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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 271 records · Page 15

Light-Dependent Impedance Spectra and Transient Photoconductivity in a Ruddlesden–Popper 2D Lead–Halide Perovskite Revealed by Electrical Scanned Probe Microscopy and Accompanying Theory

Electric force microscopy was used to record the light-dependent impedance spectrum and the probe transient photoconductivity of a film of butylammonium lead iodide, BA 2 PbI 4 , a 2D Ruddlesden–Popper perovskite semiconductor. The impedance spectrum of BA 2 PbI 4 showed modest changes as the illumination intensity was varied up to 1400 mW cm –2 , in contrast with the comparatively dramatic changes seen for 3D lead–halide perovskites under similar conditions. BA 2 PbI 4 ’s light-induced conductivity had a rise time and decay time of ~100 μs, 10 4 slower than expected from direct electron–hole recombination yet 10 5 faster than the conductivity-recovery times recently observed in 3D lead–halide perovskites and attributed to the relaxation of photogenerated vacancies. What sample properties are probed by electric force microscope measurements remains an open question. A Lagrangian-mechanics treatment of the electric force microscope experiment was recently introduced by Dwyer, Harrell, and Marohn which enabled the calculation of steady-state electric force microscope signals in terms of a complex sample impedance. Here this impedance treatment of the tip–sample interaction is extended, through the introduction of a time-dependent transfer function, to include time-resolved electrical scanned probe measurements. Here, it is shown that the signal in a phase-kick electric force microscope experiment, and therefore also the signal in a time-resolved electrostatic force microscope experiment, can be written explicitly in terms of the sample’s time-dependent resistance (i.e., conductivity).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Critical instability at moving keyhole tip generates porosity in laser melting

Laser powder bed fusion is a dominant metal 3D printing technology. However, porosity defects remain a challenge for fatigue-sensitive applications. Some porosity is associated with deep and narrow vapor depressions called keyholes, which occur under high-power, low–scan speed laser melting conditions. High-speed x-ray imaging enables operando observation of the detailed formation process of pores in Ti-6Al-4V caused by a critical instability at the keyhole tip. We found that the boundary of the keyhole porosity regime in power-velocity space is sharp and smooth, varying only slightly between the bare plate and powder bed. The critical keyhole instability generates acoustic waves in the melt pool that provide additional yet vital driving force for the pores near the keyhole tip to move away from the keyhole and become trapped as defects.

47 OTHER INSTRUMENTATION↗

In-situ X-ray scattering study of isotactic polypropylene/graphene nanocomposites under shear during fused deposition modeling 3D printing

Complementary techniques were applied to characterize the structure property relationships of FDM printed isotactic polypropylene/graphene nanocomposites. Raman spectroscopy indicated that graphene was mostly exfoliated during the nozzle extrusion process. Rheological measurements of the viscosity indicated that the presence of graphene induced shear thinning during extrusion. Azimuthal scans of wide angle x-ray scattering indicate correlated thermal fluctuations of the graphene platelets which stops abruptly at the onset of transcrystallization, or templating of the iPP chains on the graphene. X-ray microbeam SAXS analysis show the formation of ‘shish-kebab’ structures at the core of the unfilled filaments, where the ‘kebab’ component vanishes at the fiber-fiber interface enabling interdiffusion. Weak lamellar structure, and a corresponding decrease in the storage modulus are observed with the addition of 5% graphene. The lamellar structure disappears entirely with the addition of 10% graphene, while the storage modulus is decreased by nearly 50%. Thermal imaging of heat flux dissipation across molded and printed samples shows no orientational effects in pure iPP despite differences in crystal structure. Thermal conductivity increases dramatically in the samples with 10% graphene, and strong orientational effects are observed where the thermal coefficients differ by 180% between samples printed parallel or perpendicular to the heat flux.

36 MATERIALS SCIENCE↗

Investigation of Scanning Droplet Cell Technology for Electrochemical Deposition of Custom Three-Dimensional Alloys

The goal of this project was to assess the feasibility of a new method of electroplating, which we have termed “electroprinting”, for fabricating millimeter to centimeter metal parts with full density, and eventually, with bespoke 3D internal density patterns. Alloys, gradients and varying density is beyond the scope of this work, and efforts were focused on developing the technology to be capable of printing solid parts, beyond the lines and columns previously reported in the literature. Enabling this technology would expand the design space possible for the WPD program, allowing for smooth and complex density gradients in parts rather than discrete density steps between multilayers. We successfully designed and built an electroprinting apparatus, capable of printing copper in customizable 1-D patterns, which can be printed in stacked layers to form 3D parts. We successfully characterized the flat printed patterns, however, have encountered difficulty in characterizing multilayer prints. We have partially addressed the feasibility question, by developing the method for electroprinting 3D parts, however, some questions about the internal porosity and density of these parts still remain.

36 MATERIALS SCIENCE↗

Dispersion curve regression – assisted wideband local wavenumber analysis for characterizing three-dimensional (3D) profile of hidden corrosion damage

Corrosion as common damage in civil, petrochemical, nuclear, and aerospace structures affects the integrity and safety of the structures and may lead to catastrophic failures. This paper presents dispersion curve regression-assisted local wavenumber analysis method, which can analyze the time–space wavefield containing wideband information of wave-damage interaction and further extract the structural information carried by such wavefield for characterizing hidden corrosion damage in an isotropic plate. To acquire the time–space wavefield, a noncontact scanning laser Doppler vibrometer is used. In our analysis method, the acquired time–space wavefield is firstly processed to generate a local wavenumber function. The derived wavenumber function is further analyzed with a dispersion curve regression step, which searches in a set of theoretical frequency-wavenumber dispersion curves for different plate thicknesses and identifies the optimal plate thickness whose theoretical curve best matches the frequency-wavenumber relation contained in the local wavenumber function. By this means, a 3D profile including both in plane and thickness dimensions of the structure can be constructed for corrosion visualization and quantification. The experimental study demonstrates that our method can quantify the profile of hidden uniform corrosion in metal plates in terms of its in-plane shape and size as well as its out-of-plane depth in the subwavelength scale. Moreover, compared to previous Lamb wave-based corrosion inspection methods, our technique allows for noncontact 3D characterization of hidden corrosion from a far distance to the structure. Finally, we believe this work will inspire new 3D damage quantification methods that are based on wavefield analysis as well as enable potential applications for the quantification of hidden corrosion in civil, petrochemical, nuclear, and aerospace structures.

42 ENGINEERING↗

Additive manufacturing of high‐density silicon carbide ceramics through post‐processing spark plasma sintering

This research advances the field of additive manufacturing (AM) of silicon carbide (SiC) ceramics by integrating spark plasma sintering (SPS) to enhance material density, mechanical strength, and thermal properties. Traditional AM techniques struggle to achieve the high‐density SiC required for demanding applications, such as aerospace engineering, where high thermal conductivity and mechanical strength are paramount. Here, our study addresses these challenges by incorporating SPS as a post‐processing step, achieving near‐theoretical maximum densities and significantly reducing porosity, thereby resulting in outstanding thermal conductivity in SiC ceramics. We developed a specialized SiC ink optimized for 3D printing, ensuring structural integrity after deposition through tailored rheological properties. The application of SPS facilitates rapid, uniform sintering, essential for attaining superior density, mechanical properties, and thermal performance. Our experimental results, confirmed through scanning electron microscopy analysis, demonstrate significant microstructural properties, mechanical strength, and thermal conductivity, showcasing the effectiveness of integrating SPS in AM processes. This innovative approach not only expands the capabilities of AM in producing complex, high‐density ceramic structures but also broadens the potential applications of SiC in demanding environments.

36 MATERIALS SCIENCE↗

High-Energy X-ray Diffraction Microscopy for Nuclear Forensics (FY23 Project Report)

Morphological information on nuclear material has been identified using visible light and scanning electron microscopy. These identify qualitative differences in particle morphology. Three-dimensional imaging of materials through alternating scanning electron microscopy imaging and focused ion beam milling has also been used. Unfortunately, these techniques are time- and labor-intensive, with significant sample preparation required and lengthy analysis times. Further, the resulting 3D images are qualitative, require manual identification, and do not capture statistically-representative populations. High energy X-ray 3D imaging using a direct-beam or diffracted-beam (High-Energy Diffraction Microscopy) have been developed at the Advanced Photon Source and can produce quantitative information on grains (phase, location, etc.) and pores (size distribution, sphericity) in a material. These techniques require only minutes to characterize a sample volume and are non-destructive, thus suitable for a wide range of existing samples and for confirmatory analyses to be carried out using conventional microscopy techniques.

36 MATERIALS SCIENCE↗

Kirigami Engineering—Nanoscale Structures Exhibiting a Range of Controllable 3D Configurations

Abstract Kirigami structures provide a promising approach to transform flat films into 3D complex structures that are difficult to achieve by conventional fabrication approaches. By designing the cutting geometry, it is shown that distinct buckling‐induced out‐of‐plane configurations can be obtained, separated by a sharp transition characterized by a critical geometric dimension of the structures. In situ electron microscopy experiments reveal the effect of the ratio between the in‐plane cut size and film thickness on out‐of‐plane configurations. Moreover, geometrically nonlinear finite element analyses (FEA) accurately predict the out‐of‐plane modes measured experimentally, their transition as a function of cut geometry, and provide the stress–strain response of the kirigami structures. The combined computational–experimental approach and results reported here represent a step forward in the characterization of thin films experiencing buckling‐induced out‐of‐plane shape transformations and provide a path to control 3D configurations of micro‐ and nanoscale buckling‐induced kirigami structures. The out‐of‐plane configurations promise great utility in the creation of micro‐ and nanoscale systems that can harness such structural behavior, such as optical scanning micromirrors, novel actuators, and nanorobotics. This work is of particular significance as the kirigami dimensions approach the sub‐micrometer scale which is challenging to achieve with conventional micro‐electromechanical system technologies.

Zhang, Xu↗

Absence of a Dirac gap in ferromagnetic Cr x (Bi 0.1 Sb 0.9 ) 2-x Te 3

Magnetism breaks the time-reversal symmetry expected to open a Dirac gap in 3D topological insulators that consequently leads to the quantum anomalous Hall effect. The most common approach of inducing a ferromagnetic state is by doping magnetic 3d elements into the bulk of 3D topological insulators. In Cr 0.15 (Bi 0.1 Sb 0.9 ) 1.85 Te 3 , the material where the quantum anomalous Hall effect was initially discovered at temperatures much lower than the ferromagnetic transition, T C , the scanning tunneling microscopy studies have reported a large Dirac gap of ~20–100 meV. The discrepancy between the low temperature of quantum anomalous Hall effect (< C ) and large spectroscopic Dirac gaps (>>T C ) found in magnetic topological insulators remains puzzling. Here, we used angle-resolved photoemission spectroscopy to study the surface electronic structure of the pristine and potassium doped surface of Cr 0.15 (Bi 0.1 Sb 0.9 ) 1.85 Te 3 . Upon potassium deposition, the p-type surface state of the pristine sample was turned into an n-type, allowing the spectroscopic observation of Dirac point. Finally, we find a gapless surface state, with no evidence of a large Dirac gap reported in tunneling studies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

High-speed quantitative X-ray multi-contrast imaging with deep learning based modulated pattern analysis

The advent of X-ray multi-contrast imaging methods, providing absorption, phase, and dark-field images, holds tremendous promise for complementary and non-destructive visualization of inner structures within materials and bio-samples. However, the low efficiency in measuring and analyzing X-ray modulated patterns has hindered their application in high-resolution in situ imaging. In this work, the Enhanced Scanning Pattern-based Imaging Neural Network (ESPINNet) is introduced as a powerful tool for achieving high-speed, high-resolution quantitative imaging. ESPINNet is faster than correlation-based speckle tracking methods such as XSVT and UMPA, and provides a balanced performance in terms of resolution and speed for data collection by using fewer scanning images. In comparison with our previously developed neural network, ESPINNet introduces the capability to generate dark-field images, further enhancing its versatility. By leveraging scanning patterns, ESPINNet significantly improves resolution and measurement precision. Furthermore, its adaptability to various modulation patterns, including those produced by sandpaper, coded masks, or gratings, ensures broad applicability. These features enable real-time 2D and 3D multi-contrast imaging, positioning ESPINNet as a transformative solution for applications in materials science and biomedical research, particularly for high-speed and in situ measurements.

X-ray at-wavelength metrology↗

Effect of 3D-printed surface textures on wear mechanism in 3-body abrasion of soil

This study systematically investigates the enhancement of wear resistance in 3D printed surface textures through both experimental and theoretical approaches. Three distinct surface morphologies (Smooth Surface, Surface with uniformly distributed Pits, and Surface with uniformly distributed Bumps) were fabricated using High-Impact Polystyrene, where the meso-scale textures were precisely controlled through the 3D printing process. Wear behavior was evaluated using a 3-body wear tester in an abrasive particle environment, analyzing the influence of surface textures under various operating conditions. Systematic wear tests revealed that optimally designed surface textures achieved a remarkable 77 % reduction in wear compared to the worst-performing sample. The wear mechanisms were comprehensively characterized through weight loss measurements, Scanning Electron Microscopy (SEM), and Energy Dispersive Spectroscopy (EDS) analyses, elucidating the surface morphology changes and their interaction with wear particles. Notably, the study identified how the geometric characteristics of surface textures influence the movement of wear particles and the distribution of contact stresses. Discrete element method simulations corroborated the experimental findings, providing theoretical validation for the enhanced wear resistance of the optimal structure. The high correlation between simulated wear patterns and experimental results validates the reliability of the proposed design methodology. In conclusion, these results demonstrate that 3D printed surface texturing offers a cost-effective and scalable approach to significantly improve wear resistance in engineering applications, presenting a practical alternative to conventional, high-cost surface engineering methods.

3-body abrasion↗

Software Architecture and Hardware Organization in Mu2e Solenoid Field Mapping System

Herein, the Mu2e field mapping system is designed to produce high accuracy field maps of the detector solenoid used in the experiment. The data acquisition system is mobile and uses a self-propelled mapper with rotating arms equipped with 3D Hall probes. The measurements require not only accurate magnetic field readouts, but also accurate locations of all Hall probes while measuring data. The latter is accomplished by using the laser tracker to measure positions of several retroreflectors on the field mapper during data acquisition. The measurement process requires scanning the whole space inside the large solenoid and takes many hours to complete, which necessitates its full automation. The automation software includes control of the mapper, readout of Hall and NMR probes and control of a laser tracker, including prediction of retroreflector positions and execution of quality control checks. The software architecture and data acquisition hardware of the field mapping system are described, with special attention given to control of the laser tracker and its integration with the rest of the system.

3d hall probes↗

3D Printing of Polyelectrolyte Complex-Integrated Photocurable Hydrogel Resins

In this study, we developed a photocurable hydrogel resin incorporating a polyelectrolyte complex (PEC) for 3D printing. Acrylamide-based monomers were formulated with varying PEC contents (0–15 wt %) in an aqueous KBr medium to fabricate patterned porous hydrogel structures. The morphology of printed hydrogels was characterized by field-emission scanning electron microscopy and energy-dispersive X-ray spectroscopy. Notably, the PEC5 and PEC10 formulations exhibited optimal thermal stability and compressive properties, attributed to the homogeneous distribution of PEC domains within the hydrogel matrix. Furthermore, dye adsorption experiments demonstrated excellent removal efficiency, highlighting the potential of PEC-containing hydrogels for environmental remediation applications, particularly in the treatment of dye-contaminated wastewater.

Yang, Jinchul [University of Tennesse Knoxville]↗

Development of NDE/NDT Tools for High-Volume & High-Speed Inspection of CFRP Structures in Automotive Manufacturing

Main advantages of the air-coupled ultrasound testing (ACUT) and electromagnetic testing (EMT) techniques for NDE of CFRP composites were non-contact sensing, scalability for high-speed inspection, cost-effectiveness, and non-hazardous operation. Despite these advantages, no systems that would satisfy the project requirements were commercially available. Hence, one of the major efforts of the Michigan State University (MSU) team at the initial stage of the project was to close this technological gap by developing, optimizing, and validating array sensors that would provide sufficient sensitivity, spatial coverage, and resolution for robust defect detection. Optimization of the ACUT and EMT sensor designs was performed using experimentally validated finite element models. Initial experiments using array probes were conducted on relatively flat CFRP samples. In parallel, the MSU team designed and assembled a portable platform with two robotic arms. The robots were equipped with newly designed sensors that enabled high-speed NDE of curved CFRP parts. Presently, the developed robotic platform can be used as a demo/template NDE system, which is easily adaptable to manufacturing environments and in-line NDE. The ACUT NDE system developed by the MSU team used a high-power 4-channel pulser receiver for parallel data acquisition. The array probes were designed by stacking commercially available ACUT transducers, which operated in the frequency range between 100 kHz and 500 kHz. MSU optimized the excitation procedure and developed wave focusing cones so as to reduce the crosstalk between the transducers and to provide higher pulse repletion frequency (PRF). The through-transmission (TT) and single-side access (SSA) inspection modes were successfully implemented. In the TT-ACUT, structural defects in CFRP were detected by passing ultrasonic waves through the test part. Hence, the ACUT transmitters and receivers needed to be placed on the opposite sides of the test part. In the SSA-ACUT, guided waves (GW) were excited in the test part using the transmitters and were sensed by the receivers from the same side. Multi-channel TT-ACUT and SSA-ACUT provided high-speed NDE, and were successfully validated on CFRP test samples with interlaminar delaminations and other embedded defects The EM techniques developed by the MSU team included: 1) eddy current testing (ECT), 2) capacitive imaging (CI) and hybrid dual-mode imaging. In ECT, structural damage was detected in CFRP using coils sensor arrays. In ECT, the excitation magnetic field is generated by passing an alternating current through a coil, which is placed above the test sample. The excitation field penetrates the conductive sample and induces the eddy currents in its transect. In turn, the eddy currents generate the reaction field, which affects the total field sensed by a coil. Hence, the presence of structural flaws will alter the eddy current flow and the picked-up signal. ECT is mostly sensitive to local changes of the electric conductivity of the test sample, and CFRPs are mostly conductive in the direction of carbon fibers. Hence, ECT was well suited for the detection of fiber damage/fiber irregularities. The MSU team developed printed circuit boards (PCB) with coil sensor arrays optimized for NDE of CFRP. Unlike most commercial probes designed for ECT of metallic structures, the MSU array probes were designed for operation in [1-10] MHz frequency range, which was optimal for low-conductive CFRP. Multiple sensing topologies (coil groups excitation/sensing arrangements) were implemented and successfully validated. Capacitive Imaging (CI) technique developed by MSU was complementary to ECT. In contrast to ECT, which was sensitive to local changes of the electrical conductivity, the CI was sensitive to local changes of the dielectric constant. Therefore, CI could provide information about matrix damage/matrix irregularities in CFRP. The MSU CI sensor arrays were made of multiple circular or rectangular open-plate capacitors printed on PCB. Sensors of this type are not commercially available. In addition to ECT and CI, the MSU team developed a hybrid (dual-mode) inductive/capacitive measurement technique that synergistically combined the benefits of inductive and capacitive sensing for rapid NDE of fiber reinforced polymer (FRP) composite structures. Fiber damage and fiber irregularities in FRPs were detected by configuring hybrid sensors as coil sensors. Similarly, matrix damage, matrix irregularities and interlaminar delaminations were detected by configuring hybrid sensors as capacitive sensors. ECT and CI were performed sequentially by means of electronic switching. Hence, eliminating the need for mounting two separate sensor arrays on the probe. Portable robotic platform was developed by MSU for multi-technique high-speed NDE of CFRP test parts. The platform had two 6-axis robots, which enabled inspection of curved parts in approximately a 6×6×6 ft 3 active scan area. On the software side, the MSU team integrated scripts for NDE hardware control with scripts for robot motion control. MSU also implemented automated path planning for the robots, reconstruction of part’s surfaces via stereovision, 3D rendering of inspection data, and image processing algorithms for enhanced defect detection. Automotive composite parts manufactured by Plasan Composites from Phase I were used to validate the ACUT and EMT techniques on representative testbeds. Among those parts were three X-braces for a Dodge Viper, one composite calibration plaque with known defects at known locations, and four other test sections, including sections from a front splitter, a corner section from a composite hood, and a high-pressure RTM panel made using non crimp fabric. Other test samples included CFRP and GFRP calibration plates with fiber/matrix defects fabricated at MSU/CVRC.

36 MATERIALS SCIENCE↗

Direct Optoelectronic Imaging of 2D Semiconductor–3D Metal Buried Interfaces

The semiconductor-metal junction is one of the most critical factors for high performance electronic devices. In two-dimensional (2D) semiconductor devices, minimizing voltage drop at this junction is of particularly challenging and important. Despite numerous studies on contact resistance in 2D semiconductors, the exact nature of the buried interface under a 3D metal remains elusive and unclear. Herein, we report the direct observation of 2D semiconductor-metal buried interface using recently developed metal-assisted transfer technique to expose the buried interface which is then directly investigated using scanning probe techniques. We characterize the spatially varying electronic and optical properties of this buried interface with < 20 nm resolution. To be specific, potential, conductance and photoluminescence at the buried metal/MoS 2 interface are correlated under variety of metal deposition conditions as well as type of metal contacts. We observe that direct evaporation of Au on MoS 2 induces large strain of ~5% in the MoS 2 which coupled with charge transfer leads to degenerate doping of the MoS 2 underneath the contact. These factors lead to improvement of contact resistance to record values of 138 kΩ μm measured using local conductance probes. This approach was adopted to investigate MoS 2 -In/Au alloy interface, which records lowest contact resistance of 63 kΩ μm. Overall, our results highlight that the MoS 2 /Metal interface is very sensitive to method of contact making and provides a universal strategy to characterize buried contact interfaces involving 2D semiconductors.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Diffraction enhanced imaging utilizing a laser produced x-ray source

Image formation by Fresnel diffraction utilizes both absorption and phase-contrast to measure electron density profiles. The low spatial and spectral coherence requirements allow the technique to be performed with a laser-produced x-ray source coupled with a narrow slit. This makes it an excellent candidate for probing interfaces between materials at extreme conditions, which can only be generated at large-scale laser or pulsed power facilities. Here, we present the results from a proof-of-principle experiment demonstrating an effective ~2 μm laser-generated source at the OMEGA Laser Facility. This was achieved using slits of 1 × 30 μm 2 and 2 × 40 μm 2 geometry, which were milled into 30 μm thick Ta plates. Combining these slits with a vanadium He-like 5.2 keV source created a 1D imaging system capable of micrometer-scale resolution. The principal obstacles to achieving an effective 1 μm source are the slit tilt and taper—where the use of a tapered slit is necessary to increase the alignment tolerance. We demonstrate an effective source size by imaging a 2 ± 0.2 μm radius tungsten wire.

3D printing↗

Wafer-scale waveguide sidewall roughness scattering loss characterization by image processing

Photonic integrated circuits (PICs) are vital for developing affordable, high-performance optoelectronic devices that can be manufactured at an industrial scale, driving innovation and efficiency in various applications. Optical loss of modes in thin film waveguides and devices is a critical measure of their performance. Thin film growth, lithography, masking, and etching processes are imperfect processes that introduce significant sidewall and top-surface roughness and cause dominating optical losses in waveguides and photonic structures. This roughness, as perturbations couple light from guided to far-field radiation modes, leads to scattering losses that can be estimated from theoretical models. Typically, with UV-based lithography, sidewall roughness is significantly larger than wafer-top surface roughness. Atomic force microscopy (AFM) imaging measurement gives a 3D and high-resolution roughness profile, but the measurement is inconvenient, costly, and unscalable for large-scale PICs and at wafer-scale. Here, we evaluate the sidewall roughness profile based on 2D high-resolution scanning electron microscope (SEM) imaging. We characterized the loss on two homemade nitride and oxide films on 3-inch silicon wafers with 12 waveguide devices on each and correlated the scattering loss estimated from a 2D image-based sidewall profile and theoretical Payne model. The lowest loss of guided fundamental transverse electric (TE 0 ) mode is found at 0.075 dB/cm at 633 nm across 24 devices, a record at visible wavelength. Our work shows 100% success (edge continuity span exceeding 95% of image width/height) in edge detection in image processing of all images to estimate autocorrelation function and optical mode loss. These demonstrations offer valuable insights into waveguide sidewall roughness and a comparison of experimental and 2D SEM image processing based loss estimations with applications in loss characterization at wafer-scale PICs.

Khurana, Mohit (ORCID:0000000207898672)↗