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DOE OSTI2022

Roll-to-Roll Advanced Materials Manufacturing DOE Laboratory Collaboration - Early Stage R&D: Phase 2 and FY21 (Final Report)

R2R processing is used to manufacture a wide range of products for various applications which span many industrial business sectors. The overall R2R methodology has been in use for decades and this continuous technique traditionally involves deposition of material(s) onto substrates or membranes that are on moving webs, carriers or other continuous belt-fed or conveyor-based processes that enable successive steps to build a final product. Established methods that typify R2R processing include tape casting, silk-screen printing, reel-to-reel vacuum deposition/coating, and R2R lithography. Products supported by R2R manufacturing include micro-electronics, electro-chromic window films, PVs, fuel cells for energy conversion, battery electrodes and electrolytes for energy storage, and barrier and membrane materials for decarbonization and air and water filtration. Due to innovation in materials and process equipment, high-quality yet very low-cost multilayer technologies have the potential to be manufactured on a very cost-competitive basis. To move energy-related products from high-cost niche applications to the commercial sector, the means must be available to enable manufacture of these products in a cost-competitive manner. Fortunately, products such as fuel cells, thin- and mid-film PVs, batteries, electrochromic and piezoelectric films, water separation membranes, and other energy saving technologies readily lend themselves to manufacture using R2R approaches. However, more early-stage research is needed to solve the challenge of linking the materials (particles, polymers, solvents, additives) used in ink and slurry formulations and the coating and heated drying processes to the ultimate performance of the final R2R product, especially for a process that uses multiple layers of deposition to achieve the end product.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Influence of Oxygen Flow and Stoichiometry on Optical Properties and Damage Resistance of Hafnium Oxide Thin Films

Hafnium oxide (HfO 2 ) is predominantly used as a high-index material in multi-layer dielectric coatings for high-peak- and high-average-power lasers, but laser damage often initiates within the HfO 2 layers despite their wide bandgap. Oxygen deficiency during deposition can introduce vacancy-related sub-bandgap states and absorptive defects, lowering damage resistance. This study investigates how oxygen flow during HfO 2 deposition with ion beam sputtering (IBS) affects its stoichiometry, defect formation, and nanosecond laser-induced damage threshold (LIDT) and whether single-layer trends predict multilayer performance. Single layers were deposited at varying oxygen flows, characterized for optical and structural properties, and tested for the LIDT at 1064 nm and 355 nm. Increasing oxygen flow drove the layer toward near-stoichiometric HfO 2 , reduced the refractive index, and altered the density of surface pinhole-like features. The single-layer LIDT at 355 nm increased with oxygen, whereas the 1064 nm LIDT was comparatively less sensitive to oxygen flow, consistent with the wavelength-dependent roles of absorptive precursors and microstructural defects. In contrast, a HfO 2 -based high-reflector (HR) showed a higher LIDT at lower oxygen flow, indicating that the family of damage precursors changes between single layers and multilayers; in stacks, structural properties such as stress, gas entrapment and thermal dissipation may outweigh the isolated absorptive defects found in single layers. These results demonstrate that the optimal oxygen flow condition depends on both LIDT wavelength and film architecture. We identified, for single layers, a 15–35 sccm window for maximizing the 1064 nm LIDT and a high-flow optimum (45 sccm) for the 355 nm LIDT and, for 355 nm HR stacks, a distinct lower-flow regime (~10 sccm).

Optics and optical instruments↗

NASA NTRS1995

Low earth orbit durability of protected silicone for refractive photovoltaic concentrator arrays

Photovoltaic power systems with novel refractive silicone solar concentrators are being developed for use in low Earth orbit (LEO). Because of the vulnerability of silicones to atomic oxygen and ultraviolet radiation, these lenses are coated with a multilayer metal oxide protective coating. The objective of this work was to evaluate the effects of atomic oxygen and thermal exposures on multilayer coated silicone. Samples were exposed to high-fluence ground-laboratory and low-fluence in-space atomic oxygen. Ground testing resulted in decreases in both total and specular transmittance, while in-space exposure resulted in only small decreases in specular transmittance. A contamination film, attributed to exposed silicone at coating crack sites, was found to cause transmittance decreases during ground testing. Propagation of coating cracks was found to be the result of sample heating during exposure. The potential for silicone exposure, with the resulting degradation of optical properties from silicone contamination, indicates that this multilayer coated silicone is not durable for LEO space applications where thermal exposures will cause coating crack development and propagation.

McCollum, Timothy A.↗

NASA NTRS2017

Testing Seam Concepts for Advanced Multilayer Insulation

Multilayer insulation (MLI) is considered the state of the art insulation for cryogenic propellant tanks in the space environment. MLI traditionally consists of multiple layers of metalized films separated by low conductivity spacers. In order to better understand some of the details within MLI design and construction, GRC has been investigating the heat loads caused by multiple types of seams. To date testing has been completed with 20 layer and 50 layer blankets. Although a truly seamless blanket is not practical, a blanket lay-up where each individual layer was overlapped and tapped together was used as a baseline for the other seams tests. Other seams concepts tested included: an overlap where the complete blanket was overlapped on top of itself; a butt joint were the blankets were just trimmed and butted up against each other, and a staggered butt joint where the seam in the out layers is offset from the seam in the inner layers. Measured performance is based on a preliminary analysis of rod calibration tests conducted prior to the start of seams testing. Baseline performance for the 50 layer blanket showed a measured heat load of 0.46 Watts with a degradation to about 0.47 Watts in the seamed blankets. Baseline performance for the 20 layer blanket showed a measured heat load of 0.57 Watts. Heat loads for the seamed tests are still begin analyzed. So far analysis work has suggested the need for corrections due to heat loads from both the heater leads and the instrumentation wires. A careful re-examination of the calibration test results with these factors accounted for is also underway. This presentation will discuss the theory of seams in MLI, our test results to date, and the uncertainties in our measurements.

multilayer insulation↗

NASA NTRS2018

Lightweight, Durable, and Multifunctional Electrical Insulation Material Systems for High Voltage Applications

Newly developed multilayer structures of well-known polymer insulation materials significantly improved dielectric breakdown voltage, VB, or dielectric strength, K, if well-bonded, when compared to those of single material insulations or the commercial SOA systems, such as Teflon-Kapton-Teflon (TKT), at the same overall thickness. To date, the greatest improvement of the new structures from a few candidate materials, including various types of Kapton PIs and PFA or PET as bond layer (BL), was about 61% higher than that of the Kapton PI alone films, 40.1 vs. 24.9 kV, which was translated to 86.3% decrease in insulation thickness, thus significant volume and weight reduction of the final system. However, it was of interest to note that most improvements of the multilayer structures occurred at thicker overall thicknesses, above ~ 0.15 mm. Extensive analyses also showed that K of the multilayer structures increased with (i) decreasing individual layer thickness regardless of material type, (ii) increasing total accumulated thickness of PI or overall PI/BL ratio, and (iii) increasing number of interface or total number of layers, but only above the aforementioned overall thickness limit. Increases in VB of the multilayer structures were directly correlated with damage evolution and failure mode. With further material-design-process optimizations of the multilayer structures, it was expected to achieve other multifunctionalities, such as high partial discharge (PD) resistance, improved durability, EMI shielding, and high thermal dissipation in addition to high dielectric strength. These new structures can be used in various high voltage and high temperature applications, such as future hybrid or all electric aircraft wiring and power transmission as well as many other non-aerospace high power cables, electronic parts and components, printed circuit board, and so forth. The multilayer insulation system can be easily processed and manufactured with various conductor types via calendaring, compression-molding, stamping, laminating, vacuum-bagging and autoclaving, or 3D printing, even for complex 3-D components. Based on their unique structural configurations and potential capabilities, the new insulation system was identified as micro-multilayer multifunctional electrical insulation (MMEI). Patent application of the MMEI concept and current design configurations was filed for a 1-year provisional application (OAI-58834, Serial No.: 62/659,234), pending conversion to a U.S. utility application. This paper presents details of the MMEI structures, their dielectric performance analyses, potential mechanisms, and commercial scaleup feasibility assessment.

Electric aircrafts↗

NASA NTRS2018

Lightweight, Durable, and Multifunctional Electrical Insulation Material Systems for High Voltage Applications

Multifunctional↗

DOE OSTI2021

Chemical and structural characterization of EUV photoresists as a function of depth by standing-wave x-ray photoelectron spectroscopy

The success in the miniaturization of the electronic device constituents depends mostly on the photolithographic techniques. Recently, to achieve patterning at the sub-10-nm node, extreme ultraviolet (EUV) lithography has been introduced into high volume production. Continued scaling of EUV via increased numerical aperture to achieve nodes at 3-nm and below requires the development of fundamentally new patterning materials and new characterization methods. Current EUV-resist film thicknesses are in the 20- to 40-nm range, and further thickness reduction is required for the next generation. Therefore, interfaces become exceedingly important, and the properties of the resist film would be dominated by top and bottom interfacial effects. X-ray photoelectron spectroscopy (XPS) combined with standing-wave excitation (SW-XPS), a fairly new method in the EUV lithography field, previously had been largely applied in multilayers and superlattices for characterizing the composition and electronic structure of buried layers and interfaces as a function of depth. We applied the SW-XPS method to organic/inorganic photoresists to provide depth-selective information on their structural and chemical conditions of as a function of temperature, EUV exposure, different underlayers, and other fundamental parameters. As a first attempt, we perform an SW-XPS feasibility study on self-assembled monolayer (SAM) films after exposure to an electron beam. By SW-XPS, we determined that the interface between the Al 2 O 3 underlayer and the SAMs is smooth, with a mean roughness of about 0.2 nm. Moreover, we determined that the SAM chains are, on average, tilted by 1/430 deg off the sample normal. The SW-XPS results also suggest that the SAM is not a perfectly aligned and uniform monolayer, with some areas having thickness higher than a single monolayer. We demonstrated that SW-XPS can provide useful information on ultrathin materials with high potential for being used as a characterization method of organic/inorganic photoresists.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Improved Polypropylene Thermoformability through Polyethylene Layering

Due to its low cost, stiffness, and recyclability, isotactic polypropylene (iPP) is an excellent candidate for packaging applications. However, iPP is notoriously difficult to thermoform due to its low melt strength. The addition of just 10 thin layers of high-molecular-weight, linear low-density polyethylene (LLDPE) into iPP sheets by coextrusion significantly increased extensional viscosity and reduced sag. Both LLDPE and iPP were metallocene-catalyzed with excellent adhesion as measured in our previous work. Here, we performed a series of hot tensile tests and sheet sag measurements to determine the properties of the iPP sheet and the multilayer sheet between 130 and 180 °C. To evaluate the thermoformability of these multilayer sheets, truncated conical cups were positive vacuum formed at different temperatures and heating times, and the crush strength was measured. Cups that released easily from the mold with good shape retention and a crush strength within 80% of the maximum value were used to define a temperature–time thermoformability window. We estimated the maximum stress that occurred during the thermoforming process to be 5 MPa. Layer thicknesses before and after thermoforming were used to estimate an average strain of 0.78. The thin LLDPE layers decreased the yield stress below 5 MPa. This enabled thermoforming at sheet temperatures as low as 150 °C. The immiscible LLDPE interfaces increased extensional viscosity, which decreased sag in the multilayer sheets compared to iPP. This broadened the thermoforming range to temperatures as high as 180 °C and allowed longer heating times. These highly thermoformable, layered sheets may be recycled as iPP since they contain only 8% of LLDPE.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Thermal model for time-domain thermoreflectance experiments in a laser-flash geometry

Time-domain thermoreflectance (TDTR) is a well-established pump–probe method for measuring thermal conductivity and interface conductance of multilayers. Interpreting signals in a TDTR experiment requires a thermal model. In standard front/front TDTR experiments, both pump and probe beams typically irradiate the surface of a multilayer. As a result, existing thermal models for interpreting thermoreflectance experiments assume that the pump and probe beams both interact with the surface layer. Here, we present a frequency-domain solution to the heat-diffusion equation of a multilayer in response to nonhomogeneous laser heating. This model allows analysis of experiments where the pump and probe beams irradiate opposite sides of a multilayer. We call such a geometry a front/back experiment to differentiate such experiments from standard TDTR experiments. As an example, we consider a 60nm amorphous Si film. We consider how signals differ in a front/front vs front/back geometry and compare thermal model predictions to experimental data.

Peng, Wanyue↗

NASA NTRS1988

Soft X-ray spectrographs for solar observations

Recent advances in soft X-ray spectrometery are reviewed, with emphasis on techniques for studying the windowless region from roughly 1-100 A. Recent technological developments considered include multilayer mirrors, large-format CCD detectors which are sensitive to X-rays, position-sensitive photon counting detectors, new kinds of X-ray films, and optical systems based on gratings with nonuniform ruling spacings. Improvements in the extent and accuracy of the atomic physics data sets on which the analysis of spectroscopic observatons depend are also discussed.

Bruner, M. E.↗

DOE OSTI2021

Strong effect of scandium source purity on chemical and electronic properties of epitaxial Sc x Al 1–x N/GaN heterostructures

Epitaxial multilayer heterostructures of Sc x Al 1–x N/GaN with Sc contents x = 0.11–0.45 are found to exhibit significant differences in structural quality, chemical impurity levels, and electronic properties depending on the starting Sc source impurity levels. A higher purity source leads to a 2–3 orders of magnitude reduction in the carbon, oxygen, and fluorine unintentional doping densities in MBE-grown Sc x Al 1–x N/GaN multilayers. Electrical measurements of Sc x Al 1–x N/n + GaN single heterostructure barriers show a 5–7 orders of magnitude reduction in the electrical leakage for films grown with a higher purity Sc source at most Sc contents. The measured chemical and electrical properties of epitaxial Sc x Al 1–x N highlight the importance of the starting Sc source material purity for epitaxial device applications that need these highly piezoelectric and/or ferroelectric transition-metal nitride alloys.

36 MATERIALS SCIENCE↗

NASA NTRS1986

Influence of process parameter variation on the reflectivity of sputter-deposited W-C multilayer diffraction gratings

Multilayer W-C diffraction gratings with nominal d spacings of 35 A have been fabricated by magnetron sputter deposition. The peak and integrated reflectivities of these films have been measured with Al K-alpha X-rays and compared to theoretical values. The rms surface roughness has been evaluated. The influence of several sputtering-system process parameters on the reflectivities has been investigated.

Sager, B.↗

DOE OSTI2021

Electronic Structure and Stacking Arrangement of Tungsten Disulfide at the Gold Contact

There is an intensive effort to control the nature of attractive interactions between ultrathin semiconductors and metals and to understand its impact on the electronic properties at the junction. In this work, we present a photoelectron spectroscopy study on the interface between WS 2 films and gold, with a focus on the occupied electronic states near the Brillouin zone center (i.e., the Γ point). To delineate the spectra of WS 2 supported on crystalline Au from the suspended WS 2 , we employ a microscopy approach and a tailored sample structure, in which the WS 2 /Au junction forms a semi-epitaxial relationship and is adjacent to suspended WS 2 regions. The photoelectron spectra, as a function of WS 2 thickness, display the expected splitting of the highest occupied states at the Γ point. In multilayer WS 2 , we discovered variations in the electronic states that spatially align with the crystalline grains of underlying Au. Corroborated by density functional theory calculations, we attribute the electronic structure variations to stacking variations within the WS 2 films. We propose that strong interactions exerted by Au grains cause slippage of the interfacing WS 2 layer with respect to the rest of the WS 2 film. Our findings illustrate that the electronic properties of transition metal dichalcogenides, and more generally 2D layered materials, are physically altered by the interactions with the interfacing materials, in addition to the electron screening and defects that have been widely considered.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2016

Multilayer Active Shell Mirrors for Space Telescopes

A novel active mirror technology based on carbon fiber reinforced polymer (CFRP) substrates and replication techniques has been developed. Multiple additional layers are implemented into the design serving various functions. Nanolaminate metal films are used to provide a high quality reflective front surface. A backing layer of thin active material is implemented to provide the surface-parallel actuation scheme. Printed electronics are used to create a custom electrode pattern and flexible routing layer. Mirrors of this design are thin (< 1.0 mm), lightweight (2.7 kg/m2 ), and have large actuation capabilities. These capabilities, along with the associated manufacturing processes, represent a significant change in design compared to traditional optics. Such mirrors could be used as lightweight primaries for small CubeSat-based telescopes or as meter-class segments for future large aperture observatories. Multiple mirrors can be produced under identical conditions enabling a substantial reduction in manufacturing cost and complexity. An overview of the mirror design and manufacturing processes is presented. Predictions on the actuation performance have been made through finite element simulations demonstrating correct abilities on the order of 250−300× for astigmatic modes with only 41 independent actuators. A description of the custom metrology system used to characterize the active mirrors is also presented. The system is based on a Reverse Hartmann test and can accommodate extremely large deviations in mirror figure (> 100 µm PV) down to sub-micron precision. The system has been validated against several traditional techniques including photogrammetry and interferometry. The mirror performance has been characterized using this system, as well as closed-loop figure correction experiments on 150 mm dia. prototypes. The mirrors have demonstrated post-correction figure accuracies of 200 nm RMS (two dead actuators limiting performance).

Reverse Hartmann↗

DOE OSTI2020

In-plane Néel wall chirality and orientation of interfacial Dzyaloshinskii-Moriya vector in magnetic films

The interfacial Dzyaloshinskii-Moriya interaction (DMI) is of great interest as it can stabilize chiral spin structures in thin films. Experiments verifying the orientation of the interfacial DMI vector remain rare, in part due to the difficulty of separating vector components of DMI. In this study, Fe/Ni bilayers and Co/Ni multilayers were deposited epitaxially onto Cu(001) and Pt(111) substrates, respectively. By tailoring the effective anisotropy, spin reorientation transitions (SRTs) are employed to probe the orientation of the DMI vector by measuring the spin structure of domain walls on both sides of the SRTs. In our results, the interfacial DMI is found to be sufficiently strong to stabilize chiral Néel walls in the out-of-plane magnetized regimes, while achiral Néel walls are observed in the in-plane magnetized regimes. Furthermore, these findings experimentally confirm that the out-of-plane component of the DMI vector is insignificant in these fcc(001) and fcc(111) oriented interfaces, even in the presence of atomic steps.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS2002

Theoretical Studies of Liquid He-4 Near the Superfluid Transition

We performed theoretical studies of liquid helium by applying state of the art simulation and finite-size scaling techniques. We calculated universal scaling functions for the specific heat and superfluid density for various confining geometries relevant for experiments such as the confined helium experiment and other ground based studies. We also studied microscopically how the substrate imposes a boundary condition on the superfluid order parameter as the superfluid film grows layer by layer. Using path-integral Monte Carlo, a quantum Monte Carlo simulation method, we investigated the rich phase diagram of helium monolayer, bilayer and multilayer on a substrate such as graphite. We find excellent agreement with the experimental results using no free parameters. Finally, we carried out preliminary calculations of transport coefficients such as the thermal conductivity for bulk or confined helium systems and of their scaling properties. All our studies provide theoretical support for various experimental studies in microgravity.

Manousakis, Efstratios↗

DOE OSTI2020

Controlling Magnetization Vector Depth Profiles of La 0.7 Sr 0.3 CoO 3 /La 0.7 Sr 0.3 MnO 3 Exchange Spring Bilayers via Interface Reconstruction

The La 0.7 Sr 0.3 CoO 3–δ /La 0.7 Sr 0.3 MnO 3–δ (LSCO/LSMO) bilayer system is an ideal perovskite oxide platform for investigating interface reconstruction and its effect on their magnetic properties. Previous studies have shown that LSCO can separate into magnetic sublayers, which possess distinct trends as the total LSCO thickness increases. Here, we used polarized neutron reflectometry to quantify changes in the magnetic and chemical depth profiles, and it confirms the formation of ~12 Å-thick interfacial LSCO and LSMO layers, characterized by a decreased nuclear scattering length density compared to the bulk of the layers. This decrease is attributed to the combined effects of oxygen vacancy formation and interfacial charge transfer, which lead to magnetically active Co 2+ ions with ionic radii larger than the Co 3+ /Co 4+ ions typically found in bulk LSCO or single-layer films. The interfacial magnetization values, as well as Co 2+ ion and oxygen vacancy concentrations, depend strongly on the LSCO layer thickness. These results highlight the sensitive interplay of the cation valence states, oxygen vacancy concentration, and magnetization at interfaces in perovskite oxide multilayers, demonstrating the potential to tune their functional properties via careful design of their structure.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Structure and Desorption Kinetics of Acetonitrile Thin Films on Pt(111) and on Graphene on Pt(111)

Acetonitrile thin films were prepared on Pt(111) and on graphene on Pt(111) using molecular beam techniques. Temperature programed desorption (TPD) experiments of acetonitrile on Pt(111) displayed first-order kinetics for monolayer desorption and zero-order kinetics for multilayer desorption. We used reflection adsorption infrared spectroscopy (RAIRS) to characterize the orientation of the monolayer on Pt(111). Acetonitrile molecules have been shown to adopt a bridging structure where the C=N bond breaks to form two single bonds to underlying platinum atoms. When Tdeposition = 120 K our RAIRS spectra are consistent with this bridging configuration. However, when Tdeposition was lowered to 60 K molecules retained the C=N bond and adopted a vertical orientation with the nitrogen closest to the platinum. On graphene, the TPD experiments show that both the monolayer and multilayer desorb with zero-order kinetics. Our RAIRS spectra suggest that the monolayer consists of acetonitrile molecules oriented with their molecular axes parallel to the graphene substrate. This orientation did not change when Tdeposition was varied from 60 to 120 K. Our results provide a more complete picture of how acetonitrile molecules interact with Pt(111) and with graphene surfaces.

desorption tin films, molecules, thin films, desor↗