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5ω Optical Thomson Scattering Report

The 5ω Optical Thomson Scattering system on the National Ignition Facility (NIF) is a diagnostic designed to measure temporally and spatially resolved plasma conditions in Inertial Confinement Fusion (ICF) Hohlraums. The system was proposed in 2014 and a phased approach to implementation was developed. In phase one the collection system was designed, built, and fielded on the NIF to be used for 3ω Thomson scattering measurements and background measurements near 211 nm (5ω. The initial commissioning experiment for the collection system was completed in Oct. 2016. Commissioning of the collection system continued through 2017 and the system is now fielded for a range of user experiments and regularly produces publication quality data. A dedicated 5ω probe laser was designed and built to allow Thomson scattering measurements in the presence of 2 MJ of 3ω drive energy. Due to scattered light (spectral reflections, laser-plasma instabilities, and unconverted drive energy) from the 3w drive lasers typical wavelengths (2ω and 4ω) fielded at other laser facilities like the Nova Laser Facility and the Omega Laser Facility were unable to meeting the signal to background requirements in design studies. A 10 Joule 5ω probe was proposed as a solution that met requirements. This 10 Joule laser was more energetic than previously fielded 5w lasers by 2-3 orders of magnitude. As part of a risk reduction plan, phase two of the project was to develop a 1 Joule, 5ω laser to demonstrate conversion efficiency >20% from 1ω to 5ω and make initial Thomson scattering measurements in the first few nanoseconds of an ICF laser pulse. Initial tests of the 5w conversion were completed at the Laboratory for Laser Energetics (LLE) and produced record 5ω energies. Based on these results from LLE, a 1 Joule, 5w laser system was designed for the NIF in 2018 and commissioning began in 2019. Commissioning of the 5ω laser system continued through 2023 and was eventually paused in Q1 of FY24 due to completing resource constraints. Commissioning of the 5w laser system proved incredibly challenging. Multiple issues were identified during commissioning and resolved, but issues remain. Currently there is not a clear understanding of why 5ω scattered has not been detected on the OTS collection system. Based on offline measurements, calculations, and preshot measurements the system appears to meet all requirements. Potential target physics issues have been investigated and do not appear to be an issue. The current hypothesis is that there is an error in one or more aspects of the offline testing not translating to expected performance when the system is fielded on the NIF. Additional full system testing in-situ utilizing the complete OTS system and NIF target chamber center time is needed to further test potential failure modes.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Long term microparticle impact fluxes on LDEF determined from optical survey of Interplanetary Dust Experiment (IDE) sensors

Many of the IDE metal-oxide-silicon (MOS) capacitor-discharge impact sensors remained active during the entire Long Duration Exposure Facility (LDEF) mission. An optical survey of impact sites on the active surfaces of these sensors has been extended to include all sensors from the low-flux sides of LDEF (i.e. the west or trailing side, the earth end, and the space end) and 5-7 active sensors from each LDEF's high-flux sides (i.e. the east or leading side, the south side, and the north side). This survey was facilitated by the presence of a relatively large (greater than 50 micron diameter) optical signature associated with each impact site on the active sensor surfaces. Of the approximately 4700 impacts in the optical survey data set, 84% were from particles in the 0.5 to 3 micron size range. An estimate of the total number of hypervelocity impacts on LDEF from particles greater than 0.5 micron diameter yields a value of approximately 7 x 10(exp 6). Impact feature dimensions for several dozen large craters on MOS sensors and germanium witness plates are also presented. Impact fluxes calculated from the IDE survey data closely matched surveys of similar size impacts (greater than or equal to 3 micron diameter craters in Al, or marginal penetrations of a 2.4 micron thick Al foil) by other LDEF investigators. Since the first year IDE data were electronically recorded, the flux data could be divided into three long term time periods: the first year, the entire 5.8 year mission, and the intervening 4.8 years (by difference). The IDE data show that there was an order of magnitude decrease in the long term microparticle impact flux on the trailing side of LDEF, from 1.01 to 0.098 x 10(exp -4) m(exp 2)/s, from the first year in orbit compared to years 2-6. The long term flux on the leading edge showed an increase from 8.6 to 11.2 x 10(exp -4) m(exp -2)/s over this same time period. (Short term flux increases up to 10,000 times the background rate were recorded on the leading side during LDEF's first year in orbit.) The overall east/west ratio was 44, but during LDEF's first year in orbit the ratio was 8.5, and during years 2-6 the ratio was 114. Long term microparticle impact fluxes on the space end decreased from 1.12 to 0.55 x 10(exp -4) m(exp -2)/s from the first year in orbit compared to years 2-6. The earth end showed the opposite trend with an increase from 0.16 to 0.38 x 10(exp -4) m(exp -2)/s. Fluxes on rows 6 and 12 decreased from 6.1 to 3.4 and 6.7 to 3.7 x 10(exp -4) m(exp -2)/s, respectively, over the same time periods. This resulted in space/earth microparticle impact flux ratios of 7.1 during the first year and 1.5 during years 2-6, while the south/north, space/north and space/south ratios remained constant at 1.1, 0.16 and 0.17, respectively, during the entire mission. This information indicates the possible identification of long term changes in discrete microparticle orbital debris component contributions to the total impact flux experienced by LDEF. A dramatic decrease in the debris population capable of striking the trailing side was detected that could possibly be attributed to the hiatus of western launch activity experienced from 1986-1989. A significant increase in the debris population that preferentially struck the leading side was also observed and could possibly be attributed to a single breakup event that occurred in September of 1986. A substantial increase in the microparticle debris population that struck the earth end of LDEF, but not the space end, was also detected and could possibly be the result of a single breakup event at low altitude. These results point to the importance of including discrete orbital debris component contribution changes in flux models in order to achieve accurate predictions of the microparticle environment that a particular spacecraft will experience in earth orbit. The only reliable, verified empirical measurements of these changes are reported in this paper. Further time-resolved in-situ measurements of these debris populations are needed to accurately assess model predictions and mitigation practices.

Simon, C. G.↗

Electrochemical Control of the Ultrafast Lattice Response of a Layered Semimetal

The unique layer-stacking in two-dimensional (2D) van der Waals materials facilitates the formation of nearly degenerate phases of matter and opens novel routes for the design of low-power, reconfigurable functional materials. Electrochemical ion intercalation between stacked layers offers a promising approach to stabilize bulk metastable phases and to explore the effects of extreme carrier doping and strain. However, in situ characterization methods to study the structural evolution and dynamical functional properties of these intercalated materials remains limited. Here a novel experimental platform is presented capable of simultaneously performing electrochemical lithium-ion intercalation and multimodal ultrafast characterization of the lattice using both electron diffraction and nonlinear optical techniques. Using the layered semimetal WTe 2 as a model system, the interlayer shear phonon mode that modulates stacking between 2Dlayers is probed, showing that small amounts of lithiation enhance the amplitude and lifetime of the phonon, contrary to expectations. This results from the dynamically fluctuating and anharmonic structure between nearly degenerate phases at room temperature, which can be stabilized by electronic carriers accompanying the inserted lithium ions. At high lithiation, the T d ’ structure emerges and quenches the phonon response. This work defines new approaches for using electrochemistry to engineer the dynamic structure of 2D materials.

36 MATERIALS SCIENCE↗

In situ high-temperature Raman spectroscopy for online EAF slag analysis

Real-time monitoring of slag chemistry is critical for optimizing Electric Arc Furnace (EAF) steelmaking operations, where dynamic variations in slag composition directly influence slag foaming, refractory degradation, and thermal efficiency. Conventional techniques such as X-ray fluorescence (XRF), Fourier-transform infrared (FTIR), and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS) are commonly used to analyze slag composition, but their offline nature and equipment constraints limit their applicability for online monitoring in harsh industrial environments. To address this challenge, we present an in situ, high-temperature analytical approach that integrates Raman spectroscopy with a custom designed fiber-optic probe for real-time slag characterization at 1550 °C. The system enables non destructive spectral acquisition from molten slags, providing molecular-level insights into silicate polymerization and iron oxidation states. Eight synthetic slag samples were evaluated, and key Raman features—such as Q n silicate units and FeO₄/FeO₆ coordination environments—were identified and quantitatively correlated with slag basicity and Fe₂O₃ content. The results demonstrate agreement between Raman spectral ratios and bulk slag chemistry, validating the method’s capability to track compositional and structural changes under molten temperature. This work establishes the feasibility of deploying fiber-optic Raman probe for online EAF slag monitoring and highlights their potential to support closed-loop control strategies, thereby enhancing process stability, refractory protection, and steel quality in industrial steelmaking applications.

47 OTHER INSTRUMENTATION↗

Correlating activities and defects in (photo)electrocatalysts using in-situ multi-modal microscopic imaging

Photo(electro)catalysts use sunlight to drive chemical reactions such as water splitting. A major factor limiting photocatalyst development is physicochemical heterogeneity which leads to spatially dependent reactivity. To link structure and function in such systems, simultaneous probing of the electrochemical environment at microscopic length scales and a broad range of timescales (ns to s) is required. Here, we address this challenge by developing and applying in- situ (optical) microscopies to map and correlate local electrochemical activity, with hole lifetimes, oxygen vacancy concentrations and photoelectrode crystal structure. Using this multi-modal approach, we study prototypical hematite (α-Fe 2 O 3 ) photoelectrodes. We demonstrate that regions of α-Fe 2 O 3 , adjacent to microstructural cracks have a better photoelectrochemical response and reduced back electron recombination due to an optimal oxygen vacancy concentration, with the film thickness and extended light exposure also influencing local activity. Our work highlights the importance of microscopic mapping to understand activity, in even seemingly homogeneous photoelectrodes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In-situ relative calibration of Bragg crystals with Monte Carlo line ratio analysis

X-ray line emission spectra can thoroughly characterize hot plasmas, especially when line shapes and ratios convey distinct aspects of plasma conditions. However, the high spectral resolution required for observing line shapes is often at odds with the large bandwidth required to observe many line ratios across a wide spectral range. One strategy to obtain high spectral resolution over a wide bandwidth is to use multiple crystals with calibrated reflectivity so that line intensities across different crystals can be compared. Here, we explore the use of a low-resolution, wide-bandwidth mica survey spectrometer to infer relative reflectivity of two high-resolution, narrow-bandwidth quartz crystals. Finally, a Monte Carlo error analysis determines comparable x-ray line ratios measured from both spectrometers, resulting in an in situ calibration factor and associated uncertainty for the relative reflectivity of the high-resolution crystals.

47 OTHER INSTRUMENTATION↗

Materials, structures, and devices for high-speed electronics

Advances in materials, devices, and instrumentation made under this grant began with ex-situ null ellipsometric measurements of simple dielectric films on bulk substrates. Today highly automated and rapid spectroscopic ellipsometers are used for ex-situ characterization of very complex multilayer epitaxial structures. Even more impressive is the in-situ capability, not only for characterization but also for the actual control of the growth and etching of epitaxial layers. Spectroscopic ellipsometry has expanded from the research lab to become an integral part of the production of materials and structures for state of the art high speed devices. Along the way, it has contributed much to our understanding of the growth characteristics and material properties. The following areas of research are summarized: Si3N4 on GaAs, null ellipsometry; diamondlike carbon films; variable angle spectroscopic ellipsometry (VASE) development; GaAs-AlGaAs heterostructures; Ta-Cu diffusion barrier films on GaAs; GaAs-AlGaAs superlattices and multiple quantum wells; superconductivity; in situ elevated temperature measurements of III-V's; optical constants of thermodynamically stable InGaAs; doping dependence of optical constants of GaAs; in situ ellipsometric studies of III-V epitaxial growth; photothermal spectroscopy; microellipsometry; and Si passivation and Si/SiGe strained-layer superlattices.

Woollam, John A.↗

North Atlantic Aerosol Radiative Impacts Based on Satellite Measurements and Aerosol Intensive Properties from TARFOX and ACE-2

We estimate the impact of North Atlantic aerosols on the net short-wave flux at the tropopause by combining satellite-derived aerosol optical depth (AOD) maps with model aerosol properties determined via closure analyses in TARFOX and ACE 2. We exclude African dust, primarily by restricting latitudes to 25-60 N. The analyses use in situ aerosol composition measurements and air- and ship-borne sun-photometer measurements of AOD spectra. The aerosol model yields computed flux sensitivities (dFlux/dAOD) that agree with measurements by airborne flux radiometers in TARFOX. Its midvisible single-scattering albedo is 0.9. which is in the range obtained from in situ measurements of scattering and absorption in both TARFOX and ACE 2. Combining satellite-derived AOD maps with the aerosol model yields maps of 24-hour average net radiative flux changes. For simultaneous AVHRR, radiance measurements exceeded the sunphotometer AODs by about 0.04. However. shipboard sunphotometer and AVHRR AODs agreed Within 0.02 for data acquired during satellite overflights on two other days. We discuss attempts to demonstrate column closure within the MBL by comparing shipboard sunphotometer AODs and values calculated from simultaneous shipboard in-situ aerosol size distribution measurements. These comparisons were mostly unsuccessful, but they illustrate the difficulties inherent in this type of closure analysis. Specifically, AODs derived from near-surface in-situ size distribution measurements are extremely sensitive to the assumed hygroscopic growth model that itself requires an assumption of particle composition as a function of height and size, to the radiosonde-measured relative humidity, and to the vertical profile of particle number. We investigate further the effects of hygroscopic particle growth within the MBL by using shipboard lidar aerosol backscatter profiles together with the sunphotometer AOD.

Russell, P. B.↗

Step Bunch Evolution on Vicinal Faces of KDP

For in-situ studies of the formation and evolution of step patterns in solution growth, we have assembled an experimental setup based on Michelson interferometry with the growing crystal surface as one of the reflective surfaces. The device allows data collection over a relatively large area (approximately 4 sq. mm) in situ and in real time during growth. The depth resolution is improved over traditional interferometry using phase-shifted images combining by a suitable algorithm. We achieve a depth resolution of approximately 50 Angstroms. Lateral resolution, dependent on the degree of magnification, is around 0.3 to 5 microns. The crystal chosen as a model in this work is potassium dihydrogen phosphate (KDP), the optically non-linear material widely used in frequency doubling applications. Kinetics of KDP crystallization is well studied so that KDP can serve as a benchmark for our investigations. We present quantitative results on the onset, initial stages and development of instabilities in moving step trains on vicinal crystal surfaces at varying supersaturation, flow rate, and flow direction. The kinetics data suggest that at low supersaturations, step bunching is caused by impurity retardation of the steps, while at higher supersaturations, we link the non-linearity during growth to interdependence of the velocity and density of the steps evidenced in independent experiments. The behavior on the surface is very dynamic, small bunches both merge and split from larger bunches as they travel across the facet. We present evidence that despite these dynamics, under steady conditions there exists a limiting value to step bunch height. This height is reached at distances between 600 and 1000 microns from the step source. In our experiments, we observed the retention of this step bunch height limit up to the path of 1500 microns.

Booth, N. A.↗

Laboratory and In-Flight In-Situ X-ray Imaging and Scattering Facility for Materials, Biotechnology and Life Sciences

We propose a multifunctional X-ray facility for the Materials, Biotechnology and Life Sciences Programs to visualize formation and behavior dynamics of materials, biomaterials, and living organisms, tissues and cells. The facility will combine X-ray topography, phase micro-imaging and scattering capabilities with sample units installed on the goniometer. This should allow, for the first time, to monitor under well defined conditions, in situ, in real time: creation of imperfections during growth of semiconductors, metal, dielectric and biomacromolecular crystals and films, high-precision diffraction from crystals within a wide range of temperatures and vapor, melt, solution conditions, internal morphology and changes in living organisms, tissues and cells, diffraction on biominerals, nanotubes and particles, radiation damage, also under controlled formation/life conditions. The system will include an ultrabright X-ray source, X-ray mirror, monochromator, image-recording unit, detectors, and multipurpose diffractometer that fully accommodate and integrate furnaces and samples with other experimental environments. The easily adjustable laboratory and flight versions will allow monitoring processes under terrestrial and microgravity conditions. The flight version can be made available using a microsource combined with multilayer or capillary optics.

Source record↗

Application of Laser Based Ultrasound for NDE of Damage in Thick Stitched Composites

As design engineers implement new composite systems such as thick, load bearing composite structures, they must have certifiable confidence in structure s durability and worthiness. This confidence builds from understanding the structural response and failure characteristics of simple components loaded in testing machines to tests on full scale sections. Nondestructive evaluation is an important element which can provide quantitative information on the damage initiation, propagation, and final failure modes for the composite structural components. Although ultrasound is generally accepted as a test method, the use of conventional ultrasound for in-situ monitoring of damage during tests of large structures is not practical. The use of lasers to both generate and detect ultrasound extends the application of ultrasound to in- situ sensing of damage in a deformed structure remotely and in a non-contact manner. The goal of the present research is to utilize this technology to monitor damage progression during testing. The present paper describes the application of laser based ultrasound to quantify damage in thick stitched composite structural elements to demonstrate the method. This method involves using a Q-switched laser to generate a rapid, local linear thermal strain on the surface of the structure. This local strain causes the generation of ultrasonic waves into the material. A second laser used with a Fabry-Perot interferometer detects the surface deflections. The use of fiber optics provides for eye safety and a convenient method of delivering the laser over long distances to the specimens. The material for these structural elements is composed of several stacks of composite material assembled together by stitching through the laminate thickness that ranging from 0.5 to 0.8 inches. The specimens used for these nondestructive evaluation studies had either impact damage or skin/stiffener interlaminar failure. Although little or no visible surface damage existed, internal damage was detected by laser based ultrasound.

Anastasi, Robert F.↗

PING Gamma Ray and Neutron Measurements of a Meter-Sized Carbonaceous Asteroid Analog

Determining the elemental composition of carbonaceous (spectral type C) asteroids is still one of the basic problems when studying these objects. The only main source of elemental composition information for asteroids is from their optical, NIR and IR properties, which include their spectral reflectance characteristics, albedo, polarization, and the comparison of optical spectroscopy with meteorite groups corresponding to asteroids of every spectral type. Unfortunately, these sources reflect observations from widely contrasting spatial scales that presently yield a void in the continuum of microscopic and macroscopic evidence, a lack of in situ measurement confirmation, and require deeper sensing techniques to discern the nature of these asteroids. The Probing In situ with Neutrons and Gamma rays (PING) instrument is ideally suited to address this problem because it can be used to determine the bulk elemental composition, H and C content, the average atomic weight and density of the surface and subsurface layers of C-type asteroids, and can provide measurements used to determine the difference between and distinguish between different types of asteroids. We are currently developing the PING instrument that combines gamma ray and neutron detectors with a 14 Me V pulsed neutron generator to determine the in-situ bulk elemental abundances and geochemistry of C-type asteroids with a spatial resolution of 1 m down to depths of tens of cm to 1 m. One aspect of the current work includes experimentally testing and optimizing PING on a known meter-sized Columbia River basalt C-type asteroid analog sample that has a similar composition and the same neutron response as that of a C-type asteroid. An important part of this effort focuses on utilizing timing measurements to isolate gamma rays produced by neutron inelastic scattering, neutron capture and delayed activation processes. Separating the gamma ray spectra by nuclear processes results in higher precision and sensitivity elemental composition measurements. Using gated data acquisition techniques allows for the unambiguous identification of gamma ray lines from different isotopes and nuclear processes, especially in situations when limited detector resolution results in overlapping gamma ray lines that cannot be individually resolved. In this paper, we will present the PING basalt layering experimental data, taken at the test facility at NASA Goddard Space Flight Center using the time tagged event-by-event data analysis technique, compared to our MCNPX computer simulation results for the C-type asteroid and basalt layering simulant models. Comparison of these data will show the advantages, validity, and measurement sensitivity of PING's nuclear interrogation methods to obtain more precise and sensitive in situ bulk elemental composition and density measurements of the subsurface of asteroids.

Bodnarik, J.↗

Comparison of Surface and Column Variations of CO2 Over Urban Areas for Future Active Remote CO2 Sensors

High resolution in-situ CO2 measurements were recorded onboard the NASA P-3B during the DISCOVER-AQ (Deriving Information on Surface Conditions from Column and Vertically Resolved Observations Relevant to Air Quality) Field Campaign, to investigate the ability of space-based observations to accurately assess near surface conditions related to air quality. This campaign includes, Washington DC/Baltimore, MD (July 2011), San Joaquin Valley, CA (January - February 2013), Houston, TX (September 2013), and Denver, CO (July-August 2014). Each of these campaigns consisted of missed approaches and approximately two hundred vertical soundings of CO2 within the lower troposphere (surface to about 5 km). In this study, surface (0 - 1 km) and column-averaged (0 - 3.5 km) CO2 mixing ratio values from the vertical soundings in the four geographically different urban areas are used to investigate the temporal and spatial variability of CO2 within the different urban atmospheric emission environments. Tracers such as CO, CH2O, NOx, and NMHCs are used to identify the source of CO2 variations in the urban sites. Additionally, we apply nominal CO2 column weighting functions for potential future active remote CO2 sensors operating in the 1.57-microns and 2.05-microns measurement regions to convert the in situ CO2 vertical mixing ratio profiles to variations in CO2 column optical depths, which is what the active remote sensors actually measure. Using statistics calculated from the optical depths at each urban site measured during the DISCOVER-AQ field campaign and for each nominal weighting function, we investigate the natural variability of CO2 columns in the lower troposphere; relate the CO2 column variability to the urban surface emissions; and show the measurement requirements for the future ASCENDS (Active Sensing of CO2 Emissions over Nights, Days, and Seasons) in the continental U.S. urban areas.

Choi, Yonghoon↗

Non-Topographic Space-Based Laser Remote Sensing

In the past 20+ years, NASA Goddard Space Flight Center (GSFC) has successfully developed and flown lidars for mapping of Mars, the Earth, Mercury and the Moon. As laser and electro-optics technologies expand and mature, more sophisticated instruments that once were thought to be too complicated for space are being considered and developed. We will present progress on several new, space-based laser instruments that are being developed at GSFC. These include lidars for remote sensing of carbon dioxide and methane on Earth for carbon cycle and global climate change; sodium resonance fluorescence lidar to measure environmental parameters of the middle and upper atmosphere on Earth and Mars and a wind lidar for Mars orbit; in situ laser instruments include remote and in-situ measurements of the magnetic fields; and a time-of-flight mass spectrometer to study the diversity and structure of nonvolatile organics in solid samples on missions to outer planetary satellites and small bodies.

Laser↗

Low-Temperature Production of Cosmic Grains Analogs From Gas-Phase Molecular Precursors with the NASA Ames' COSmIC Facility

Complex carbon molecules and ions are ubiquitous in space and form the building blocks of carbonaceous cosmic dust grains, ultimately contributing to the formation of planets. Here, we report the first experimental investigations of the low temperature chemical pathways leading to the production of cosmic grain analogs from gas phase molecular precursors in order to better understand the evolution of cosmic carbon. The experiments were performed using the COsmic SImulation Chamber (COSmIC) to generate and characterize grains formed from gas phase precursors under controlled conditions representative of astrophysical environments [1]. Using COSmIC, it is possible to investigate the evolution of cosmic carbon from the formation of neutral and ionized gas phase hydrocarbons and PAHs [2], to carbon grains [3, 4]. This is achieved by using a discharge nozzle to (1) produce an adiabatic jet expansion and cool down Ar-hydrocarbon/PAH gas mixtures to astrophysically relevant temperature (150 K) before inducing chemistry by generating a plasma discharge in the stream of the expansion. This plasma-induced chemistry results in the formation of complex molecules and solid particles, analogs of cosmic grains. Solid grains are produced in-situ in the plasma expansion, carried by the accelerated gas in the expansion, and collected on substrates placed a few centimeters downstream of the electrodes. The results of a preliminary solid phase ex-situ analysis of cosmic grain analogs produced at low temperature in COSmIC from gas mixtures including molecular precursors of cosmic carbon grains, i.e., such as CH4 and C2H2 found in circumstellar ejecta of late C stars [3] as well as PAHs ubiquitously detected in IR emission bands seen in galactic and extragalactic environments [4] will be discussed. Scanning Electron Microscopy imaging was used to provide insight on the morphology and growth structure of the grains produced in COSmIC, and to investigate how the precursors used to produce the grains affect these parameters [3]. Laser desorption mass spectrometry was used to identify the molecules making up the main structures within the condensed grains [4]. NIR to FIR optical properties are characterized to provide critical information (functional groups, optical constants) to the scientific community, for use in radiative transfer models in particular, and to help decipher and enhance the return data from space observations.

F. Salama↗

The Additive Manufacturing Moment Measure - A Parallel Computation Technique for Determining Build Variance in the Laser Powder Bed Fusion Process

Additive manufacturing (AM) has unique process attributes that facilitate the creation of optimized, complex, and unique parts for aerospace applications. However, the multi-scale and complicated building process for AM parts can cause unexpected build conditions that result in microstructural variability within the deposited material. The need for richer datasets and computational modeling capabilities to improve AM process reliability is a consequence of this microstructural variability. A computational approach, referred to as the Additive Manufacturing Moment Measure (AM3), addresses this need by leveraging the way AM processes fuse material in precise, incremental steps. During the layering sequence, each previous step contributes to the condition of the current step at the center of the heat source. The precise steps can be selected to systematically create a time-space point field with co-located machine input and in-situ sensor data. The sequential nature of the AM process, coupled with nearest neighbor calculations, allows for a fully parallel computation for part-scale build profile analysis. The AM3 concept introduced here enables part-scale assessment directly from build files and in-situ process monitoring sensors alike. The AM moment measures were calculated for build point fields and compared with co-located in-situ and ex-situ nondestructive evaluation and optical microscopy observations. These comparisons permit a better understanding of how the sequential process actions can affect the quality of a laser powder bed fusion (LPBF) build. Details of the AM3technique will be discussed and compared to measured LPBF part characteristics. The AM3 results indicate a strong potential to advance the qualification process for aerospace applications.

Additive Manufacturing↗

In-Situ Process Monitoring, Synchronization, and Mapping Laser Powder Bed Fusion Builds of Ti6Al4V

The use of in-situ process monitoring is of interest to lower the cost of inspection for the qualification of laser powder bed fusion (LPBF) parts. Precise monitoring of the LPBF-AM build process constitutes a multi-scale and multi-discipline task. There are several significant challenges to the in-situ approach: the synchronization of sensor signals to process steps, the physical interpretation and classification of sensor signals, managing very large datasets, and comparing the inputs with the observed monitoring signals. At NASA Langley Research Center, a configurable architecture additive testbed has been developed to monitor the build process with synchronized sensors. The philosophy and method adopted for the synchronization of the cameras with laser power & position Ti-6Al-4V LPBF are described. The synchronized in-situ monitoring signals are compared with ex-situ nondestructive inspection and optical microscopy observations. Such comparisons permit a better understanding of how the sequential process actions of LPBF-AM can affect build quality.

Laser Powder Bed Fusion↗

Advances in Molecular Beam Epitaxy Growth of Ultra-Wide Bandgap Ga2O3 Based Alloys

Gallium oxide (Ga2O3) is an emerging ultra-wide bandgap semiconductor material that has attracted attention for its potential to outperform existing SiC and GaN based devices operating at high breakdown voltages and high temperature. Isovalent alloying of In and Al in Ga2O3 provides the ability to engineer bandgap energy and strain of the material. Alloying with Al increases the bandgap energy and the theoretically achievable Baliga's figure of merit, a key measure of a material's ultimate performance limits for high power switching devices. Alloying with In introduces compressive strain and can be used to counteract the tensile strain of Al incorporation. The resulting (AlxGa1-x-yIny)2O3 alloy can be lattice-matched to commercially available Ga2O3 wafers and has a tunable bandgap energy greater than that of Ga2O3, 4.76 eV. Such lattice-matched material can be grown arbitrarily thick without the detrimental effects of elastic strain and relaxation, making it suitable for high voltage diodes and transistors. However, efforts to synthesize isovalent alloys are complicated by their tendency to phase separate into corundum Al2O3 or bixbyite In2O3. Literature reports of the quaternary (AlxGa1-x-yIny)2O3 are limited to <1% unintentional indium incorporation in In-catalyzed (AlxGa1-x)2O3. The primary limitation to quaternary growth is the limited incorporation of indium at elevated growth temperatures. This limited incorporation is due to both the volatility of indium oxide and Al and Ga cation exchange reactions which replace indium in In2O3. We report on the development of a novel high-throughput molecular beam epitaxy (MBE) technique to screen the growth conditions for the ternary alloy (InyGa1-y)2O3, and the application of these findings to the first successful synthesis of phase pure monoclinic (AlxGa1-x-yIny)2O3 by MBE. By leveraging the unique sub-oxide chemistry of Ga2O3 and in-situ monitoring of crystal properties by reflection high-energy electron diffraction (RHEED), a cyclical growth and etch-back method is developed and applied to rapidly characterize the (InyGa1-y)2O3 growth space. This cyclical method provides approximately 10x increase in experimental throughput and up to 46x improvement in Ga2O3 substrate utilization. Appropriate growth conditions for monoclinic (InyGa1- y)2O3 are identified by machine learning analysis of RHEED patterns and targeted growths are characterized ex-situ to confirm improved In incorporation. These growth conditions are then combined with established (AlxGa1-x)2O3 growth conditions to grow quaternary (AlxGa1-x-yIny)2O3 with Al mole fractions ranging from 1.4% - 24.4% and In mole fractions ranging from 3.1% to 15.5%. The chemical and optical properties of the alloys are investigated by XRD, XPS, and spectroscopic ellipsometry. A lattice-matched (AlxGa1-x-yIny)2O3 alloy is examined by 4D-STEM and the chemical and physical uniformity of Al and In incorporation are discussed.

alloy↗