acceptability for Reuse in Additive Manufacturing

Characterization techniques for powder feedstocks used in additive manufacturing (AM) have long been relied upon to describe the inputs to an AM workflow. However, functional gaps remain between tests to measure intrinsic and extrinsic properties with the direct performance within AM equipment. Furthermore, the common practice of reusing powder through multiple build cycles introduces effects and changes to feedstock performance that are otherwise difficult to measure quantitatively. Here, standardization and the development of new test methods have not kept pace with the rapid evolution of the AM industry and its reliance on highly coupled process-structure–property-performance relationships.

Characterization and Analytical Technique↗

An instrument for in situ characterization of powder spreading dynamics in powder-bed-based additive manufacturing processes

In powder-bed-based metal additive manufacturing (AM), the visualization and analysis of the powder spreading process are critical for understanding the powder spreading dynamics and mechanisms. Unfortunately, the high spreading speeds, the small size of the powder, and the opacity of the materials present a great challenge for directly observing the powder spreading behavior. In this study, we report a compact and flexible powder spreading system for in situ characterization of the dynamics of the powders during the spreading process by high-speed x-ray imaging. The system enables the tracing of individual powder movement within the narrow gap between the recoater and the substrate at variable spreading speeds from 17 to 322 mm/s. The instrument and method reported here provide a powerful tool for studying powder spreading physics in AM processes and for investigating the physics of granular material flow behavior in a confined environment.

47 OTHER INSTRUMENTATION↗

Ceramics in gas turbines - Powder and process characterization

The role of powder and process characterization in producing high quality silicon nitride and silicon carbide components, for gas turbine applications, is described. Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability have been pointed out. The essential features/parameters to characterize a batch of powder have been discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. It is inevitable that significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

Dutta, S.↗

Additive Manufacturing: Assessing Metal Powder Quality Through Characterizing Feedstock and Contaminants

The quality of powder feedstock for additive manufacturing (AM) metal powder bed fusion methods can significantly affect the quality of parts built from it. Particle size distribution (PSD) and shape factors influence flowability as well as the thickness and uniformity of each powder layer in the build box. For high-performance applications such as aerospace, medical, power generation and military, it becomes important to identify critical additional factors: the types, numbers and sizes of particulate contaminants that may be present in the powder. This is true for virgin, used and blended powders. Contaminants may be introduced during powder manufacture (e.g., ceramic insulation fragments from gas atomization equipment), handling (building insulation, talc) or possibly during the build process itself. Contaminants contained within a batch of powder can be physically built into an additive part when they are incorporated into the melt pool, and they can remain as discrete particulates or non-fused interfaces that act as stress concentrators. Their presence may decrease fatigue life by increasing the likelihood of fatigue crack initiation. This article describes three methods to rapidly and quantifiably characterize powder feedstock. (1) Computer-controlled scanning electron microscopy (CCSEM) provides quantitative size and shape parameters, as well as fine surface details from individual images on a particle-by-particle basis in large populations of powder. (2) Energy-dispersive spectroscopy (EDS) can be included, providing insights into variations within a batch of powder, as well as contaminant compositions. (3) For critical applications, the heavy liquid separation (HLS) method physically extracts low-density contaminants from a sample of powder metal down to part-per-billion detection limits to allow direct examination of contaminants and enhance identification and prevention of their sources. Altogether, these methods permit direct comparisons among powder metal samples. Better quantification of powder characteristics aids determination of suitability for end uses.

36 MATERIALS SCIENCE↗

Detector Characterization for Quantitative Spectral Radiography of Uranium Powder Samples

Pacific Northwest National Laboratory (PNNL) is developing a prototype spectral x-ray radiography (SpecX) non-destructive assay system for noninvasive material mass quantification of uranium-bearing powders. The SpecX system uses a custom material estimation algorithm, which requires a high-fidelity pixel-by-pixel detector response model for accurate quantification. We performed a detailed characterization and built a model of a High-Energy X-ray Imaging Technology (HEXITEC) CdTe pixelated spectral detector. Here we present the detector characterization which led to that model, including a determination of the pixel-wise energy calibration, the detection efficiency, the detector uniformity, the detector stability, and a comparison of methods to remove charge-shared events.

spectral X-ray radiography, pixelated detector, ca↗

Development and characterization of Powder Metallurgy (PM) 2XXX series Al alloy products and Metal Matrix Composite (MMC) 2XXX Al/SiC materials for high temperature aircraft structural applications

The results of a series of material studies performed by the Lockheed Aeronautical Systems Company over the time period from 1980 to 1991 are discussed. The technical objective of these evaluations was to develop and characterize advanced aluminum alloy materials with temperature capabilities extending to 350 F. An overview is given of the first five alloy development efforts under this contract. Prior work conducted during the first five modifications of the alloy development program are listed. Recent developments based on the addition of high Zr levels to an optimum Al-Cu-Mg alloy composition by powder metallurgy processing are discussed. Both reinforced and SiC or B4C ceramic reinforced alloys were explored to achieve specific target goals for high temperature aluminum alloy applications.

Chellman, D. J.↗

Ceramics in gas turbine: Powder and process characterization

Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability are pointed out. The essential features/parameters to characterize a batch of powder are discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. Significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

Dutta, S.↗

Ceramic Inclusions In Powder Metallurgy Disk Alloys: Characterization and Modeling

Powder metallurgy alloys are increasingly used in gas turbine engines, especially as the material chosen for turbine disks. Although powder metallurgy materials have many advantages over conventionally cast and wrought alloys (higher strength, higher temperature capability, etc.), they suffer from the rare occurrence of ceramic defects (inclusions) that arise from the powder atomization process. These inclusions can have potentially large detrimental effect on the durability of individual components. An inclusion in a high stress location can act as a site for premature crack initiation and thereby considerably reduce the fatigue life. Because these inclusions are exceedingly rare, they usually don't reveal themselves in the process of characterizing the material for a particular application (the cumulative volume of the test bars in a fatigue life characterization is typically on the order of a single actual component). Ceramic inclusions have, however, been found to be the root cause of a number of catastrophic engine failures. To investigate the effect of these inclusions in detail, we have undertaken a study where a known population of ceramic particles, whose composition and morphology are designed to mimic the 'natural' inclusions, are added to the precursor powder. Surface connected inclusions have been found to have a particularly large detrimental effect on fatigue life, therefore the volume of ceramic 'seeds' added is calculated to ensure that a minimum number will occur on the surface of the fatigue test bars. Because the ceramic inclusions are irregularly shaped and have a tendency to break up in the process of extrusion and forging, a method of calculating the probability of occurrence and expected intercepted surface and embedded cross-sectional areas were needed. We have developed a Monte Carlo simulation to determine the distributions of these parameters and have verified the simulated results with observations of ceramic inclusions found in macro slices from extrusions and forgings. The ultimate goal of this study will be to use probabilistic methods to determine the reliability detriment that can be attributed to these ceramic inclusions.

Bonacuse, Pete↗

Ceramic Inclusions in Powder Metallurgy Disk Alloys: Characterization and Modeling

Powder metallurgy alloys are increasingly used in gas turbine engines, especially in turbine disk applications. Although powder metallurgy materials have many advantages over conventionally cast and wrought alloys (higher strength, higher temperature capability, etc.), they suffer from the rare occurrence of ceramic defects (inclusions) that are inherent to the powder atomization process. These inclusions can have a potentially large detrimental effect on the durability of individual components. An inclusion in a high stress location can act as a site for premature crack initiation and thereby considerably reduce the fatigue life. Because these inclusions are exceedingly rare, they typically do not reveal themselves in the process of characterizing the material for a particular application (the cumulative volume of the test bars in a fatigue life characterization is typically on the order of a single actual component). Ceramic inclusions have, however, been found to be the root cause of a number of catastrophic engine failures. To investigate the effect of these inclusions in detail, we have undertaken a study where known populations of ceramic particles, whose composition and morphology are designed to mimic the "natural" inclusions, are added to the precursor powder. Surface-connected inclusions have been found to have a particularly large detrimental effect on fatigue life; therefore, the quantity of ceramic "seeds" added is calculated to ensure that a minimum number will intersect the surface of the fatigue test bars. Because the ceramic inclusions are irregularly shaped and have a tendency to break up in the process of extrusion and forging, a method of calculating the probability of occurrence and expected intercepted surface area was needed. We have developed a Monte Carlo simulation to determine the distributions of these parameters and have verified the simulated results with observations of ceramic inclusions found in macroscopic slices from extrusions and forgings. Fatigue specimens have been machined from Udimet 720 (a powder metallurgy superalloy) forgings, to determine the effects of the inclusions on fatigue life. The ultimate goal of this study will be to use probabilistic methods to determine the reliability detriment that can be attributed to these ceramic inclusions. This work has been supported by the Ultra Safe and Ultra- Efficient Engine Technologies programs.

Bonacuse, Peter J.↗

Stability of Solid Uranyl Peroxides under Irradiation

The effects of radiation on a variety of uranyl peroxide compounds were examined using γ-rays and 5 MeV He ions, the latter to simulate α-particles. The studied materials were studtite, [(UO 2 )(O 2 )(H 2 O)2](H 2 O) 2 , the salt of the U 60 uranyl peroxide cage cluster, Li 44 K 16 [(UO 2 )(O 2 )(OH)] 60 ·255H 2 O, the salt of U 60 Ox 30 uranyl peroxide oxalate cage cluster, Li 12 K 48 [{(UO 2 )(O 2 )} 60 (C 2 O 4 ) 30 ]·$n$H 2 O, and the salt of the U 24 Pp 12 (Pp = pyrophosphate) uranyl peroxide pyrophosphate cage cluster, Li 24 Na 24 [(UO 2 ) 24 (O 2 ) 24 (P2O7)12]·120H 2 O. Irradiated powders were characterized using powder X-ray diffraction, Raman spectroscopy, infrared spectroscopy, X-ray photoelectron spectroscopy, and UV–vis spectroscopy. A weakening of the uranyl bonds of U60 was found while studtite, U 60 Ox 30 , and U 24 Pp 12 were relatively stable to $γ$-irradiation. Studtite and U 60 are the most affected by α-irradiation forming an amorphous uranyl peroxide as characterized by Raman spectroscopy and powder X-ray diffraction while U 60 Ox 30 and U 24 Pp 12 show minor signs of the formation of an amorphous uranyl peroxide.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Discerning the Impact of Powder Feedstock Variability on Structure, Property, and Performance of Selective Laser Melted Alloy 718: A Principal Component Analysis (PCA) of Feedstock Variability

Extensive mechanical, chemical and microstructural analyses were conducted on additively manufactured Alloy 718 to characterize powders from multiple vendors to determine the effects of variations observed in the powders had on the consolidated material. With over 190 variables examined, it was necessary to reduce the number of variables and identify the variables and classes of variables that had the greatest effect. Principle Component Analysis (PCA) was used to reduce the number of variable to effectively 12 while identifying several classes of variables as most important.

Ellis, David↗

Metal Powder Recyclability in Binder Jet Additive Manufacturing

The recyclability of 316L stainless steel powder in the binder jetting process has been determined. The powder characterization results demonstrated a 22% increase in the number of coarse particles (> 30 µm) and an 18.2% reduction in the number of small particles (< 10 µm) after recycling up to 16 times. A few elongated and irregular-shaped particles were found after recycling, possibly due to particle agglomeration during handling and sieving. Here, a negligible increase in the oxygen content by 0.036% was detected in the recycled powder. The density of sintered parts produced using recycled powder was approximately 1.5% lower than when using fresh powder due to the changes in the particle size distribution and the flowability of the powder caused by the changes in morphology. Final parts built using fresh and recycled powder showed similar hardness (155 ± 3 HV and 165 ± 9 HV) and yield strength (206 ± 16 MPa and 192 ± 10 MPa), respectively.

36 MATERIALS SCIENCE↗

Evolution of AISI 304L stainless steel part properties due to powder recycling in laser powder-bed fusion

Selective laser melting (SLM) is a powder-bed fusion process in Additive Manufacturing (AM) that uses a laser beam to selectively fuse layers of powder into near net-shape components with little porosity. However, inconsistencies in the part properties due to the presence of defects in as-built components has hindered the widespread adoption of SLM for industrial applications forcing researchers to study the sources of variation for quality control purposes. A critical area suspected of creating variation in the part properties is the feedstock, where batch-to-batch differences as well as changes in the powder properties with reuse have the potential to affect performance. During processing, laser spatter and condensate eject from the melt pool and deposit into the powder-bed surrounding the parts. These particulates, more commonly known as ejecta, differ morphologically and chemically from the virgin powder compromising its reusability. In this study, 304L stainless steel powder was recycled for a total of 5 times through a systematic approach aimed at accelerating powder degradation to reveal the influence on both the tensile and impact toughness properties. Through analysis of variance (ANOVA), it was found that tensile properties did not change with reuse, while the impact toughness showed a steady decline illustrating the differences in static and dynamic part properties due to powder recycling.

36 MATERIALS SCIENCE↗

Directed energy deposition of functionally graded V-4Cr-4Ti to Fe-9Cr transition for fusion power systems

This study proposes a graded structure via additive manufacturing for divertor and first wall blanket applications in fusion reactors. Materials were selected based on thermodynamic calculations to operate from 1100 °C at the plasma-facing level to 550 °C at the structural steel level. Conventional joining methods often lead to failures due to discrete reaction layers with significant mechanical property differences. Using laser beam-directed energy deposition (LB-DED), this study demonstrates the fabrication of a VCrTi-Gr91 steel functionally graded component through a novel process parameter optimization framework. A systematic approach included powder characterization, single-track depositions, and construction of printability maps. Near full-density specimens of each interlayer were additively manufactured, and a transition from V-based alloys to reduced activation ferritic martensitic steels was achieved. Computational material selection of interlayer alloys and thermodynamic/diffusion kinetics simulations prevented most interface incompatibilities. A brittle intermetallic formed at one interface, causing cracking, which was not predicted by current thermodynamic models. Transition alloy design approach was updated with a more recent database and a mitigation strategy has been proposed to eliminate the formation of deleterious intermetallic phases. Ultimately, LB-DED has proven effective for producing multi-material graded systems for fusion applications, with the demonstrated process parameter optimization framework applicable to various materials.

Additive manufacturing↗

A Blind Test of Hapke's Photometric Model

Hapke's bidirectional reflectance equation is a versatile analytical tool for predicting (i.e. forward modeling) the photometric behavior of a particulate surface from the observed optical and structural properties of its constituents. Remote sensing applications of Hapke s model, however, generally seek to predict the optical and structural properties of particulate soil constituents from the observed photometric behavior of a planetary surface (i.e. inverse-modeling). Our confidence in the latter approach can be established only if we ruthlessly test and optimize it. Here, we summarize preliminary results from a blind-test of the Hapke model using laboratory measurements obtained with the Bloomsburg University Goniometer (B.U.G.). The first author selected eleven well-characterized powder samples and measured the spectrophotometric behavior of each. A subset of twenty undisclosed examples of the photometric measurement sets were sent to the second author who fit the data using the Hapke model and attempted to interpret their optical and mechanical properties from photometry alone.

Helfenstein, P.↗