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DOE OSTI2022

Temporal and spatial laser intensification within nodular defects overcoated with multilayer dielectric mirrors over a wide range of defect geometries

The nodular defect shape and the laser incidence angle have a dramatic impact on the spatial distribution of light intensification within the nodule as well as how the laser light is drained from the defect. Nodular defect geometries unique to ion beam sputtering, ion-assisted deposition, and electron-beam (e-beam) deposition, respectively, are modeled in this parametric study over a wide range of nodular inclusion diameters and layer count for optical interference mirror coatings constructed with quarter-wave thicknesses and capped with a half wave of the low index material. It was found for hafnia ($n$=1.9) and silica ($n$=1.45) multilayer mirrors that the light intensification in nodular defects with a $C$ factor of 8, typical of e-beam deposited coatings deposited with a wide range of deposition angles, was maximized for a 24-layer design. For intermediate size inclusion diameters, increasing the layer count for normal incidence multilayer mirrors reduced the light intensification within the nodular defect. A second parametric study explored the impact of the nodule shape on the light intensification for a fixed number of layers. In this case, there is a strong temporal trend for the different nodule shapes. Narrow nodules tend to drain more laser energy through the bottom of the nodule into the substrate while wide nodules tend to drain more laser energy through the top of the nodule when irradiated at normal incidence. Further, at a 45° incidence angle, waveguiding is an additional method to drain laser energy from the nodular defect. Finally, laser light resonates within nodular defects longer than within the adjacent nondefective multilayer structure.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

Utilization of Ultrasonication as a Method of Reducing Organic and Inorganic Contamination in Post‐Consumer Plastic Film Waste

Post-consumer plastic film waste often carries organic and inorganic contaminants that challenge recycling processes and affect the quality of recycled products. An effective contaminant removal procedure through washing such single-used plastic films (SUPFs) can address environmental and waste management concerns. This study compares the efficiency of different washing techniques in reducing SUPF contamination. To evaluate the efficacy of each washing technique, film samples collected from material recovery facilities are individually exposed to friction, ultrasonic-assisted, and a combination of both washes. Thermal analysis indicates that the polymers' melting temperature, crystallization temperature, and crystallinity remain unaffected by the washing methods, demonstrating method aptness. Confocal laser scanning microscope images show that washing results in a cleaner sample surface. 91% ash reduction during the combined wash treatment indicates a high method efficiency compared to the individual friction and ultrasonic wash procedures. This is further validated by reducing characteristic contaminant IR bands (3600–3000, 1750–1600, and 1100–1000 cm −1 ). Elements of concern such as Cd, Cr, Hg, and Pb in SUPFs after each washing technique applied conform with regulations (<100 ppm) for packaging products. This research shows the novel ultrasonic washing reduces more contamination than friction with shorter wash times and no surfactants.

42 ENGINEERING↗

DOE OSTI2022

Report summarizing demonstration of thermal conductivity measurement methods for coated zirconium cladding

Thermal diffusivity measurements on Zirconium-based cladding materials have historically been a challenge due to the difficulty to measure on specimens with curved geometries, including nuclear grade Zircaloy cladding materials. In this work, we first used Laser Flash Analysis methods to measure the thermal diffusivity of Zircaloy tubes, which show good agreement with Zircaloy plates in this work, as well as previously published data. The consistent results proved the applicability of the Laser Flash Analysis setup for investigating thermal diffusivity of Zircaloy tubes. We further investigate the hydrogen effect on thermal diffusivity of Zircaloy tubes. Hydrogen plays significant roles in temperature dependent thermal diffusivity trends of Zircaloy tube. For low hydrogen concentration, where hydride dissolved into single phase α-Zr at higher temperature, thermal diffusivity is relatively unchanged at low temperature at two phase regions (α-Zr and δ-hydride), and it increases as a function of temperature at single phase α-Zr region. For high hydrogen concentration, where phase transformation (α-Zr + δ-hydride → α-Zr + β-Zr) occurs at 567 °C, thermal diffusivity decreases as a function of temperature below 567 °C before the transformation (α-Zr and δ-hydride), while increase at higher temperature after the transformation (α-Zr and β-Zr).

36 MATERIALS SCIENCE↗

DOE OSTI2023

Nanosecond Laser Drying in Wafer Foundries for Significant Energy Efficiency Improvement

Surface drying is a critical process in microelectronics wafer fabrication. In order to reduce and eliminate watermarks, many surface drying processes have been studied and used. Most of the wafer foundries currently use drying processes based on Isopropyl Alcohol (IPA), which causes serious safety (fire), health, environmental, and energy efficiency issues. The long-term goal of this project is to develop a fast, effective, chemical-free, and extremely energy efficient wafer drying technology that employs nanosecond laser-induced sub-surface evaporation and explosion. The objectives of this project are to 1) experimentally develop and verify the laser surface drying method, explore and identify how and to what extent various physical parameters influence the drying efficiency and effectiveness; and 2) understand and optimize the underlying thermodynamics in the proposed laser surface drying, including micro/nanoscale sub-surface superheating, evaporation, explosion, and photo/thermochemical bond breaking via atomistic modeling and experimental characterization. Toward these objectives, five tasks have been accomplished successfully, including 1) develop in-lab laser surface drying setup and study the effect of varied laser parameters, 2) use multiscale hybrid-modeling to study and understand the physics of water behavior during drying toward process optimization, 3) investigate the effect of drying conditions on the drying effectiveness, 4) develop a large-scale laser drying scanning system with automatic scanning, and 5) conduct large-scale simulation to study the effect of dopant level and develop strategies for system development toward industry deployment.

42 ENGINEERING↗

DOE OSTI2021

Femtosecond Laser Desorption Postionization MS vs ToF-SIMS Imaging for Uncovering Biomarkers Buried in Geological Samples

The study of lipid molecular fossils by traditional biomarker analysis requires bulk sample crushing, followed by solvent extraction, and then the analysis of the extract by gas chromatography-mass spectrometry (GC–MS). This traditional analysis mixes all organic compounds in the sample regardless of their origins, with a loss of information on the spatial distribution of organic molecules within the sample. These shortcomings can be overcome using the chemical mapping of intact samples. Spectroscopic techniques such as UV fluorescence or Raman spectroscopy, laser ablation inductively coupled plasma mass spectrometry, and time-of-flight secondary ion mass spectrometry (ToF-SIMS) are among those elemental and molecular mapping techniques. This study employed femtosecond (fs) laser ablation combined with single-photon ionization, a method called fs-laser desorption postionization mass spectrometry (fs-LDPI-MS). In this work, a pulsed ~75 fs, 800 nm laser was used to ablate the geological sample, which was then photoionized after a few microseconds by a pulsed 7.9 eV vacuum ultraviolet laser. An organic carbon-rich geological sample was used for this study to map hydrocarbon biomarkers in sediments that were previously studied by GC–MS. The petrography of this sample was examined by optical and fluorescence microscopy. It is demonstrated here that fs-LDPI-MS combined with petrography for multimodal imaging can expose buried compounds within the sample via in situ layer removal. When used in conjunction with traditional organic geochemical analysis, this method has the potential to determine the spatial distribution of organic biomarkers in geological material. Finally, fs-LDPI-MS imaging data are compared with ToF-SIMS imaging that is commonly used for such studies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Uncovering Uranium Isotopic Heterogeneity of Fuel Pellets from the Fifth Collaborative Materials Exercise of the Nuclear Forensics International Technical Working Group

In 2017, the Nuclear Forensics International Technical Working Group (ITWG) organized their fifth 37 Collaborative Materials Exercise (CMX-5). The exercise samples were two uranium dioxide fuel pellets 38 manufactured from the same starting materials by different processes to have similar bulk isotopic 39 composition, but different spatial uranium isotopic distributions. Sets of identical materials were sent to 40 all participating laboratories, who then utilized their existing nuclear forensic capabilities to 41 independently analyse fuel pellets and identify similarities and differences of the materials’ 42 characteristics. The analytical methods used to probe the fuel pellets included ex situ, such as sectioning 43 or breaking up the pellets and analyzing dissolved pieces using inductively coupled plasma mass 44 spectrometry (ICP-MS), analyzing particles collected from intact or fragmented pellets by secondary ion 45 mass spectrometry (SIMS), as well as in situ methods, such as laser ablation coupled with ICP-MS, 46 autoradiography and nanoSIMS. In this paper we present the results of these independent analyses and 47 compare the capabilities of those nuclear forensic analytical methods to uncover details of the isotopic 48 heterogeneity of uranium fuel pellets.

Nuclear Forensic Analysis of Uranium Fuel Pellets,↗

DOE OSTI2024

Microfluidic film evaporation with femtosecond laser-patterned surface

Systems, apparatuses, and methods for microfluidic fluid evaporation using femtosecond laser-patterned surfaces are disclosed. A microfluidic device may comprise a femtosecond laser-patterned substrate having at least one input path and at least one output path. The femtosecond laser-patterned substrate may comprise both superhydrophobic and superhydrophilic sections. Fluid deposited at an input path may be wicked to an output path due to the surface pattern. A heating device may be provided to heat the fluid to evaporate volatiles therefrom. Vacuums and gas streams may be used to aid in volatile removal. Gas streams may add gas to the microfluidic device to react with the fluid.

Pearson, Connor Daniel↗

DOE OSTI2025

Versatile system for ion energy measurements generated by pulsed laser ionization: Insights into electron-ion dynamics

Ion energy distributions generated by pulsed laser interactions with materials are essential for applications ranging from materials science to oncology. Ion energy characterization is particularly important for an emerging mass spectrometry technique called virtual-slit cycloidal mass spectrometry (VS-CMS). The ion energy distribution influences the design and performance of VS-CMS instruments, as well as the efficacy of laser-driven ionization methods in various fields. Several established techniques, including the retarding potential method, time-of-flight (TOF) analysis, and electrostatic energy analyzers, have been employed to measure ion energy distributions. The wide range of ion energies reported highlights the strong dependence of ion energy on laser parameters, target materials, and experimental conditions, as well as the necessity of making independent measurements of the ion energy distribution for specific laser systems and materials. This paper presents the design and characterization of a simple TOF-based apparatus for measuring ion energy distributions from pulsed laser ionization without external fields. This approach minimizes perturbation of electron-ion dynamics and enables simultaneous energy measurements at multiple spatial positions. Here, the apparatus was tested using a nanosecond pulsed Nd:YAG laser operating at 1064 nm, 532 nm, and 266 nm on solid copper sheets at various laser fluences. Simultaneous measurements at different distances provide new insights into ion-electron interactions post-ionization and demonstrate the influence of laser wavelength and fluence on ion energy distributions.

Ion energy↗

DOE OSTI2025

Remote detection of radioactive material using a short-pulse CO 2 laser

Detection of radioactive material at distances greater than the radiated particle range is an important goal with applications in areas such as national defense and disaster response. Here, we demonstrate avalanche-breakdown-based remote detection of a 3.6 mCi α-particle source at a standoff distance of 10 m, using 70 ps, long-wave infrared (λ = 9.2 µm) CO 2 laser pulses. This is ∼10 times longer than our previous results using a mid-IR laser. The primary detection method is direct backscatter from microplasmas generated in the laser focal volume. The backscatter signal is amplified as it propagates back through the CO 2 laser chain, enhancing sensitivity by >100 times. Here we also characterize breakdown plasmas with fluorescence imaging, and present a simple model to estimate backscattered signals as a function of the seed density profile in the laser focal volume. All of this is achieved with a relatively long-drive laser focal geometry (f/200) that is readily scalable to >100 m.

43 PARTICLE ACCELERATORS↗

DOE OSTI2022

System and method for determining absolute carrier-envelope phase of ultrashort laser pulses

A system for determining an absolute carrier-envelope phase (CEP) of ultrashort laser pulses includes a laser system for generating a laser beam including ultrashort optical pulses of a duration of less than 10 fs, an ultrabroadband quarter-wave plate configured to polarize the laser beam, and a gas jet emitting a continuous jet stream into the laser beam. The system includes focusing optics to adjust a focal spot of the laser beam to the gas jet, and a detector arrangement including a beam block and a microchannel plate (MCP) imaging detector, wherein the laser beam is directed to the detector arrangement. The method involves using angular streaking to determine the absolute CEP of both elliptically and linearly polarized light.

Li, Wen↗

DOE OSTI2024

Viability of Miniature Discs in LFA-427

Miniature disc samples pose challenging measuring conditions for laser flash analysis. With reductions in signal from lower radiosity and lower half-rise times from low thicknesses, optimal selections of coatings and laser parameters are critical in a successful measurement. This report explains the methodology in successfully measuring two different material types—metals and ceramics—in proper coating selection, laser parameters, and post analysis for each material, as well as applying it to un-irradiated uranium samples of each type (U-metal, UO 2 ). This was done through a combination of analysis techniques combining automatic commercial methods (Neztech) and manual methods for correcting laser pulse impact aberrations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Method for Rapid Modeling of Distortion in Laser Powder Bed Fusion Metal Additive Manufacturing Parts

The simulation and modeling of part-level distortion and residual stress in diverse metal additive manufacturing (AM) geometries has great potential to enable the rapid adoption of this technology in engineering design. Moreover, the use of additive manufacturing component libraries (CLs) offer a computationally efficient means of quantifying these part-level defects resultant from AM processing. We report on how the individual simulations of simple shapes, potential entries in a CL, can be superimposed to provide an indication of distortion and residual stresses in complex geometries. Laser powder bed fusion AM was used to construct test geometries of varied shapes and their combinations in the form of CLs in an effort to characterize location-dependent and feature-dependent distortion distributions. Blue light scanning was used to experimentally measure 3D distortions in order to investigate the interaction between the component shapes and local boundary conditions. Overall, part-level distortions were highly dependent on test component geometry, local boundary conditions, and shape combination. Commercial finite element software was used to verify experimental trends and to make predictions of distortion. The use of CLs resulted in over 20 times savings in computational cost while reproducing overall trends in distortion for test geometry assemblies. Therefore, it is anticipated that the use of CLs for L-PBF AM geometries has demonstrated potential to facilitate efficient simulations of full component AM assemblies, thereby reducing the need for costly trial-and-error-type experimental analysis.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Methods for 2-color radiography with laser-compton X-ray sources

High-contrast, subtraction, x-ray images of an object are produced via scanned illumination by a laser-Compton x-ray source. The spectral-angle correlation of the laser-Compton scattering process and a specially designed aperture and/or detector are utilized to produce/record a narrow beam of x-rays whose spectral content consists of an on-axis region of high-energy x-rays surrounded by a region of slightly lower-energy x-rays. The end point energy of the laser-Compton source is set so that the high-energy x-ray region contains photons that are above the k-shell absorption edge (k-edge) of a specific contrast agent or specific material within the object to be imaged while the outer region consists of photons whose energy is below the k-edge of the same contrast agent or specific material. Scanning the illumination and of the object by this beam will simultaneously record and map the above edge and below k-edge absorption response of the object.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2025

Quantification and prediction of solidification textures under additive manufacturing conditions

Crystallographic textures are a major determinant of the macroscale anisotropic properties of polycrystalline metallic alloys produced in a wide range of additive manufacturing (AM) processes. Here, we introduce a statistical method that can accurately quantify the degree of orientational order of textures despite the large random fluctuations in the orientation of individual grains inherent in AM processes. The method, demonstrated for laser and resolidification of AlSi thin films, extends Z-scoring to a dynamical regime to assess the statistical significance of observed textures compared to randomly generated ones at different stages of solidification. We further show that, combined with phase-field modeling, this method can be used to infer fundamental anisotropic properties of the solid-liquid interface that are essential for texture prediction, and are compared here to the results of atomistic simulations. In addition, phase-field modeling reveals that, even at rapid AM solidification rates, the observed 〈110〉-dominated textures in the AlSi thin films are controlled predominantly by the anisotropy of the interface free-energy and sheds light on the physical mechanism of grain competition. These results significantly enhance both the existing tools for the quantification and prediction of AM crystallographic textures and our basic understanding of their formation.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Laser Doppler vibrometry for piezoelectric coefficient ($d_{33}$) measurements in irradiated aluminum nitride

Sensors used for experiments in advanced reactors must survive in harsh environments. Few material systems can be used to construct sensors viable for extreme conditions. Aluminum nitride (AlN) is one such material because it has high thermal stability and radiation resistance and sustains good piezoelectric and dielectric properties at high temperatures. In this work, the piezoelectric coefficient $d_{33}$ of the AlN single-crystal with thermal and irradiation damage was investigated using an indirect method with a laser Doppler vibrometer (LDV). Surface electrodes were deposited on the AlN samples, and the vibration response of the samples to an applied voltage was monitored using the LDV as a function of the excitation frequency. The $d_{33}$ estimation was based on the excitation voltage and the thickness-mode displacement extracted from the LDV measurements. Further, six AlN substrates were irradiated with 8 MeV Al 2+ at three fluences (10 15 , 10 16 , and 10 17 ions/cm 2 ) and two temperatures (300 °C and 500 °C). The $d_{33}$ for the six irradiated samples and one pristine sample were measured, and the measurement uncertainty was estimated based on five repeated tests. All samples were also measured by a commercial piezometer for comparison. The experimental results demonstrate that the piezoelectric coefficients obtained by LDV were about 0.8–1.16 pm/V lower than those obtained by the piezometer. With the compensation of the clamping effect, the corrected LDV values are similar to the piezometer results. Both show similar trends in all samples, which validates the feasibility of the proposed method for $d_{33}$ measurement. Based on the LDV results, the irradiated samples show a 12%–22% decrease in $d_{33}$ compared with the pristine samples. The samples irradiated under the same fluence at a higher temperature (500 °C) demonstrated a lower $d_{33}$ than those at 300 °C. The effect of the retro-reflective tape, sample temperature, and sample size on the $d_{33}$ measurement were also studied.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Nuclear Structural Component Relevant Properties of Nickel-Based Alloys Produced via Additive Manufacturing

Idaho National Laboratory initiated examination of nickel-based alloys manufactured via three different additive manufacturing methods for potential applications in nuclear, high temperature structural components. The three methods analyzed included laser powder bed fusion, blown powder laser directed energy deposition, and wire-fed gas metal arc directed energy deposition. With the rapid push towards additive manufacturing, codes do not exist that definitively define what is or is not tolerable for each process and application, such as with conventional, wrought products. This report contains the initial work to understand possible manufacturing methods for high temperature alloys, and specifically, void formation, microstructure evolution, corrosion, and mechanical properties. To generate mechanical test data, specimens were tested irrespective of voids and microstructures were analyzed to better understand how to negate/improve these issues. The preliminary results showed major decreases in mechanical performance for material tested. Test specimens will continue to be produced to further improve each additive manufacturing processes, quantify void acceptance, and better understand the most suitable high temperature alloys receptive to additive manufacturing and high temperature nuclear applications.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Determination of nonradiative carrier lifetimes in quantum well laser diodes from subthreshold characteristics

A method for determination of non-radiative carrier lifetimes in the waveguide and active regions of quantum well laser diodes is presented. This method is suitable for characterization of fully packaged devices and requires no special measurement equipment if the device structure is known. Furthermore, the proposed approach is experimentally demonstrated for several 800 nm laser diodes.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2021

Laser pre-sintering for denudation reduction in the laser powder bed fusion additive manufacturing of Ti-6Al-4V alloy

As a fundamentally different process for creation of complex parts, laser powder bed fusion (LPBF) additive manufacturing exhibits complex behavior at the melt pool that has a direct influence on the macroscopic properties of the final material. Powder denudation, a previously studied deleterious phenomenon, is the displacement of powder due to entrainment in a jet of rapidly vaporized metal created by the process laser. To minimize the effect of denudation and inspired by methods in adjacent fields, a laser pre-sintering (LPS) method was studied in an effort to reduce denudation. LPS was found to be most effective in the 1–4 J/mm3 volumetric energy density processing regimes, minimizing the common experimentally observed problems with the LPBF process. Scanning electron microscopy of the LPS-treated powder bed revealed insight into the accelerating effect morphological irregularities along the powder particle surface have in the pre-sintering process. To further understand the process, an estimation of the sintered neck sizes necessary to eliminate denudation in LPS is made, qualitatively affirming the low energy densities needed to prevent denudation. Here, the results presented in this work represent an initial step towards understanding and implementing LPS as a quality-enhancing step in LPBF.

36 MATERIALS SCIENCE↗