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NASA NTRS1992

Long Duration Exposure Facility M0003-5 thermal control coatings on DoD flight experiment

The M0003-5 thermal control coatings and materials orbited on the LDEF M0003 Space Environment Effects on Spacecraft Materials were a part of a Wright Laboratories Materials Directorate larger experiment. They were selected from new materials which emerged from development programs during the 1978-1982 time frame. Included were materials described in the technical literature which were being considered or had been applied to satellites. Materials that had been exposed on previous satellite materials experiments were also included to provide data correlation with earlier space flight experiments. The objective was to determine the effect of the LDEF environment on the physical and optical properties of thermal control coatings and materials. One hundred and two specimens of various pigmented organic and inorganic coatings, metallized polymer thin films, optical solar reflectors, and mirrors were orbited on LDEF. The materials were exposed in four separate locations on the vehicle. The first set was exposed on the direct leading edge of the satellite. The second set was exposed on the direct trailing edge of the vehicle. The third and fourth sets were exposed in environmental exposure control canisters (EECC) located 30 degrees off normal to the leading and trailing edges. The purpose of the experiment was to understand the changes in the properties of materials before and after exposure to the space environment and to compare the changes with predictions based on laboratory experiments. The basic approach was to measure the optical and physical properties of materials before and after long-term exposure to a low earth orbital environment comprised of UV, VUV, electrons, protons, atomic oxygen, thermal cycling, vacuum, debris, and micrometeoroids. Due to the unanticipated extended orbital flight of LDEF, the thermal control coatings and materials in the direct leading and trailing edge were exposed for a full five years and ten months to the space environment and the canister materials were exposed for approximately one year to the full environment.

Hurley, Charles J.↗

DOE OSTI2021

Salivary Antibodies against Multiple Environmental Pathogens Found in Individuals Recreating at an Iowa Beach

Detecting environmental exposures and mitigating their impacts are growing global public health challenges. Antibody tests show great promise and have emerged as fundamental tools for large-scale exposure studies. Here, we apply, demonstrate and validate the utility of a salivary antibody multiplex immunoassay in measuring antibody prevalence and immunoconversions to six pathogens commonly found in the environment. The study aimed to assess waterborne infections in consenting beachgoers recreating at an Iowa riverine beach by measuring immunoglobulin G (IgG) antibodies against select pathogens in serially collected saliva samples. Results showed that nearly 80% of beachgoers had prior exposures to at least one of the targeted pathogens at the beginning of the study. Most of these exposures were to norovirus GI.1 (59.41%), norovirus GII.4 (58.79%) and Toxoplasma gondii (22.80%) and over half (56.28%) of beachgoers had evidence of previous exposure to multiple pathogens. Of individuals who returned samples for each collection period, 6.11% immunoconverted to one or more pathogens, largely to noroviruses (GI.1: 3.82% and GII.4: 2.29%) and T. gondii (1.53%). Outcomes of this effort illustrate that the multiplex immunoassay presented here serves as an effective tool for evaluating health risks by providing valuable information on the occurrence of known and emerging pathogens in population surveillance studies.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

Unraveling the Hsp70-ROS-autophagy axis in pentachlorophenol-challenged lung and liver epithelial cells

Pentachlorophenol (PCP) was extensively utilized as an organochlorine pesticide and wood preservative in the United States from the 1930s until the Environmental Protection Agency (EPA) imposed restrictions due to concerns about its toxicity and potential carcinogenic properties. Although it is no longer widely used, PCP remains a concern due to its environmental persistence and potential for long-term health effects. Significant occupational and environmental exposures have likely occurred, with the health and economic costs of PCP exposure potentially being substantial given its known toxicity. Notably, PCP exhibits rapid absorption through both the skin and respiratory system and has been shown to cause hepatotoxicity, developmental toxicity, immunotoxicity, irritation, and carcinogenicity in laboratory animal studies. PCP exposure induces oxidative stress, a key mechanism underlying its inflammatory and toxic effects, which can activate cellular stress responses including upregulation of heat shock protein 70 (Hsp70). Previous studies in lung and liver epithelial cells have shown that Hsp70 and oxidative stress play pivotal roles in triggering autophagy. This study establishes the critical role of the Hsp70-reactive oxygen species (ROS)-autophagy axis in regulating cellular responses to PCP exposure in human alveolar (A549) and liver carcinoma (HepG2) epithelial cells. Our research elucidated the molecular mechanisms underlying PCP's cellular effects, demonstrating that its exposure resulted in increased expression of autophagy-related proteins (Beclin-1, LC3B, ATG12, and ATG16), subunits of NADPH oxidase (NCF-1, NCF-2, NOX2, and Rac), and antioxidant proteins (SOD and GPx) in both lung and liver cell types. Notably, PCP augmented the interaction between Hsp70 and the autophagy regulator Beclin-1. Pretreatment with the ROS inhibitor N-acetylcysteine or Hsp70 knockdown markedly reversed PCP-induced responses. Our in-silico protein–protein docking analysis and molecular dynamics simulation studies revealed enhanced interactions and/or stable confirmations maintained throughout the simulations for TLR4-Hsp70 and Hsp70-Beclin-1 complexes in the presence of PCP. These findings provide a strong foundation for future studies, employing in vivo experimental models and human populations to identify promising targets for PCP-induced toxicity and cellular injury. As a result, these findings may have far-reaching implications for public health and environmental policy, ultimately leading to the identification of biomarkers and the development of more effective interventions for environmentally induced toxicity and diseases.

97 MATHEMATICS AND COMPUTING↗

NASA NTRS1992

Durability evaluation of photovoltaic blanket materials exposed on LDEF tray S1003

Several candidate protective coatings on Kapton and uncoated Kapton were exposed to the low Earth orbital (LEO) environment on the Long Duration Exposure Facility (LDEF) to determine if the coatings could be used to protect polymeric substrates from degradation in the LEO environment. The coatings that were evaluated were 700 A of aluminum oxide, 650 A of silicon dioxide, and 650 A of a 4 percent polytetrafluoroethylene-96 percent silicon dioxide mixed coating. All of the coatings evaluated were ion beam sputter deposited. These materials were exposed to a very low atomic oxygen fluence (4.8 x 10 exp 19 atoms/sq. cm) as a result of the experiment tray being located 98 degrees from the ram direction. As a result of the low atomic oxygen fluence, determination of a change in mass was not possible for any of the samples including the uncoated Kapton. There was no evidence of spalling of any of the coatings after the approximately 33,600 thermal cycles recorded for LDEF. The surface of the uncoated Kapton, however, did show evidence of grazing incidence texturing. There was a 7-8 percent increase in solar absorptance for the silicon dioxide and aluminum oxide coated Kapton and only a 4 percent increase for the mixed coating. It appears that the addition of a small amount of fluoropolymer may reduce the magnitude of absorptance increase due to environmental exposure. Thermal emittance did not change significantly for any of the exposed samples. Scanning electron microscopy revealed few micrometeoroid or debris impacts, but the impact sites found indicated that the extent of damage or cracking of the coating around the defect site did not extend beyond a factor of three of the impact crater diameter. This limiting of impact damage is of great significance for the durability of thin film coatings used for protection against the LEO environment.

Sharon K Rutledge↗

DOE OSTI2025

Comparison of measurement techniques and sorption of radium-226 in low and high salinity aqueous samples

Human activities have the potential to redistribute radium (Ra) in the marine environment in a manner that may necessitate monitoring or management of subsequent human or environmental exposures. There is therefore a need to identify accurate and accessible techniques for Ra measurement in high salinity samples and to describe the distribution of Ra in estuarine and marine environments, but most efforts in these areas have focused on low salinity matrices. In addition, rapid and reliable measurements are crucial for time-sensitive samples such as short-lived isotopes or emergency situations. The objective of this study is to describe the limits of detection, cost, and relative ease for measurement of Ra in both low and high salinity aqueous samples via three analytical methods: liquid scintillation counting (LSC), high purity germanium (HPGe) gamma spectrometry, and inductively coupled plasma mass spectrometry (ICP-MS). To contextualize these measurements for real-world scenarios, the partitioning of 226 Ra to substrates relevant to the marine environment was also characterized. Although HPGe detection with solid phase extraction had the lowest limit of detection for low salinity samples (0.27 Bq L −1 ), poor 226 Ra recovery for high salinity samples and high materials costs make this method prohibitive for many users. Limits of detection for high salinity samples were lower for LSC (1.28 Bq L −1 ) than for ICP-MS without dilution (11.4 Bq L −1 ), but significant and unexpected degradation of the high salinity LSC standards was observed after six months. Furthermore, our preferred measurement method for high salinity Ra samples is ICP-MS with sample dilution as necessary to reduce matrix effects.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2023

Probing Defects and Spin‐Phonon Coupling in CrSBr via Resonant Raman Scattering

Abstract Understanding the stability limitations and defect formation mechanisms in 2D magnets is essential for their utilization in spintronic and memory technologies. Here, defects in mono‐ to multilayer CrSBr are correlated with structural, vibrational, and magnetic properties. Resonant Raman scattering is used to reveal distinct vibrational defect signatures. In pristine CrSBr, it is shown that bromine atoms mediate vibrational interlayer coupling, allowing for distinguishing between surface and bulk defect modes. Environmental exposure is shown to cause drastic degradation in monolayers, with the formation of intralayer defects. This is in contrast to multilayers that predominantly show bromine surface defects. Through deliberate ion irradiation, the formation of defect modes is tuned: these are strongly polarized and resonantly enhanced, reflecting the quasi‐‐1D electronic character of CrSBr. Strikingly, pronounced signatures of spin‐phonon coupling of the intrinsic phonon modes and the ion beam‐induced defect modes are observed throughout the magnetic transition temperature. Overall, defect engineering of magnetic properties is possible, with resonant Raman spectroscopy serving as a direct fingerprint of magnetic phases and defects in CrSBr.

2D magnetic semiconductors↗

DOE OSTI2025

Transparent and Conductive Inorganic/Polymer‐Composite Encapsulants for Long‐Term Perovskite Solar Cells Operation

An innovative inorganic/polymer-composite encapsulation scheme comprising a polymer-based transparent conductive composite (TCC) coupled with a transparent conductive oxide is introduced to extend the lifetime of moisture-sensitive devices such as perovskite solar cells (PSC). The TCC comprises conductive silver-coated polymethyl methacrylate (Ag-PMMA) microsphere fillers protruding from a transparent non-conductive polymer matrix. TCC samples (5% Ag-PMMA by area) demonstrate high optical transparencies (%T approx. 85% in the 370–1200 nm region), low out-of-plane electrical resistivities (R < 0.2 Ω cm 2 ), and equilibrium permeabilities of less than 1 g mm/m 2 /day, all of which are well-maintained after 1,000 hours of environmental exposure. In practice, the TCC is employed between two indium zinc oxide (IZO) thin films, with the in-plane conductivity of IZO and the out-of-plane conductivity of TCC working collectively to function as a single encapsulating electrode. This encapsulation scheme is exemplified by benchmarking performances of PSCs subjected to accelerated aging conditions of quasi-maximum power point tracking under light soaking in air at 50 °C, 40% R.H. to 60% R.H. Notable improvements in operational lifetimes are observed, with a champion encapsulated PSC maintaining over 90% of its initial efficiency of 21.65% for up to 1,430 hours, compare to less than 300 hours for an unencapsulated control.

14 SOLAR ENERGY↗

DOE OSTI2021

Thirdhand cigarette smoke leads to age-dependent and persistent alterations in the cecal microbiome of mice

The gut microbiome composition is influenced by many factors including environmental exposures. Here, we investigated the effect of thirdhand cigarette smoke (THS) and exposure age on gut microbiome diversity. C57BL/6 mice were exposed to THS at human exposure relevant levels for three weeks during three different life stages: postnatal (0–3 weeks of age), pubescent (4–7 weeks of age), and adult (9–12 weeks of age), respectively. Cecal microbiome profiles were assessed at 17 weeks of age by 16S rRNA gene sequencing. We found that age at THS exposure strongly influenced the cecal microbiome composition. Although postnatal THS exposure significantly influenced the microbial composition, pubescent and adulthood exposures only had minor effects. The microbiome of postnatally THS-exposed mice significantly increased several degradation pathways that regulate glycolysis and pyruvate decarboxylation, and significantly decreased coenzyme A biosynthesis and pyrimidine deoxyribonucleoside salvage. Our results indicate that mouse postnatal development is particularly susceptible to persistent THS exposure effects on the gut microbiome.

16S rRNA gene sequencing↗

DOE OSTI2020

Linear viscoelastic characterization of electrically conductive adhesives used as interconnect in photovoltaic modules

Electrically conductive adhesives (ECAs) are incorporated into recent designs of photovoltaic (PV) modules and replace the traditional metallic solders as interconnects. This transition depicts a significant material change, and a proper understanding of the interconnects' mechanical response has not yet been established. However, such an understanding is necessary to (a) identify the driving forces for module degradation and failure, (b) allow for module design optimization, and (c) enable accurate lifetime predictions. This study summarizes the framework for the mechanical materials characterization and modeling of ECAs for PV applications. Only high-fidelity material models are able to capture the rate and temperature dependency of the ECA interconnect and allow for accurate modeling of the materials response. Furthermore, a linear viscoelastic representation is found to describe the mechanical response of the ECAs sufficiently well. The effects of curing conditions and environmental exposure are investigated, and material models for a variety of ECAs are reported and prepared for the use in numerical simulations. Overall, a finite element simulation of a generic submodel of a shingled cell module is used to highlight the need for high-fidelity material models and demonstrates the error made in the predicted stress states by using less sophisticated models.

14 SOLAR ENERGY↗

DOE OSTI2023

Biological toxicity and environmental hazards associated with PLGA nanoparticles

There have been tremendous advances in nanotechnology. More recently, the use of nanoparticles has expanded to applications including materials, packaging, energy, and medical uses such as drug delivery, diagnostics, and therapeutics. The American Society for Testing and Materials (ASTM) and the International Organization for Standardization (ISO) define nanoparticles as particles with at least one dimension measuring between 1 and 100 nm (2), but this view is generally too limited, and recommendations have been made to consider all materials with a dimension measuring under 1,000 nm as nanoparticles. The biomedical uses of nanoparticles are particularly promising because of their ability to reach and target various sites and organs. However, some nanoparticles can be composed of toxic materials or are limited by issues of biodistribution and bioaccumulation, which have hampered their use in biomedicine. The copolymer poly lactic-co-glycolic acid (PLGA) has gained use in biomedical applications as a delivery system because it is considered biocompatible and can be formulated with controlled degradation in physiological environments. PLGA has a history in biomedicine that dates to the 1970s when biodegradable sutures were developed using PLGA. In addition, the United States (US) Food and Drug Administration (FDA) and the European Medicine Agency (EMA) have approved various PLGA particle formulations as therapeutic delivery vehicles. Interest in biocompatible materials to deliver a range of therapeutic drugs, proteins, nucleic acids, and other molecules has risen recently. In addition to drug delivery, sustained drug release can be achieved by tuning the physical properties of PLGA, such as the molecular weight, ratio of lactic to glycolic acid, drug concentration, stabilizing molecules, and particle size. Given the rise of nanoparticles, human and environmental exposure to them is inevitable as more applications use free, unbound, and highly mobile particles. Although PLGA is generally considered safe, a detailed understanding of how PLGA and the other components used to help formulate this copolymer into a nanoparticle delivery vehicle is useful for assessing potential harmful effects. Despite recent advances in PLGA nanoparticle formulations, residual stabilizing molecules, inconsistent preparations, and batch-to-batch variations can lead to toxicity. Poor preparations of PLGA can lead to common mechanisms of toxicity observed with nanoparticles, such as inflammation and oxidative stress. Consistency in PLGA formulations and accurate methods to evaluate nanoparticle toxicity are needed to ensure safety. In order to better assess PLGA nanoparticles as non-toxic delivery systems, it is critical to understand their physical and chemical properties and the formulation protocols that may introduce toxic components into particles.

Biology, nanoparticle, toxicity↗

DOE OSTI2024

Predicting nutrition and environmental factors associated with female reproductive disorders using a knowledge graph and random forests

Female reproductive disorders (FRDs) are common health conditions that may present with significant symptoms. Diet and environment are potential areas for FRD interventions. We utilized a knowledge graph (KG) method to predict factors associated with common FRDs (for example, endometriosis, ovarian cyst, and uterine fibroids). We harmonized survey data from the Personalized Environment and Genes Study (PEGS) on internal and external environmental exposures and health conditions with biomedical ontology content. We merged the harmonized data and ontologies with supplemental nutrient and agricultural chemical data to create a KG. We analyzed the KG by embedding edges and applying a random forest for edge prediction to identify variables potentially associated with FRDs. We also conducted logistic regression analysis for comparison. Across 9765 PEGS respondents, the KG analysis resulted in 8535 significant or suggestive predicted links between FRDs and chemicals, phenotypes, and diseases. Amongst these links, 32 were exact matches when compared with the logistic regression results, including comorbidities, medications, foods, and occupational exposures. Mechanistic underpinnings of predicted links documented in the literature may support some of our findings. Our KG methods are useful for predicting possible associations in large, survey-based datasets with added information on directionality and magnitude of effect from logistic regression. These results should not be construed as causal but can support hypothesis generation. This investigation enabled the generation of hypotheses on a variety of potential links between FRDs and exposures. Future investigations should prospectively evaluate the variables hypothesized to impact FRDs.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2021

Morphological and chemical characteristics of oxide scales formed on δ-Phase plutonium metal alloys I: 3.5 at% ga

Focused ion-beam scanning electron microscopy (FIB-SEM) and three-dimensional (3D) microscopy were applied to characterize the subsurface morphological features of oxide scales formed on an ~3.5 at.% Ga plutonium (Pu) metal alloy. Using the FIB-SEM technique, a number of morphological features formed in the interior of the oxide scale from Pu metal's environmental exposure were observed and identified. Here, Auger electron spectroscopy (AES) was utilized to characterize the cross-sectional composition and chemistry of the oxide scale. The oxide scale formed during inert storage and operational environments has a characteristic internal scale structure that includes a relatively dense oxide layer with some lateral and transverse cracking. Generally, after subsequent exposure to dry air environment, the oxide scale retained most of the original structural and chemical characteristics. However, after aging in a moist air environment, while the oxide scale was found to maintain the chemical characteristics of the source oxide, the scale was found to be on average thinner and without the previously observed internal microcracking, likely the result of spallation of the source scale during exposure to the new environment.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Morphological and chemical characteristics of oxide scales formed on δ-phase plutonium metal alloys II: 2.0 at% Ga

The focused ion-beam scanning electron microscopy (FIB-SEM) and three-dimensional (3D) microscopy were applied to characterize the subsurface morphological features of oxide scales formed on an ~2.0 at. % Ga plutonium (Pu) metal alloy. Using the FIB-SEM technique, a number of morphological features formed in the interior of the oxide scale from Pu metal’s environmental exposure were observed and identified. Auger electron spectroscopy (AES) was utilized to characterize the cross-sectional composition and chemistry of the oxide scale. The oxide scale formed during inert storage and operational environments was found to be highly variable in thickness and morphology, presenting some regions with a thin (<400 nm), dense oxide layer and others with a thick (>2 µm) scale with substantial lateral cracking. After subsequent exposure to dry air environment, the oxide scale became thicker (~4 µm) and slightly more porous. The changes following aging in a moist air environment were observed to be more severe, with the formation of a highly porous internal structure containing significant lateral and transverse cracking. In comparison to the scale formed on an ~3.5 at. % Ga-Pu metal alloy, the oxide morphology of the lower gallium alloy investigated here exhibited greater variation in thickness and a noteworthy dependence on the presence of water vapor, particularly in terms of the internal porosity formed during growth of the oxide.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Predicting material microstructure evolution via data-driven machine learning

The recent rapid rise in data-driven practices in the materials science domain has led to the development of efficient, generalizable, and accurate approaches for several applications, including: material property prediction, mining (micro)structure- property and (micro)structure-processing relationships, and characterization of material microstructures. Central to the materials science domain is linking microstructure to properties and performance, and critical to building such linkages is understanding how microstructures evolve as a function of environmental exposure or processing conditions (e.g., time, temperature, applied stress or strain, irradiation). This preview article summarizes recent work on the development of recurrent neural networks for predicting spatio-temporal microstructure evolution detailed by Yang et al in their manuscript entitled 'Self-supervised Learning and Prediction of Microstructure Evolution with Recurrent Neural Networks'.

machine learning (ML), materials characterization↗

DOE OSTI2024

Investigation of inter-subject variation in ultrafine particle deposition across human nasal airways: A study involving children, adults, and the elderly

Occupational and environmental exposure to toxic nanoparticles, driven by the rapid expansion of nanotechnology, raises significant respiratory health concern. Numerous studies have explored airflow and particle dynamics in adult nasal airways, but understanding the impact of age-related anatomical changes in children and the elderly remains limited. This study systematically investigates age-related anatomical variations and associated influence on nasal airflow dynamics and ultrafine particle deposition characteristics. Using Computational Fluid-Particle Dynamics (CFPD) method, simulation was conducted under diverse inhalation conditions spanning a wide age range, including: two children (5 years old), two young adults (in their twenties), and two elderly (over 77 years old). Our results reveal distinctive variations across age groups in anatomical dimensions, which affect distribution of wall shear stress where the elderly and children display unique patterns distinct from the young adults. While total deposition efficiency differs significantly between children and adults, filtration efficiency in the subregion with most deposition, main respiratory, remains consistent. However, inter-subject differences are observed in the vestibular and olfactory regions,emphasizing nuanced impact of age-related anatomical variations. Overall and subregional empirical equations for deposition efficiency were developed by incorporating the combined diffusion parameter, Sc a Δ b , corroborating the use of geometrical characteristic parameters for each specific subject in predicting nasal deposition efficiency across age groups. Our findings contribute to predictive nanoparticle exposure analysis in nasal airways across different age groups, thereby enhancing respiratory healthcare for individuals across the life span.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2020

Characterizing photovoltaic backsheet adhesion degradation using the wedge and single cantilever beam tests, Part II: Accelerated tests

Photovoltaic (PV) backsheets provide critical moisture, mechanical, and electrical insulation to the backside of PV modules, but their continued functionality depends upon their ability to remain well adhered over years of harsh environmental exposure. A study of adhesive strength was conducted on several PV backsheet types exposed to indoor accelerated weathering. Two adhesion tests – the wedge test and single cantilever beam test – were used to measure adhesion energy in four backsheets: two with fluoropolymer-based outer (airside) layers – polyvinyl fluoride (PVF), polyvinylidene fluoride (PVDF) – and two with non-fluoropolymer-based outer layers–polyamide (PA) and polyethylene terephthalate (PET). The effects of changes in temperature, ultraviolet (UV) irradiance, relative humidity, and a periodic water spray were studied. The PET-, PVF- and PVDF-based backsheets all showed instances of debonding in an adhesive layer, which is commonly reported. Furthermore, for the PA-, PET-, and PVDF-based backsheets, adhesion energy dropped fairly rapidly with exposure, reaching very low levels by 4000 h. The PVF-based backsheet was relatively robust to weathering. Pull-off of an outer chalking layer in the PA- and PET-based backsheets suggested a sensitivity to UV. Adhesion in these two backsheets was also highly sensitive to changes in moisture level. Changes in UV irradiance and temperature did not show a statistically significant effect on adhesion loss for the exposure levels used. The present work is part of a two-part adhesion study on both field-weathered and indoor-exposed backsheets, and forms a basis for understanding adhesion degradation across a variety of backsheet types and degradation factors.

14 SOLAR ENERGY↗

DOE OSTI2021

Silicon Dioxide Deposited Using Atmospheric Pressure Plasma Chemical Vapor Deposition for Improved Adhesion and Water Intrusion Resistance for Lightweight Manufacturing

This work aims to demonstrate the barrier coating, and adhesion promoting properties of silica-based coatings deposited using an atmospheric pressure plasma torch (APPT). This is achieved by applying an industrial grade adhesive to silica thin films deposited, on the surfaces to be joined, using atmospheric pressure plasma chemical vapor deposition (APP-CVD), to make single joint lap shear samples of different metal combinations commonly found in lightweight manufacturing such as aluminum and magnesium as well as steel. To deposit these thin films, two separate silicon based organic precursors, hexamethyldisiloxane (HMDSO), and tetraehylorthosilicate (TEOS), are used. Here, samples are bonded using DuPont Betamate 1486 adhesive, and the lap shear results for these films are compared to the lap shear results of a chemically cleaned control using the same adhesive. The APPT uses a microwave power supply and gas mixtures of N 2 and Ar. The adhesion of the films are tested using lap shear, and elevated temperature water soaks are conducted on the joints as well to simulate environmental exposure. Lap shear results from samples with silica thin films max shear stress are 25%-115% increase compared to control samples depending on material. After exposure to water soak the max shear strength of the joints decreased by less than 15%, which demonstrates the films capabilities as a water barrier. Film morphology is examined using Scanning Electron Microscopy (SEM), and the film’s composition and approximate thickness are obtained using Rutherford Backscattering Spectroscopy (RBS).

36 MATERIALS SCIENCE↗

DOE OSTI2025

Encapsulation of Monolayer 2D Materials Using Kinetic Energy-Controlled Pulsed Laser Deposition

The integration of monolayer (ML) two-dimensional (2D) materials into next-generation microelectronics, optoelectronics, and sensors is hindered by their sensitivity to environmental exposure. Deposition of additional layers for encapsulation or growth on ML 2D materials by versatile but energetic plasma techniques such as pulsed laser deposition (PLD) has not been considered at the monolayer level because of potential damage caused by hyperthermal species with kinetic energies (KEs) exceeding the threshold displacement energy (TDE) of the ML. Here, we describe a general strategy to understand and mitigate damage during PLD by reducing the incident KE of ablated species below the TDE of the 2D monolayer using background gas collisions. Ion flux diagnostics, combined with in situ Raman spectroscopy of monolayer graphene during PLD of amorphous boron nitride (a-BN) as a dielectric encapsulation layer, show that damage is primarily correlated with fast ions that penetrate the background gas in accordance with Beer’s Law and are often overlooked in ICCD imaging due to the dominance of the bright, delayed plasma luminescence. Significantly, if fast ions are eliminated and a ∼2 nm-thick a-BN layer is “soft landed”, the monolayer graphene is effectively protected from damage by high KE species in the boron nitride plasma plume. Deposited a-BN films display a characteristic dielectric constant of 3.6 at 100 kHz and tunable charge injection properties. Our results enable PLD as a viable option for encapsulation and thin film growth onto ML 2D materials, with implications for both fundamental research and device integration.

2D materials↗