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DOE OSTI2025

Advancing microelectronics through nanoscale science: A perspective on needs and opportunities from the nanoscale science research centers

Microelectronics are the cornerstone of the modern world, enhancing our daily lives by providing services such as communications and datacenters. These resources are accessible thanks to the continual pursuit of a deeper understanding of the chemical and physical phenomena underlying the materials synthesis approaches and fabrication processes used to create microelectronic components and subsequently the components' responses to electrical, optical, and other stimuli that are utilized within microelectronic systems. Today, further development of microelectronics requires multidisciplinary expertise across scientific disciplines and fields of study—synthesis, materials characterization, nanoscale fabrication, and performance characterization—with focus placed on comprehending the nanoscale forms and features of microelectronic components. The Nanoscale Science Research Centers (NSRCs) are Department of Energy, Office of Science user facilities that support the international scientific community in advancing nanoscale science and technology. As a key component of the U.S. Government's National Nanotechnology Initiative, the NSRCs enable transformative discoveries by providing world-class facilities, expertise, and collaborative opportunities. Here, in this perspective, we showcase a non-exhaustive cross-section of the capabilities housed at and developed by the NSRCs and their user communities to address fundamental synthesis, metrology, fabrication, and performance considerations toward advancing the development of new microelectronics. Finally, we provide a timely outlook on the next major areas of necessary development in nanoscale sciences to continue the innovation of microelectronics into the next generation.

2D materials↗

DOE OSTI2025

Sample glue layer investigation and mitigation for laser induced prompt impulse experiments

Understanding longer timescale material reactions under dynamic stress loading is critical for applications in materials engineering, shock physics, and planetary science. Prompt impulse experiments generate lower pressures since the ablator—the material first removed by the laser—is thicker and farther from the diagnostic plane, capturing aggregate material responses from the initial shock wave, rarefaction waves, and later time effects. This complexity demands thorough material characterization and simulation support. Since traditional sample construction is specific to supported shock experiments, designing prompt impulse experiments requires reconsideration around target design and sample engineering. Here, we present sample preparation techniques, experimental investigations, and theoretical simulations to investigate glue layer impacts, aiming to standardize samples for consistent data at lower laser fluences. We find that glue layers <30 μm have a minimal impact on peak velocity and pulse shape. The peak velocity scales linearly with glue layer thickness until a glue layer of 75 μm. For glue layers >75 μm, the peak velocity no longer scales with thickness; however, the pulse shape continues to degrade as described by simulations.

Lasers↗

DOE OSTI2025

Investigation of the distribution of laser-induced damage precursors in etched grating sidewalls fabricated using inductively coupled plasma reactive-ion etching

Inductively coupled plasma reactive-ion etching for grating fabrication is explored with emphasis on the type and distribution of process-induced defects that can act as precursors to laser-induced damage initiation. To provide flexibility in the ability to perform a variety of material characterization methods, grating-like features with large pitch were fabricated in silica monolayers. The results indicate that the etch process introduces surface fluorine and subsurface carbon-containing contamination, which reduces the laser-induced damage threshold. The local relative concentrations of the laser-damage precursors introduced during the etch step of the manufacturing process were investigated using angle-resolved damage testing, taking advantage of the shift of the location of the peak electric-field intensity incident on the grating sidewall. The results suggest an increased level of etch-related defects near the base of the sidewall, with directly fluorinated silicon identified as the primary defect.

Dent, R. [Univ. of Rochester, NY (United States). ↗

NASA NTRSDate not supplied

Assessing Degradation of Advanced Coatings for Carbon/Carbon Composites

Carbon/carbon (C/C) composites are a well-utilized material system for hot structures to enable hypersonic flight. However, C/C materials are susceptible to attack by environmental degradation mechanisms, notably oxidation, which can limit the durability of components resulting in premature failure. Environmental barrier coatings (EBCs) have been developed to mitigate deleterious oxidation. Coating compositions based on silicon carbide (SiC) offer promise as a protective coating material for C/C composites. Under particular hypersonic flight conditions, a passivating silica scale can form at the surface of the EBC, acting as a barrier that can protect the underlying coating and substrate. However, the transition from passive to active oxidation, which varies with temperature and pressure, causes the formation of gaseous SiO that volatilizes leading to detrimental consumption of the SiC coating. In this work, arc-jet testing of SiC-based coatings developed to protect Advanced C/C-6 (ACC-6) was performed under a range of conditions to replicate varying oxidation conditions. In-situ optical emission spectroscopic measurements of the gas-surface interactions were collected and evaluated to render compositional degradation of the coating and underlying composite during arc-jet testing. Specimens were evaluated before, during and after arc-jet testing using destructive and non-destructive materials characterization methods, including optical and scanning electron microscopy and energy dispersive spectroscopy.

Coatings, Hypersonics, Composites↗

NASA NTRSDate not supplied

The Two-Cavity Method for Characterizing Acoustical Materials—an Interlaboratory Study

This study focuses on understanding the sound absorption characteristics of porous acoustic materials, which are determined by two key parameters independent of material thickness: characteristic impedance and propagation constant. These parameters can be characterized by testing a porous sample concept in a normal incidence impedance tube using either the two-thickness or the two-cavity method. In the two-thickness method, two samples of varying thicknesses are required. In contrast, the two-cavity method requires testing one sample at two different air cavity depths behind the porous material. This method is particularly advantageous for materials that are costly or challenging to fabricate. This interlaboratory study evaluates the variability of characteristic properties determined using the two-cavity method. Porous acoustic materials were additively manufactured and tested in the Liner Technology Facility(LTF)at NASA Langley Research Center and the Mechanics, Acoustics and Dynamics Lab (MADLab) at Michigan Technological University. The characteristic properties derived from various cavity depth combinations were used to predict the surface impedance of the sample with a rigid backing. The prediction was then compared the measured impedance spectrum. It was also found that the combinations of cavity depths can significantly influence the accuracy of the deduced properties.

acoustic liners↗

NASA NTRSDate not supplied

The Two-Cavity Method for Characterizing Acoustical Materials--an Interlaboratory Study

Explore the source record for details and available documents.

acoustics↗

NASA NTRS1978

A new experimental method for the accelerated characterization of composite materials

A method which permits the prediction of long-term properties of graphite/epoxy laminates on the basis of short-term (15 min) laboratory tests is described. Demonstration of delayed viscoelastic fracture in one laminate configuration, and data on the time and temperature response of a matrix-dominated unidirectional laminate contributed to a characterization of the viscoelastic process in the graphite/epoxy composites. Master curves from short-term tests of certain laminate configurations can be employed to generate long-term master curves. In addition, analytical predictions from short-term results can be used to predict long-term (25-hour) laminate properties.

Brinson, H. F.↗

DOE OSTI2024

STUDIES ON PIPELINE POLYETHYLENES IN HYDROGEN GAS ENVIRONMENTS USING IN-SITU AND EX-SITU CHARACTERIZATION METHODS

Polymeric materials are commonplace in the natural gas infrastructure as distribution pipes, coatings, seals, and gaskets. Under the auspices of the U.S. Department of Energy HyBlend program, one of the means to reduce greenhouse gas emissions is with replacing natural gas, either partially or completely, with hydrogen. This approach makes it imperative that we conduct near-term and long-term materials compatibility research in these relevant environments. Insights into the effects of hydrogen and hydrogen gas blends on polymer integrity can be gained through both ex-situ and in-situ analytical methods. Our work represented here highlights a study of the behavior of pipeline polyethylene (PE) materials, including HDPE (Dow 2490 and GDB50) and MDPE (Ineos and legacy Dupont Aldyl A), when exposed to hydrogen by means of in-situ X-ray scattering and ex-situ Raman spectroscopy techniques. Samples were tested in ex-situ hydrogen and argon gas environments and in-situ hydrogen environments to identify differences due to permeation and solubility of these gases. These methods complemented each other because Raman spectroscopy could capture permanent effects after materials were removed from gaseous environments, and in-situ X-ray scattering analysis collected real-time data to elucidate the impact of the gas environment on polymer microstructure. Data collected revealed that the aforementioned polymers did not show significant changes in crystallinity and microstructure under the exposure conditions tested. Our findings from these studies will help establish real-time effects caused by hydrogen gas transport through pipeline polyethylenes by way of its influence on polymer structure and chemistry, which is directly related to pipeline mechanical strength and longevity of service.

Hydrogen materials compatibility, Natural gas pipe↗

DOE OSTI2025

Invariant discovery of features across multiple length scales: Applications in microscopy and autonomous materials characterization

Physical imaging is a foundational characterization method in areas from condensed matter physics and chemistry to astronomy and spans length scales from atomic to universe. Images encapsulate crucial data regarding atomic bonding, materials microstructures, and dynamic phenomena such as microstructural evolution and turbulence, among other phenomena. The challenge lies in effectively extracting and interpreting this information. Variational Autoencoders (VAEs) have emerged as powerful tools for identifying the underlying factors of variation in image data, providing a systematic approach to distilling meaningful patterns from complex data sets. However, a significant hurdle in their application is the definition and selection of appropriate descriptors reflecting local structures. Here, we introduce the scale-invariant VAE approach (SI-VAE) based on the progressive training of the VAE with the descriptors sampled at different length scales. The SI-VAE allows the discovery of the length scale-dependent factors of variation in the system. Here, we illustrate this approach using the ferroelectric domain images and generalize it to the movies of the electron-beam induced phenomena in graphene and topography evolution across combinatorial libraries. This approach can further be used to initialize the decision making in automated experiments including structure–property discovery and can be applied across a broad range of imaging methods. This approach is universal and can be applied to any spatially resolved data including both experimental imaging studies and simulations, and can be particularly useful for exploration of phenomena such as turbulence and scale-invariant transformation fronts.

36 MATERIALS SCIENCE↗

NASA NTRS2009

Metal Standards for Waveguide Characterization of Materials

Rectangular-waveguide inserts that are made of non-ferromagnetic metals and are sized and shaped to function as notch filters have been conceived as reference standards for use in the rectangular- waveguide method of characterizing materials with respect to such constitutive electromagnetic properties as permittivity and permeability. Such standards are needed for determining the accuracy of measurements used in the method, as described below. In this method, a specimen of a material to be characterized is cut to a prescribed size and shape and inserted in a rectangular- waveguide test fixture, wherein the specimen is irradiated with a known source signal and detectors are used to measure the signals reflected by, and transmitted through, the specimen. Scattering parameters [also known as "S" parameters (S11, S12, S21, and S22)] are computed from ratios between the transmitted and reflected signals and the source signal. Then the permeability and permittivity of the specimen material are derived from the scattering parameters. Theoretically, the technique for calculating the permeability and permittivity from the scattering parameters is exact, but the accuracy of the results depends on the accuracy of the measurements from which the scattering parameters are obtained. To determine whether the measurements are accurate, it is necessary to perform comparable measurements on reference standards, which are essentially specimens that have known scattering parameters. To be most useful, reference standards should provide the full range of scattering-parameter values that can be obtained from material specimens. Specifically, measurements of the backscattering parameter (S11) from no reflection to total reflection and of the forward-transmission parameter (S21) from no transmission to total transmission are needed. A reference standard that functions as a notch (band-stop) filter can satisfy this need because as the signal frequency is varied across the frequency range for which the filter is designed, the scattering parameters vary over the ranges of values between the extremes of total reflection and total transmission. A notch-filter reference standard in the form of a rectangular-waveguide insert that has a size and shape similar to that of a material specimen is advantageous because the measurement configuration used for the reference standard can be the same as that for a material specimen. Typically a specimen is a block of material that fills a waveguide cross-section but occupies only a small fraction of the length of the waveguide. A reference standard of the present type (see figure) is a metal block that fills part of a waveguide cross section and contains a slot, the long dimension of which can be chosen to tailor the notch frequency to a desired value. The scattering parameters and notch frequency can be estimated with high accuracy by use of commercially available electromagnetic-field-simulating software. The block can be fabricated to the requisite precision by wire electrical-discharge machining. In use, the accuracy of measurements is determined by comparison of (1) the scattering parameters calculated from the measurements with (2) the scattering parameters calculated by the aforementioned software.

Lambert, Kevin M.↗

DOE OSTI2026

A Review of Advanced Characterization Methods and Techniques for Amorphous and Poorly Crystalline Materials Applicable to Cementitious Waste Forms

This review covers advanced characterization methods of cementitious materials. The particular focus is to understand cementitious compositions with amorphous content because conventional techniques such as X-ray diffraction are more applicable to materials with long range order. Also of interest is advanced characterization that provides deeper insights into properties such as porosity. There are five groups of characterization methods discussed in this review which are: electron beam/microscopy, X-ray, neutron diffraction and scattering, nuclear magnetic resonance, and optical techniques. The techniques can be further grouped by the categories of nanoscale structural understanding (transmission electron microscopy and pair distribution function), microscale structural understanding (focused ion beam and x-ray tomography), microscopic elemental distributions (energy dispersive spectroscopy and X-ray fluorescence), and chemical binding information (electron energy loss spectroscopy, x-ray absorption spectroscopy, nuclear magnetic resonance, Raman spectroscopy, and infrared spectroscopy), with advantages and disadvantages of each method discussed. The recommendation for further research is to begin with techniques that are easier to prepare samples for, measure, and analyze, such as the optical techniques of Raman and infrared spectroscopy. If more information is needed, pursue collaborations, other techniques, or proposals for beam time at the synchrotron sources.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS2005

Assessment of Technologies for the Space Shuttle External Tank Thermal Protection System and Recommendations for Technology Improvement - Part III: Material Property Characterization, Analysis, and Test Methods

The objective of this report is to contribute to the independent assessment of the Space Shuttle External Tank Foam Material. This report specifically addresses material modeling, characterization testing, data reduction methods, and data pedigree. A brief description of the External Tank foam materials, locations, and standard failure modes is provided to develop suitable background information. A review of mechanics based analysis methods from the open literature is used to provide an assessment of the state-of-the-art in material modeling of closed cell foams. Further, this report assesses the existing material property database and investigates sources of material property variability. The report presents identified deficiencies in testing methods and procedures, recommendations for additional testing as required, identification of near-term improvements that should be pursued, and long-term capabilities or enhancements that should be developed.

Gates, Thomas S.↗

NASA NTRS2003

On the Use of Accelerated Test Methods for Characterization of Advanced Composite Materials

A rational approach to the problem of accelerated testing for material characterization of advanced polymer matrix composites is discussed. The experimental and analytical methods provided should be viewed as a set of tools useful in the screening of material systems for long-term engineering properties in aerospace applications. Consideration is given to long-term exposure in extreme environments that include elevated temperature, reduced temperature, moisture, oxygen, and mechanical load. Analytical formulations useful for predictive models that are based on the principles of time-based superposition are presented. The need for reproducible mechanisms, indicator properties, and real-time data are outlined as well as the methodologies for determining specific aging mechanisms.

Gates, Thomas S.↗

NASA NTRS1992

Method of characterizing residual stress in ferromagnetic materials using a pulse histogram of acoustic emission signals

The invention is a method and apparatus for characterizing residual uniaxial stress in a ferromagnetic test member by distinguishing between residual stresses resulting from positive (tension) forces and negative (compression) forces by using the distinct and known magnetoacoustic (MAC) and a magnetoacoustic emission (MAE) measurement circuit means. A switch permits the selective operation of the respective circuit means.

Namkung, Min↗

NASA NTRS2010

Effect of Microscopic Damage Events on Static and Ballistic Impact Strength of Triaxial Braid Composites

The reliability of impact simulations for aircraft components made with triaxial-braided carbon-fiber composites is currently limited by inadequate material property data and lack of validated material models for analysis. Methods to characterize the material properties used in the analytical models from a systematically obtained set of test data are also lacking. A macroscopic finite element based analytical model to analyze the impact response of these materials has been developed. The stiffness and strength properties utilized in the material model are obtained from a set of quasi-static in-plane tension, compression and shear coupon level tests. Full-field optical strain measurement techniques are applied in the testing, and the results are used to help in characterizing the model. The unit cell of the braided composite is modeled as a series of shell elements, where each element is modeled as a laminated composite. The braided architecture can thus be approximated within the analytical model. The transient dynamic finite element code LS-DYNA is utilized to conduct the finite element simulations, and an internal LS-DYNA constitutive model is utilized in the analysis. Methods to obtain the stiffness and strength properties required by the constitutive model from the available test data are developed. Simulations of quasi-static coupon tests and impact tests of a represented braided composite are conducted. Overall, the developed method shows promise, but improvements that are needed in test and analysis methods for better predictive capability are examined.

Littell, Justin D.↗

DOE OSTI2024

Progress in development of characterization capabilities to evaluate candidate materials for direct air capture applications

As part of U.S. national efforts to combat the detrimental effect of global climate change, the National Institute of Standards and Technology (NIST) was recently tasked to support efforts in direct air capture (DAC) of carbon dioxide research and deployment. In order to develop test procedures, materials, and documentary standards, key characterization methods relevant to DAC materials have been investigated and used to identify desirable properties for a potential Standard Reference Material (SRM). Select amine-supported materials that previously showed potential for DAC applications have been characterized using commonly available laboratory methods. Further insights into the adsorption characteristics have been gained from developing and applying more specialized characterization tools ideal for probing low concentrations of carbon dioxide. A broad suite of capabilities that examine relevant properties under appropriate conditions gives the most profound insights into a material's specific performance. We advocate for even more specialized capabilities to be developed and standardized to quantitatively monitor the interactions of CO 2 with molecular species in complex and often disordered systems to advance DAC and support carbon dioxide reduction (CDR) in general.

carbon dioxide↗

NASA NTRS2015

Method and Apparatus for Non-Destructive Evaluation of Materials

Methods and apparatus for characterizing composite materials for manufacturing quality assurance (QA), periodic inspection during the useful life, or for forensic analysis/material testing. System are provided that relate eddy-current sensor responses to the fiber layup of a composite structure, the presence of impact damage on a composite structure with or without a metal liner, volumetric stress within the composite, fiber tow density, and other NDE inspection requirements. Also provided are systems that determine electromagnetic material properties and material dimensions of composite materials from capacitive sensor inspection measurements. These properties are related to the presence of buried defects in non-conductive composite materials, moisture ingress, aging of the material due to service or environmental/thermal exposure, or changes in manufacturing quality.

Goldfine, Neil J.↗

NASA NTRS2017

Method and Apparatus for Non-Destructive Evaluation of Materials

Goldfine, Neil J.↗