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At least 667 records · Page 37

Advances in Non-contact Measurement of Creep Properties

Our team has developed a novel approach to measuring creep at extremely high temperatures using electrostatic levitation (ESL). This method has been demonstrated on niobium up to 2300 C, while ESL has melted tungsten (3400 C). High-precision machined spheres of the sample are levitated in the NASA MSFC ESL, a national user facility, and heated with a laser. The laser is aligned off-center so that the absorbed photons transfer their momentum to the sample, causing it to rotate at up to 250,000+ RPM. The rapid rotation loads the sample through centripetal acceleration, causing it to deform. The deformation of the sample is captured on high-speed video, which is analyzed by machine-vision software from the University of Massachusetts. The deformations are compared to finite element models to determine the constitutive constants in the creep relation. Furthermore, the noncontact method exploits stress gradients within the sample to determine the stress exponent in a single test. This method was validated in collaboration with the University of Tennessee for niobium at 1985 C, with agreement within the uncertainty of the conventional measurements. A similar method is being employed on Ultra-High-Temperature ZrB2- SiC composites, which may see application in rocket nozzles and sharp leading edges for hypersonic vehicles.

Hyers, Robert W.↗

Calcium-Magnesium-Aluminosilicate (CMAS) Infiltration and Cyclic Degradations of Thermal and Environmental Barrier Coatings in Thermal Gradients

In a continuing effort to develop higher temperature capable turbine thermal barrier and environmental barrier coating systems, Calcium-Magnesium-Aluminosilicate (CMAS) resistance of the advanced coating systems needs to be evaluated and improved. This paper highlights some of NASA past high heat flux testing approaches for turbine thermal and environmental barrier coatings assessments in CMAS environments. One of our current emphases has been focused on the thermal barrier - environmental barrier coating composition and testing developments. The effort has included the CMAS infiltrations in high temperature and high heat flux turbine engine like conditions using advanced laser high heat flux rigs, and subsequently degradation studies in laser heat flux thermal gradient cyclic and isothermal furnace cyclic testing conditions. These heat flux CMAS infiltration and related coating durability testing are essential where appropriate CMAS melting, infiltration and coating-substrate temperature exposure temperature controls can be achieved, thus helping quantify the CMAS-coating interaction and degradation mechanisms. The CMAS work is also playing a critical role in advanced coating developments, by developing laboratory coating durability assessment methodologies in simulated turbine engine conditions and helping establish CMAS test standards in laboratory environments.

Thermal Barrier Coatings↗

Time-Variable Gravity from Satellite-Laser-Ranging and Doppler Measurements: An Update on the Low-degree components as well as the connections with Geophysical/Climatic Processes

The oblateness of the Earth's gravity field, 52, has long been observed to undergo a slight decrease due to post-glacial rebound of the mantle. Sometime around 1998 this trend reversed quite suddenly. This reversal persisted until 2001, at which point the atmosphere-corrected time series appears to have reversed yet again. Presently, the time series appears to be returning to the value that would nominally have been reached had the anomaly not occurred. This anomaly signifies a large interannual change in global mass distribution whose J2 effect overshadows that of the post-glacial rebound over such timescales. A number of possible causes have been considered, with oceanic mass redistribution as the leading candidate although other effects, such as glacial melting and core effects may be contributing. The amount by which J2 returns to it's nominal value provides a valuable constraint on the separation of the causes, and will be considered. We will present our latest Satellite Laser Ranging and DORIS Doppler derived time series for J2, and various other low-degree harmonic terms, as well as our investigations into the causes. In addition, we will show the comparison of the J2 results with those derived from CHAMP, as computed at NASA GSFC, and the recently released GRACE gravity model.

Cox, Christopher M.↗

InGaAsP/InP laser development for single-mode, high-data-rate communications

Materials studies as well as general and specific device development were carried out in the InGaAsP system. A comparison was made of three standard methods of evaluating substrate quality by means of dislocation studies. A cause of reduced yield of good wafers, the pullover of melt from one bin to the next, has been analyzed. Difficulties with reproducible zinc acceptor doping have been traced to segregation of zinc in the In/Zn alloy used for the doping source. Using EBIC measurments, the pn junction was shown to drift in location depending on factors not always under control. An analysis of contact structures by SIMS showed that the depth to which the sintered Au/Zn contact penetrates into the structure is typically 0.13 microns, or well within the cap layer and out of the p-type cladding and thus not deleterious to laser prformance. The problem of single-mode laser development was investigated and it was shown to be related to the growth habit over four different possible substrate configurations. The fabrication of constricted double heterojunctions, mesa stripe buried heterostructures, and buried heterostructures was discussed, and measurements were presented on the device properties of single-mode buried heterostructure lasers. Results include single spectral line emission at 3 mW and a threshold current of 60 mA.

Ladany, I.↗

Boron coordination change in barium borate melts and glasses and its contribution to configurational heat capacity, entropy, and fragility

High-energy x-ray diffraction from molten and glassy BaB 2 O 4 and BaB 4 O 7 has been performed using aerodynamic levitation and laser heating over a wide range of temperatures. Remarkably, even in the presence of a heavy metal modifier dominating x-ray scattering, it was possible to extract accurate values for the tetrahedral, sp 3 , boron fraction, N 4 , which declines with increasing temperature, using bond valence-based mapping from the measured mean B–O bond lengths while accounting for vibrational thermal expansion. These are used within a boron-coordination-change model to extract enthalpies, ΔH, and entropies, ΔS, of isomerization between sp 2 and sp 3 boron. The results for BaB 4 O 7 , ΔH = 22(3) kJ mol -1 boron, ΔS = 19(2) J mol -1 boron K -1 , agree quantitatively with those found previously for Na 2 B 4 O 7 . Analytical expressions for N 4 (J, T) and associated configurational heat capacity, $C_{P}^{conf}$(J, T), and entropy, S conf (J, T), contributions are extended to cover a wide composition range 0 ≤ J = BaO/B 2 O 3 ≤ 3 using a model for ΔH(J) and ΔS(J) derived empirically for lithium borates. Maxima in the $C_{P}^{conf}$(J, T g ) and fragility index contributions are thereby predicted for J ≲ 1, higher than the maximum observed and predicted in N 4 (J, T g ) at J ≃ 0.6. We discuss the utility of the boron-coordination-change isomerization model in the context of borate liquids containing other modifiers and the prospect of neutron diffraction to aid in empirical determinations of modifier-dependent effects, illustrated by new neutron diffraction data on Ba 11 B 4 O 7 glass, its well-known α-polymorph, and lesser-known δ-phase.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Optically and thermally driven huge lattice orbital and spin angular momenta from spinning fullerenes

Lattice vibration in solids may carry angular momentum. But unlike the intrinsic spin of electrons, the lattice vibration is rarely rotational. To induce angular momentum, one needs to find a material that can accommodate a twisted normal mode, two orthogonal modes, or excitation of magnons. If excitation is too strong, one may exceed the Lindemann limit, so the material melts. Therefore these methods are not ideal. Here, we theoretically propose a route to phonon angular momentum in a molecular crystal C 60 . We find that a single laser pulse is able to inject a significant amount of angular momentum to C 60 , and the momentum transfer is helicity dependent. Changing from right-circularly polarized light to left-circularly polarized light switches the direction of phonon angular momentum. On the ultrafast timescale, the orbital angular momentum change closely resembles the displacive excitation of coherent phonons, with a cosine-function dependence on time, different from the spin counterpart. Atomic displacements, even under strong laser excitation, remain far below the Lindemann criterion. Under thermal excitation, spinning C 60 even at room temperature generates a huge angular momentum close to several hundred h¯. Our finding opens the door to a large group of fullerenes, from C 60 , C 70 to their endohedral derivatives, where angular momentum can be generated through light or temperature. Furthermore, this paves the way to the phononic control electronic spin and harvesting thermal energy through phonon angular momentum.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Removing Contamination from Genesis Sapphire Collectors by Polishing

The Genesis Solar Wind Sample Re-turn Mission used a variety of materials as solar wind (SW) collectors. “Sapphire”, which is single crystal corundum, was ~6.7% of the collector material flown. But, a much higher percentage of Genesis sapphire collectors (SAP) survived the crash of the sample-return capsule as SAP is chemically inert, physically tough, and hard (MOHS 9, by definition). In fact, 39 sapphire fragments of bulk SW collector having areas ≥60 sq mm are available in JSC’s Genesis online catalog, whereas only 1 similarly sized silicon fragment is available (accessed 1/1/2020). In spite of the ease of accessing larger fragments, sapphire has not been popular among Genesis re-searchers because it is an electrical insulator (making SIMS more difficult) and its chemical inertness, high melting point and high hardness precludes the use of many mass-spectroscopic techniques. Recently, as alternative techniques for measuring Genesis samples are developed (e.g., synchrotron TXRF, INAA, laser ablation mass spectroscopy), more researchers are choosing to analyze sapphire. Thus, a number of researchers are actively studying how to best remove contamination from the Genesis sapphire surfaces. This report extends the task in Schmeling et al. that used polishing compounds to remove contamination from Genesis sapphire and focuses on contaminants (welded silicon, aluminum) that current chemical methods find recalcitrant.

M. Schmeling↗

Unveiling mechanisms and onset threshold of humping in high-speed laser welding

The fabrication of fuel cells relies on a rapid laser welding process. However, challenges arise with the occurrence of humping when the welding speed surpasses a critical threshold, which poses difficulties in achieving a smooth surface finish and a consistent weld strength. This study aims to elucidate the humping mechanisms by analyzing the morphology of molten pool and the characteristics of melt flow at varying welding speeds via in situ synchrotron high-speed X-ray imaging and computational fluid dynamics simulations. Our findings indicate that the short keyhole rear wall, the high backward melt velocity, and the prolonged tail of molten pool are the primary factors contributing to the onset of humping. Furthermore, a dimensionless humping index (π h ) was introduced, which successfully captured the onset threshold of humping across different literatures. This index not only provides a quantitative description of the humping formation tendency but also serves as a valuable tool for optimizing the laser welding process.

42 ENGINEERING↗

Correlation of SWIR imaging with LPBF 304L stainless steel part properties

In the Laser Powder Bed Fusion (LPBF) process, the local thermal history can vary significantly over a part as the heat transfer characteristics and the laser scan path are geometry dependent. The variations introduce the potential for defects that lead to part failure, some of which are difficult to identify non-destructively with common ex-situ evaluation techniques. These defects include significant microstructural and mechanical property differences in the part interiors. In this paper, thermal features are extracted from in-situ Short-Wave Infrared (SWIR) imaging measurements to compile voxel based part representations and understand how the complexities in the thermal history affect part performance. The deviations in thermal features due to different laser processing parameters and complex scan pathing are explored. Empirical correlations are developed to map thermal features with the engineering properties (bulk yield strength, area percentage porosity, and local state) of 304L stainless steel parts manufactured by LPBF. Processing modes (insufficient melting and keyholing) are determined by mapping part property measurements with multiple thermal features. Generating the relationships between thermographic measurements and resulting SLM part properties lays the foundation for in-situ part qualification.

36 MATERIALS SCIENCE↗

A laser powder bed fusion system for operando synchrotron x-ray imaging and correlative diagnostic experiments at the Stanford Synchrotron Radiation Lightsource

Laser powder bed fusion (LPBF) is a highly dynamic multi-physics process used for the additive manufacturing (AM) of metal components. Improving process understanding and validating predictive computational models require high-fidelity diagnostics capable of capturing data in challenging environments. Synchrotron x-ray techniques play a vital role in the validation process as they are the only in situ diagnostic capable of imaging sub-surface melt pool dynamics and microstructure evolution during LPBF-AM. In this article, a laboratory scale system designed to mimic LPBF process conditions while operating at a synchrotron facility is described. The system is implemented with process accurate atmospheric conditions, including an air knife for active vapor plume removal. Significantly, the chamber also incorporates a diagnostic sensor suite that monitors emitted optical, acoustic, and electronic signals during laser processing with coincident x-ray imaging. The addition of the sensor suite enables validation of these industrially compatible single point sensors by detecting pore formation and spatter events and directly correlating the events with changes in the detected signal. Experiments in the Ti–6Al–4V alloy performed at the Stanford Synchrotron Radiation Lightsource using the system are detailed with sufficient sampling rates to probe melt pool dynamics. X-ray imaging captures melt pool dynamics at frame rates of 20 kHz with a 2 µm pixel resolution, and the coincident diagnostic sensor data are recorded at 470 kHz. Furthermore, this work shows that the current system enables the in situ detection of defects during the LPBF process and permits direct correlation of diagnostic signatures at the exact time of defect formation.

36 MATERIALS SCIENCE↗

Effect of rare earth size on network structure and glass forming ability in binary aluminum garnets

Rare earth aluminate glasses are potentially useful for optical, luminescence, and laser applications. As reluctant glass formers, these materials exhibit unconventional atomic structures. To better understand how their structures correlate with glass formation, we investigate two rare earth aluminum garnet melts, La 3 Al 5 O 12 (LAG) and Yb 3 Al 5 O 12 (YbAG), which represent the relative extremes of good and poor glass forming ability in rare earth aluminates. Structural models have been refined to high-energy X-ray diffraction data over 1340–2740 K. Both melts contain mixtures of AlO 4 , AlO 5 , and AlO 6 polyhedra, with larger fractions of [5] Al and [6] Al in YbAG. Extrapolation of the Al–O coordination distributions to the glass transition match closely with 27 Al nuclear magnetic resonance measurements of (La 1−z Y z ) 3 Al 5 O 12 glasses, z = 0 to 1. During cooling, the mean coordination numbers increase for La–O in LAG from 6.45(8) to 6.98(8) and for Yb–O in YbAG from 6.02(8) to 6.21(8). Linkedness among Al–O polyhedra at ∼2450 K is mostly corner-sharing, with 9% edge-sharing in LAG and 19% in YbAG. Among [4] Al units, both melts have 6% edge-sharing that convert to all corner-sharing upon cooling. Network connectivity is compared using a newly defined metric, K n , that is similar to the Q n distribution but that accounts for the edge-sharing and triply bonded oxygen present in these melts. The lower glass forming ability in YbAG as compared to LAG correlates with more edge-sharing, associated with the larger fractions of [5] Al and [6] Al, and lower connectivity among [4] Al units.

Wilke, Stephen K. [Materials Development, Inc., Ar↗

3D Printing with Mixed Powders of Boron Carbide and Al Alloy

Laser additive manufacturing with mixed powders of boron carbide and aluminum alloy is investigated. Parameters such as laser power, scan speed, scan pattern, and hatching space are systematically evaluated and optimized to obtain the desired density and porosity. These results show that the AM part contains 20 wt% boron carbide and 80 wt% aluminum alloy, which are well mixed and synthesized during the melting process. Its mechanical properties are close to those of aluminum. A thin-wall structure based two dimensional and three dimensional radial collimators were fabricated with well-controlled geometry for neutron scattering measurement.

36 MATERIALS SCIENCE↗

Effects of shielding gas and spot reduction on humping suppression in high-speed laser welding

High-speed laser welding is a crucial process to enhance the production rate of fuel cell fabrication. However, exceeding a critical welding speed leads to defect formation such as humps and root concavities, which degrade weld quality and mechanical performance. This study employed shielding gas and spot reduction approaches to suppress these defects. The relationships between individual defect types and their influence on weld strength were systematically examined. Moreover, in situ high-speed synchrotron X-ray imaging was employed to comprehend the mechanisms of humping mitigation by shielding gas through analysis of instantaneous keyhole and melt pool dynamics. The observations reveal that shielding gas mitigates humping by shortening the molten pool through enhanced surface heat convection and by altering surface tension to prevent melt flow collisions. The effects of shielding gas and spot reduction were further incorporated into the dimensionless humping index (π h ) that describes the humping formation tendency. These findings provide mechanistic insights and quantitative guidance for defect control strategies in high-speed laser welding.

08 HYDROGEN↗

Micro-segregation phenomena and related spectroscopic signals in melt-grown β-Ga2O3 single crystals

One of the primary advantages of β-Ga2O3 over incumbent wide bandgap semiconductors is the ability to grow directly from the melt. Melt growth, using Czochralski or similar methods, results in impurities in the crystal which originate from the crucible, such as iridium and other transition metals like chromium. These impurities exhibit optoelectronic signatures useful for their identification and sensitive to the Fermi energy of a given crystal (i.e., signatures vary with the electrical conductivity of the matrix). In this work, we describe how laser Raman systems can be used to map and spatially correlate Cr3+ photoluminescence, electronic-coupled Raman scattering from Ir4+d–d internal transitions, and the Raman line attributed to hydrogenic shallow donors. Laser ablation inductively coupled plasma mass spectrometry directly measured spatially dependent relative metal concentrations and confirmed spectroscopic signals resulting from heterogeneities in impurity concentrations in β-Ga2O3 boules. Mapping of photoluminescence and Raman-related signatures is, thus, demonstrated as an effective and facile method for spatial measurement of chemical heterogeneities in both insulating and conductive melt-grown β-Ga2O3 crystals.

Dutton, Benjamin L. (ORCID:000000031272130X)↗

A novel sample-positioning system for microgravity application

This paper proposes a novel method for sample positioning in containerless processing at microgravity, using a system based on pulsed lasers. The method has two attributes. First, by generating beams that cancel out vectorially, the suspended material can be heated without being accelerated, a feature that can be used in melting and heat-treatment applications. Second, the specimen can be positioned within a fairly large work space. It is emphasized that this method can service a regime unfulfilled by the other levitation methods, such as electromagnetic levitation, active magnetic suspension, acoustic levitation, of electrostatic suspension.

Sridharan, G.↗

The Combined Strength of Thermodynamics and Comparative Planetology: Application of Activity Models to Core Formation in Terrestrial Bodies

Recent models for accretion of terrestrial bodies involve metal-silicate equilibrium as the metallic core formed during growth. Most elements considered are either refractory or well studied elements for which effects of pressure, temperature, oxygen fugacity, and metallic liquid composition are well known. There are a large number of elements that are both siderophile and volatile, whose fate in such models is unknown, largely due to a lack of data at comparable conditions and com-positions (FeNi core with light elements such as S, C, Si, and O). We have focused on Ge, In, As, Sb and determined the effect of Si and C on metal-silicate partitioning, and developed a thermo-dynamic model that allows application of these new data to a wide range of planetary bodies. New experiments: We have previously carried out experiments with FeSi metallic liquid at C-saturated conditions at 1600 and 1800 C [4]. In a new series of experiments we investigate the effect of Si in carbon-free systems at 1600 C for comparison. Experiments were carried out at 1 GPa in MgO capsules using the same basaltic starting composition as in previous studies. The MgO capsule reacts with the silicate melt to form more MgO-rich liquids that have 22-26 wt% MgO. Experimental met-als and silicates were analyzed using a combination of electron microprobe analysis and laser ablation ICP-MS. Results: The new results can be interpreted by considering Ge as an example, in the simple exchange equilibrium Fe + GeO = FeO + Ge, where the equilibrium constant Kd can be examined as a function of Si content of the metal. The slope of lnKd vs. (1-XSi) for this new series allows derivation of the epsilon interaction parameter for each of these four elements and Si (both C-saturated and C-free).All four elements have positive epsilon values, indicating that Si causes a decrease in the partition coefficients; values are 6.6, 6.5, 27.8 and 25.2 for In, Ge, As, and Sb, respectively, at 1 GPa and 1600 C. As an example of how large the effect of Si can be, these epsilon values correspond to activity coefficients (gamma) for As of 0.01 when XSi = 0, and up to gamma = 23 when XSi = 0.2. Combining these new results with previous determinations [5,6] of epsilon parameters for S and C for these elements allows us calculate activity of Ge, In, As, and Sb in Fe-Ni-Si-S-C-O metallic liquids. We apply this new model to sever-al terrestrial bodies such as Earth (Si-rich core), Mars (S-rich core), Moon (S-, C-, and Si-poor core), and Vesta, and examine the resulting core and mantle concentrations of these elements. Mantle concentrations of these four elements are well explained for Earth and Mars in models that call for mid-mantle equilibration between Si-bearing and S-bearing FeNi cores, respectively. Modeling results for the Moon and Vesta will also be presented.

Righter, K.↗

Chemically Tunable Aspect Ratio Control and Laser Refrigeration of Hexagonal Sodium Yttrium Fluoride Upconverting Materials

Hexagonal sodium yttrium fluoride with Na 3x Y 2-x F 6 stoichiometry (β-NaYF) is a promising material for luminescence upconversion applications due to the narrow crystal field splitting of the Yb(III) ion’s lower 2 F 7/2 manifold. However, growing single crystals of β-NaYF remains an outstanding challenge due to thermal expansion stresses that cause cracking during melt growth. Here, we demonstrate a novel hydrothermal synthesis of β-NaYF with the ability to tune the aspect ratio from microplatelets to microrods with aspect ratios that match computationally predicted cavity (Mie) resonances. These crystals have a root-mean-square roughness below 1 nm after calcination, which makes them ideal for optical cavities. The β-NaYF microcrystals are doped with 10% Yb(III) cations and are used to build optomechanical laser-refrigeration devices consisting of a hexagonal β-NaYF crystal located at the end of a cantilever. Laser refrigeration of these devices by >12.5 °C is observed using calibrated measurements of both the cantilever’s fundamental eigenfrequency and a Boltzmann fit to crystal field luminescence from the Yb(III) ions.

36 MATERIALS SCIENCE↗

Microstructural Development in Inconel 718 Nickel-Based Superalloy Additively Manufactured by Laser Powder Bed Fusion

Excellent weldability and high temperature stability make Inconel 718 (IN718) one of the most popular alloys to be produced by additive manufacturing. Here in this study, we investigated the effects of laser powder bed fusion (LPBF) parameters on the microstructure and relative density of IN718. The samples were fabricated with independently varied laser power (125 - 350W), laser scan speed (200 - 2200 mm/s), and laser scan rotation (0° - 90°). Archimedes’ method, optical microscopy, and scanning electron microscopy were employed to assess the influence of LPBF parameters on the relative density and microstructure. Optimal processing windows were identified for a wide range of processing parameters and relative density greater than 99.5% was achieved using volumetric energy density between 50 and 100 J/mm3. Microstructural features including melt pool geometry, lack of fusion defect, keyhole porosity, and sub-grain cellular microstructure were examined and quantified to correlate to LPBF parameters. A simple empirical model was postulated to relate relative sample density and LPBF volumetric energy density. Melt pool dimensions were quantitatively measured and compared to estimations based on Rosenthal solution, which yielded a good agreement with the width, but underestimated the depth, particularly at high energy input, due to lack of consideration for keyhole mode. In addition, the sub-grain cellular-dendritic microstructure in the as-built samples was observed to decrease with increasing laser scan speed. Quantification of the sub-micron cellular-dendritic microstructure yielded estimated cooling rate in the order of 10 5 – 10 7 K/s.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗