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At least 109 records · Page 6

MAB Phase Ceramics for Lunar Applications

During the ten-week internship my work focused on designing characterization protocol for 3D printed MAB phase ceramics on steel and Tiplates. I was mentored by Dr. Samuel Hocker of NASA and advised by Dr. Gupta from University of North Dakota. I also collaborated with Mackenzie Short from the University of North Dakota. The characterization protocol was divided into following steps; initially, we performed visual inspection of the plates. During this process, the coatings which spalled or delaminated were discarded for further evaluation. During the next step, we performed optical microscopy to discern and document surface features and porosities of the samples. We also noted some decomposition under the optical microscope as well. Thereafter, profilometry analysis was performed to understand the effect of power density on the surface roughness. Due to the deposited powder over the samples, the profilometry was inconclusive. We then cleaned the samples on the steel plate using ethanol and cotton swabs to wipe up the loose powder covering the samples. Detailed SEM analysis was then performed on the cleaned specimens. In parallel, the 3D printed samples on the Tiplate were cleaned by using an ultrasonic bath for 1h. Optical imaging showed that this cleaning process was more effective for cleaning except that small cracks propagated through the layered ceramics. The profilometry data gathered on the titanium plate after cleaning was more conclusive. The SEM data on the steel plate showed that there is decomposition at all wattages although at 100 W the extent of decomposition was lower. We are planning to characterize the steel samples after cleaning in ultrasonic bath for 5-10 min to minimize cracking during the cleaning process. In addition, we are also planning to study the fractured surface by SEM analysis.

Additive Manufacturing, Laser Powder Bed Fusion, S↗

Understanding the Feasibility of MAB Phase Structures for Lunar Applications

During the ten-week internship, my work focused on synthesis, characterization, and tailoring the flowability of the MAB phase powders for improving the surface finish and decreasing porosity of 3D-printed MAB phase structures. My mentor for the project was Dr. Samuel Hocker from NASA Langley and my faculty advisor was Dr. Surojit Gupta from the University of North Dakota. I also collaborated with Daniel Trieff from the University of North Dakota in developing characterization paradigm of 3D printed samples. The microencapsulation was performed via novel solvent casting-based microencapsulation process pioneered in UND, wherein a polymer (PLA, PHA) was dissolved into dichloromethane and precipitated onto the surface of the MoAlB particles. Two 100mL samples of microencapsulated powder was outsourced to Particle Technology Labs for flowability testing along with a 100mL control sample to determine if microencapsulation is a valid method for improving the flowability. The microencapsulated powders were characterized using SEM, Differential Scanning Calorimetry, and optical microscopy. The SEM images showed no change between the pure and microencapsulated powders. The optical microscopy analysis indicated a reduction in reflectivity for the PLA microencapsulated powders as well as hydrophobic properties. Both results suggest that microencapsulation was successful as PLA is a hydrophobic polymer and the change in reflectivity could be a result of the light being dispersed through the polymer coating. A reflectivity analysis will be done to bring more perspective to these observations. If powder flowability is improved, then the project will move forward with testing the printability of the microencapsulated powders and characterizing the structures using the designed characterization protocol. We are waiting for the DSC results. The characterization protocol for the 3D-printed MAB structures included a visual inspection of the plates to rule out any samples that had spalled or delaminated, optical microscopy to document surface features, porosity, and decomposition, and cleaning of the plates using an ultrasonic bath in preparation for SEM, EDS, and profilometry analyses.

MAB Phase↗

Uncertainty Quantification of Classical Theories of Dendritic Growth Kinetics Applied to Nickel-Based Alloys

The solidification velocity in a model nickel-alloy single crystal during laser spot melting was recently characterized using synchrotron X-ray imaging. The measured solidification velocity was found to exceed the absolute stability threshold predicted by the Kurz-Giovanola-Trivedi (KGT) model. The discrepancies between the model and experiments motivate the further assessment of accurate material properties. This work quantifies the impact material property uncertainty has on model predictions of the absolute stability threshold velocities. Properties from the literature are reviewed and compared to those calculated using computational thermodynamics to provide uncertainty estimates on input properties to the KGT model. Global sensitivity analysis is used to quantify the influence of each uncertain input property on the predicted threshold velocity. This work supports the understanding of the nickel-alloy solidification during powder bed fusion additive manufacturing and identifies the solidification material properties that are the most important to assess from first-principles computations and experiments.

Computational thermodynamics↗

Melting of troilite at high pressure in a diamond cell by laser heating

A system for measuring melting temperatures at high pressures is described. The sample is heated with radiation from a YAG laser. The beam is reflected downward through a microscope objective, through the upper diamond anvil, and focused onto the sample. Hense, intense heating is produced only at the sample and not within the diamond anvils. A vidicon system is used to observe the sample during heating. Incandescent light from the heated sample passes back through the objective lens into a grating spectrometer. The spectrum of the incandescent light is received by the photodiode array and stored in the multichannel analyzer. These data can then be transferred to floppy disk for analysis. A curve fitting program is used to compare the spectra with standard blackbody curves and to determine the temperature. Pressure is measured by the ruby fluorescence method. The system was used to study the melting behavior of natural troilite (FeS).

Bassett, William A.↗

CO2 lasers and applications II; Proceedings of the Third European Congress on Optics, The Hague, Netherlands, Mar. 12-14, 1990

Recent advances in CO2 laser technology and its applications are examined. Topics discussed include the excitation of CO2 lasers by microwave discharge, a compact RF-excited 12-kW CO2 laser, a robotic laser for three-dimensional cutting and welding, three-dimensional CO2-laser material processing with gantry machine systems, and a comparison of hollow metallic waveguides and optical fibers for transmitting CO2-laser radiation. Consideration is given to an aerodynamic window with a pump cavity and a supersonic jet, cutting and welding Al using a high-repetition-rate pulsed CO2 laser, speckle reduction in CO2 heterodyne laser radar systems, high-power-laser float-zone crystal growth, melt dynamics in surface processing with laser radiation, laser hardfacing, surface melting of AlSi10Mg with CO2 laser radiation, material processing with Cu-vapor lasers, light-induced flow at a metal surface, and absorption measurements in high-power CW CO2-laser processing of materials.

Opower, Hans↗

Determination of H2O and CO2 concentrations in fluid inclusions in minerals using laser decrepitation and capacitance manometer analysis

Water and carbon dioxide concentrations within individual and selected groups of fluid inclusions in quartz were analyzed by using laser decrepitation and quantitative capacitance manometer determination. The useful limit of detection (calculated as ten times the typical background level) is about 5 x 10(-10) mol of H2O and 5 x 10(-11) mol of CO2; this H2O content translates into an aqueous fluid inclusion approximately 25 micrometers in diameter. CO2/H2O determinations for 38 samples (100 separate measurements) have a range of H2O amounts of 5.119 x 10(-9) to 1.261 x 10(-7) mol; CO2 amounts of 7.216 x 10(-10) to 1.488 x 10(-8) mol, and CO2/H2O mole ratios of 0.011 to 1.241. Replicate mole ratio determinations of CO2/H2O for three identical (?) clusters of inclusions in quartz have average mole ratios of 0.0305 +/- 0.0041 1 sigma. Our method offers much promise for analysis of individual fluid inclusions, is sensitive, is selective when the laser energy is not so great as to melt the mineral (laser pits approximately 50 micrometers in diameter), and permits rapid analysis (approximately 1 h per sample analysis).

Water/analysis↗

Silicon-Web-Growing Machine

Silicon replenished automatically as web is withdrawn. Semiautomatic silicon-web-growing machine set down in detailed engineering drawings. Melt level sensed with He/Ne laser beam and melt-level error signal used to control motor-driven pellet feeder, speeding up when level is low. System reduces demand upon operator's time.

Duncan, C.↗

Laser Wire Stripper

NASA-developed space shuttle technology is used in a laser wire stripper designed by Raytheon Company. Laser beams cut through insulation on a wire without damaging conductive metal, because laser radiation that melts plastic insulation is reflected by the metal. The laser process is fast, clean, precise and repeatable. It eliminates quality control problems and the expense of rejected wiring.

Source record↗

Compositional and Microstructural Evolution of Olivine During Pulsed Laser Irradiation: Insights Based on a FIB/Field-Emission TEM Study

Introduction: The use of pulsed laser irradiation to simulate the short duration, high-energy conditions characteristic of micrometeorite impacts is now an established approach in experimental space weathering studies. The laser generates both melt and vapor deposits that contain nanophase metallic Fe (npFe(sup 0)) grains with size distributions and optical properties similar to those in natural impact-generated melt and vapor deposits. There remains uncertainty, however, about how well lasers simulate the mechanical work and internal (thermal) energy partitioning that occurs in actual impacts. We are currently engaged in making a direct comparison between the products of laser irradiation and experimental/natural hypervelocity impacts. An initial step reported here is to use analytical TEM is to attain a better understanding of how the microstructure and composition of laser deposits evolve over multiple cycles of pulsed laser irradiation. Experimental Methods: We irradiated pressed-powder pellets of San Carlos olivine (Fo(sub 90)) with up to 99 rastered pulses of a GAM ArF excimer laser. The irradiated surface of the sample were characterized by SEM imaging and areas were selected for FIB cross sectioning for TEM study using an FEI Quanta dual-beam electron/focused ion beam instrument. FIB sections were characterized using a JEOL2500SE analytical field-emission scanning transmission electron microscope (FE-STEM) optimized for quantitative element mapping at less than 10 nm spatial resolutions. Results: In the SEM the 99 pulse pressed pellet sample shows a complex, inhomogeneous, distribution of laser-generated material, largely concentrated in narrow gaps and larger depressions between grains. Local concentrations of npFe0 spherules 0.1 to 1 micrometers in size are visible within these deposits in SEM back-scatter images. Fig. 1 shows bright-field STEM images of a FIB cross-section of a one of these deposits that continuously covers the top and sloping side of an olivine grain. The deposit has 3 microstructurally distinct sub-layers composed of silicate glass with varying modal fractions and size distributions of npFe( sup 0) spherules, along with nanocrystalline silicate material. A relatively thin (50-300 nm) topmost surface layer has a high-concentration of npFe0 spherules 5-20 nm in size. Element mapping shows the layer to be enriched in Fe by a factor of 2.5 relative to the olivine substrate, with Mg and Si depleted by 20% and 10% respectively. This is compositionally complementary to the underlying, middle layer of the deposit that is depleted in Fe, enriched in Mg and has a much lower npFe0 concentration. A third layer of nanocrystalline olivine occurs at the substrate interface. Discussion: The FE-STEM results suggest the topmost layer is a vapor deposit, underlain by a thicker microstructurally complex melt-generated layer. The compositional relations suggest the melt layer was partially vaporized, preferentially losing more volatile elements (e.g., Fe). The vaporized material re-condensed to form the thin, npFe(sup 0)-rich surface deposit during or immediately after the scan cycle. Nanocrystalline olivine that grew within the melt layer as it formed and cooled is similar in volume and microstructure to what we have observed in the impact melt lining of a micrometeorite impact crater in olivine. This suggest the time-temperature relations attained in the laser sample may not be too different from a micrometeorite impact. Our TEM observations, however, do not show evidence for the same level of mechanical dam-age (e.g., fracturing) seen around the natural micrometeorite crater.

Christoffersen, R.↗

Effects of Microsecond Pulse Laser Irradiation on Vis-NIR Reflectance Spectrum of Carbonaceous Chondrite Simulant: Implications for Martian Moons and Primitive Asteroids

Goal of this study is to make a progress in understanding the optical effects of space weathering on small bodies believed to be similar in composition to carbonaceous chondrites: C, G, B, F, T, D, and P asteroids and possibly Martian satellites Phobos and Deimos. The companion work focuses on petrological and mineralogical aspects of this process. One of the main factors of space weathering is meteorite and micrometeorite bombardment leading, in particular, to impact melting of components of the regolith. Studies of lunar regolith and laboratory experiments simulating impact melting show that the melting products differ from the unmelted material in mineralogy and distribution of chemical components among different phases that results in spectral changes. We simulate impact melting of CM chondrite by pulse laser irradiation of an artificial analog of such a meteorite. The analog is a mixture of 46 wt.% non-magnetic fraction of L5 ordinary chondrite Tsarev, 47 wt.% serpentine, 5 wt.% kerite, and 2 wt.% calcite. It simulates rather well bulk chemistry, including volatiles such as H2O and CO2, and only approximately the CM chondrite mineralogy. Thus, we do not expect the mixture to be spectrally similar to CM chondrites, but expect the laser melting products to be similar to those formed by impact melting of natural CM chondrites.

Hiroi, T.↗

Near Infrared In-situ Measurements for the Detection of Keyhole Porosity in Autogenous Ti-6AL-4V Welds

Certification of additive manufactured metal parts requires nondestructive evaluation (NDE) to ensure build quality. NDE can be performed during the build process or post build. For large parts with complex geometries, post build NDE can be challenging. In-situ NDE potentially provides a way to perform the inspection layer by layer. This work explores the use of a high speed near infrared (NIR) camera that is focused in-line with a laser to obtain high spatial and temporal resolution thermal imagery of the melt pool and associated cooling areas. The thermal data is obtained during a laser melting process using Ti-6AL-4V plate and of particular interest is the detection of keyhole porosity. Keyhole porosity can result from non-optimal build conditions, such as excessive laser power at a given laser scanning speed, that creates an entrapped bubble. The NIR measured melt pool and cooling areas are processed to detect keyhole porosity. The results are compared to X-ray CT results for validation.

additive manufacturing↗

Near Infrared In-situ Measurements for the Detection of Keyhole Porosity in Autogenous Ti-6AL-4V Welds

Certification of additive manufactured metal parts requires nondestructive evaluation (NDE) to ensure build quality. NDE can be performed during the build process or post build. For large parts with complex geometries, post build NDE can be challenging. In-situ NDE potentially provides a way to perform the inspection layer by layer. This work explores the use of a high speed near infrared (NIR) camera that is focused in-line with a laser to obtain high spatial and temporal resolution thermal imagery of the melt pool and associated cooling areas. The thermal data is obtained during a laser melting process using a Ti-6Al-4V plate and of particular interest is the detection of keyhole porosity. Keyhole porosity can result from non-optimal build conditions, such as excessive laser power at a given laser scanning speed, that creates an entrapped bubble. The NIR measured melt pool and cooling areas are processed to detect keyhole porosity. The results are compared to X-ray CT results for validation. Small keyhole pores buried deep were not detectable with this technique, however, some larger subsurface elongated pores along with some open surface pores did show some promise for detectability.

additive manufacturing↗

Compositional and Microstructural Evolution of Olivine Under Multiple-Cycle Pulsed Laser Irradiation as Revealed by FIB/Field-Emission TEM

The use of pulsed laser irradiation to simulate the short duration, high-energy conditions characteristic of micrometeorite impacts is now an established approach in experimental space weathering studies. The laser generates both melt and vapor deposits that contain nanophase metallic Fe (npFe(sup 0)) grains with size distributions and optical properties similar to those in natural impact-generated melt and vapor deposits. There remains uncertainty, however, about how well lasers simulate the mechanical work and internal (thermal) energy partitioning that occurs in actual impacts. We are currently engaged in making a direct comparison between the products of laser irradiation and experimental/natural hypervelocity impacts. An initial step reported here is to use analytical SEM and TEM is to attain a better understanding of how the microstructure and composition of laser deposits evolve over multiple cycles of pulsed laser irradiation.

Christoffersen, R.↗

Laser annealing of ion implanted CZ silicon for solar cell junction formation

The merits of large spot size pulsed laser annealing of phosphorus implanted, Czochralski grown silicon for function formation of solar cells are evaluated. The feasibility and requirements are also determined to scale-up a laser system to anneal 7.62 cm diameter wafers at a rate of one wafer/second. Results show that laser annealing yields active, defect-free, shallow junction devices. Functional cells with AM 1 conversion efficiencies up to 15.4% for 2 x 2 cm and 2 x 4 cm sizes were attained. For larger cells, 7.62 cm dia., conversion efficiencies ranged up to 14.5%. Experiments showed that texture etched surfaces are not compatible with pulsed laser annealing due to the surface melting caused by the laser energy. When compared with furnace annealed cells, the laser annealed cells generally exhibited conversion efficiencies which were equal to or better than those furnace annealed. In addition, laser annealing has greater throughput potential.

Katzeff, J. S.↗

Manufacturing of Thermoset Polyimide Composites by Laser Sintering

Selective Laser Sintering (SLS) is an additive manufacturing technique that builds 3D models layer by layer using a laser to selectively melt cross sections in powdered polymeric materials, following sequential slices of the computer-aided design (CAD) model. SLS generally uses thermoplastic polymeric powders such as polyamides. The resultant 3D-printed objects are often weaker in their strength compared to traditionally processed materials, due to their higher porosity. This paper described the process development of using melt-processable imide oligomers terminated with reactive 4-phenylethynylphthalic anhydride (4-PEPA) to conduct laser sintering (LS). The first successful 3D-printing of high temperature RTM370 thermoset polyimide carbon fiber composites were further post-cured to promote additional crosslinking for achieving higher temperature (T g = 370°C) capability. Another novel imide oligomer, RTM385-SLS, formulated with a complex melt viscosity [ƞ*] of ~104-105 poise is also suitable for LS. RTM385-SLS resin powder was mixed with 20-25% of hexagonal boron nitride (h-BN) and subjected to LS to print out “Green” specimens which could be further post-cured to afford a thermally conductive but electrically insulating composites with high T g of 385 °C. The cured composite specimens were then subjected to mechanical testing, thermal conductivity and porosity measurements as well as SEM characterization.

additive Manufacturing↗

Understanding the Space Weathering of Mercury Through Laboratory Experiments

Introduction: Airless surfaces across the solar system are continually modified by energetic particles from solar wind and micrometeoroid bombardment [1,2]. This process is known as space weathering, and it alters the chemical, microstructural, and optical properties of surface regoliths on airless bodies, including Mercury. On the Moon and S-type asteroids, the reflectance spectral signatures of space weathering include reddening (increasing reflectance with increasing wavelength), darkening (lowering of reflectance), and the attenuation of characteristic absorption bands [2]. Such spectral changes are driven by the production of Fe-bearing nanoparticles(npFe) through both solar wind irradiation and micrometeoroid bombardment. While our understanding of space weathering for the Moon and near-Earth S-types asteroids is advanced, insight into how these processes operate on other planetary bodies is limited. In particular, Mercury experiences a uniquely intense space weathering environment than planetary counterparts at 1 AU, including a moreintense solar wind flux and higher velocity micrometeoroid impacts [4]. Additionally, Mercury has a surface composition unique in the inner solar system, including regions of the surface with very low albedo known as the low reflectance material (LRM), which is enriched in carbon, likely graphite, up to 4wt.% [5].In addition, the concentration of Fe across Mercury’s surface islow (<2 wt.%) compared to the Moonor S-type asteroids asteroids[6]. Our understanding of the effects of space weathering on C-rich and Fe-poor phases is limited. Since Fe plays a critical role inthe development of space weathering characteristicson other airless surfaces(e.g., npFe), its limited availability may significantly affect the development of space weathering features in Mercury surface materials. We can simulate space weathering processes in the laboratory to explore their effects on the microstructural, chemical, and spectral characteristics of Mercury surface materials[7]. Here we used pulsed laser irradiation to simulate the short duration, high-temperature events associated with micrometeoroid impacts. We performed coordinated analyses including reflectance spectroscopy and electron microscopy to investigate the spectral, chemical, and microstructural changes in these mercurian analog samples. Methods: For these experiments, we usedforsteritic olivine with varying FeOcontents, a mineral phase proposed to be abundant on the surface of Mercury. We mixed each sample with graphite to simulate LRM regions of the surface. Wesynthesized the olivinesamplesat 1-bar at NASA’s Johnson Space Centerand prepared pressed powder pellets for laser irradiation [8].We prepared three samples, each with a base layer of olivineto maintain structural integrity and topped witha surface layer containing the graphite-olivine mixture: 1) Sample SC-001 San Carlos olivine(Fo90.91),2)Sample F-S-002 with0.05 wt.% FeO olivine, and 3) F-T-004 with 0.53 wt.% FeO olivine. Each sample was mixed with 5 wt.% powdered graphite and had grain sizes ranging from 45to 125μm. We irradiated each sample usinga pulsed Nd-YAG laser, (l=1064 nm, ~6 ns pulse duration, energy of 48 mJ/pulse) while undervacuumat Northern Arizona University. The laser was rastered1x and then 5x over the surfaceof each sample to simulate progressive space weathering. We collected in situreflectance spectra from the samples after each laser pulse witha Nicolet IS50 Fourier-Transform Infrared spectrometer (lfrom 0.65-2.5 μm). We used an FEI Nova NanoSEM200scanning electron microscope (SEM) and a Hitachi TM4000 Plus benchtop SEM at Purdue University to image the surface morphology and topography of the samples. We extracted thin sections for analysis in the transmission electron microscope(TEM)using the FEI Helios NanoLab 660 focused ion beam (FIB) SEM at the University of Arizona.We performed analysis of the microstructural and chemical characteristics of the samples using the 200 keV JEOL 2500 scanning TEM at Johnson Space Center. Reflectance Spectroscopy Results:Reflectance spectra for each sample are shown in Fig. 1.SC-001:The spectrum of the unirradiated sample exhibits a weak 1.0 μm absorption feature, associated with Fe2+in the olivine,and low overall reflectance (Fig. 1a). Thereflectance and the depth of the absorption band increases after 1x laser raster but are at their lowest after 5x laser rasters.F-T-004:The unirradiated sample has a blue-sloped spectrum with low reflectance without identifiable absorption features (Fig. 1b). With progressive laser irradiation, the sample reflectance increases and becomes strongly red-sloped.F-S-002:The unirradiated sample exhibits a dark, blue-slopedspectrum. The brightness of the sample increases significantly from <0.2average reflectance over >0.8 reflectance in the most irradiated sampleand thespectral slope also becomesslightly reddened (Fig. 1c). Microstructural and Chemical Analysis: Two primary alteration textures were observed in the samples exposed to simulated space weathering: 1) fluffy C-rich,and 2) vesiculated melt. The fluffy C-rich texture is composed oflow-densitydeposits distributed across the surface of the sample(Fig. 2A). Analysis of a FIB section extracted from a low-density C-rich region in sample SC-001 reveals multiple globule-type deposits, discrete from stacked graphite, likely produced via melting from the laser irradiation [9].The vesiculated melt textureis smooth and uniformly distributed across isolated regions of the sample surface. The vesicles measure up to 100s of nmin diameter. Analysis of a FIB section from this texture was extracted from sample F-T-004 reveals a layer of amorphous melt material, close to 100 nm thick and uniform across the FIB section (Fig. 2B). Isolated regions of this melt layer contain small nanoparticles, <5 nm in diameter. Chemical analysis through energy dispersive X-ray spectroscopy reveals the composition of this layer is enriched in Si and depleted in Mg and O compared to the underlying sample. Implications for Space Weathering on Mercury: Previous experiments simulating space weathering of Mercury have showndarkening and reddening of spectra[7,10].However, our use of low-Fe materials and graphite to create a sample set more analogous to the mercurian surface. Our results indicate that sample composition plays a significant and important role in the space weathering of Mercury. In particular, our spectral data demonstrates a strong correlation between spectral slope, Fe content, and simulated space weathering. While the variation in FeO content between samples F-S-002 and F-T-004 is <0.6 wt.%, the spectra deviate from flat to strongly red-sloped(F-T-004). This reddeningmay be linked to the presence of very small nanoparticles observed in the melt textures extracted from sample F-T-004. For the SC-001 sample, the fluffy C-rich textures may be developed by the amalgamation of small graphite particles into these unique morphologies. Such observations indicate that space weathering on Mercury may result in both familiar and new microstructural and chemical characteristics. References: [1]Hapke B. (2001) J. Geophys. Res.-Planet.,106,10039–10073. [2]Pieters C.M. and Noble S.K. (2016) J. Geophys. Res-Planet., 121, 1865–1884. [3] Lucey P.G., and Riner, M.A. (2011) Icarus,212, 451-462.[4]CintalaM.J.(1992)J. Geophys. Res.-Planet.,97,947–973.[5]Klima R.L.et al.(2018)Geophys.Res.Letters, 45, 2945–2953. [6]Nittler L.R., et al. (2011) Science 333, 1847-1850.[7]Sasaki S. and Kurahashi E. (2004) Space weathering on Mercury, Adv.Space Res., 33, 2152-2155.[8] Vander KaadenK.E., et al. (2018) LPSCXLIX, Abstract 1230. [9] McGlaun M.L. et al. (2019) LPSCL, Abstract 2019. [10] TrangD.et al. (2018)LPSCXLIX,Abstract2083

M S Thompson↗