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DOE OSTI2020

Functional Photoresists for Energy Applications. Final Report

Monolithic ultralow-density porous bulk materials have recently attracted much interest due to many emerging applications in the areas of catalysis, energy storage and conversion, and thermal insulation. They are also important components of high energy density (HED) and inertial confinement fusion (ICF) targets. However, despite tremendous progress that has been made in the synthesis of porous materials, deterministic and independent control over microscopic architecture, density and composition remain key issues, and their integration in high precision devices requires cost and time-intensive mechanical machining that not only reduces reproducibility by generating debris but also limits the complexity of the 3D shapes that can be realized. In this project, we overcame these limitations by developing a universal templating capability that provides deterministic and independent control over density, composition, architecture, and macroscopic sample shape. This was achieved by developing the technology to 1) 3D print ultrahigh resolution, ultra-high precision polymeric micro-lattice templates, 2) coat these templates with the desired materials, and 3) removing the template (Fig. 1a). Atomic layer deposition (ALD) provides the atomic scale coating thickness accuracy required for precisely controlling density. While this templating approach had been demonstrated in prior work, limitations in suitable photoresists, 3D print technologies, print design, and template removal techniques did not allow the fabrication of millimeter-sized high-precision parts with sub-micron resolution. To enable this technology, we developed 1) two-photon polymerization (TPP) print designs that enable the fabrication of millimeter-sized, mechanically robust polymeric templates with sub-micron resolution and 2) a continuum level TPP printing simulation capability for additional print design guidance; 3) atomistic models to study photoresist polymerization kinetics and network topography, 4) refractive index matched polymeric and preceramic TPP photoresists, and 5) functional TPP photoresists including porous voxel structures and self-immolative polymer photoresist chemistries; and 6) damage free template removal techniques that enable the fabrication of defect-free high-precision low-density foam components. We also developed a templating approach for pure carbon microlattices with a unique tube-in-tube ligament morphology. As a test platform, we pursued the fabrication of foam liners that promise to further increase the neutron yield in indirect drive ICF experiments by improving implosion symmetry control and coupling between the laser and the deuterium-tritium fuel. This application requires fabrication and integration of a ultra-high precision, millimeter-sized, thin-walled (200-400 micrometer thick), low-density (10-30 mg/cc), high atomic number (high Z) cylindrical foam tube into the gold hohlraum of an indirect drive ICF target (Fig. 1b). While our hohlraum liner test case will mainly find application in HED and ICF experiments, the underlying science will also directly apply to previously developed nanoparticle and additive manufacturing technologies and will advance those techniques as well.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Mechanical Consequences of Oxygen Inhibition in Vat Polymerization

Vat polymerization is a type of additive manufacturing that is used extensively to produce micro-architected structures for mechanical applications, which brings the mechanical properties of photopolymerized resins into sharp focus. However, it is known that photopolymerization is sensitive to a number of factors, perhaps the most notorious of which is oxygen inhibition. Herein, the degree to which oxygen inhibition influences the macroscopic and microscopic properties of structures made using vat polymerization is explored. This work is motivated by an observation of lattices being >4 times softer in the experiment than predicted by simulation, which is hypothesized to be due to the material at the surface being incompletely cured. Furthermore, this hypothesis is supported by four-point bending tests in which flexural modulus is found to increase with beam thickness. Nanoindentation and bulk compression studies show that this surface softening is present for three distinct resins. Importantly, it is observed that structures post-print cured in nitrogen are stiffer than those post-print cured in air, however, regardless of the post-print curing environment, printing samples in the presence of oxygen makes them softer than samples photocured in nitrogen. Collectively, these results show the outsized influence of oxygen inhibition on micro-architected structures realized using vat polymerization.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effects of a Layered Morphology on Drip Suppression in Burning Polymers

Fire safety in polymers is critically important with products such as textiles and consumer goods, as well as materials used in construction, aerospace, transportation, and furniture. Additives used as anti-dripping and flame-retardant agents impose acute human health issues and have negative environmental impacts. With a focus on developing additive-free solutions, here we used multilayer coextrusion to fabricate layered polyethylene/polypropylene (PE/PP) films and investigated the effect of a layered morphology on dripping and burning rates. The experimental results for multilayered PE/PP samples were compared to control groups of melt blended PE/PP samples. The multilayer configuration provides two significant advantages: 154% delay in the time to the first drip and up to 87% reduction in the number of drips compared to the value for the melt blended samples with no additives. PE/PP blends with up to 2 wt % polytetrafluoroethylene, a commonly used anti-dripping agent in the industry, showed only 85% delay in the time to the first drip and about 60% reduction in the number of drips. We discovered a linear relationship between film thickness and burning rate, which allows for the use of the volumetric burning rate to normalize the effect of film thickness. No benefit in the burning rate was observed when comparing multilayered structures and conventional melt blended architectures or blends with PTFE. Annealing studies and transmission electron microscopy at areas close to the combustion zones confirmed that higher extensional viscosities induced by the layered structures and morphological changes due to the layer breakup play an important role in reducing dripping. By combining the first drip time and overall drip numbers, a parameter, “dripping index”, was defined to establish a fire safety map to simplify material comparisons. This study demonstrates that a multilayer film geometry can provide an additive-free solution to yield control over fire safety parameters in polymers.

36 MATERIALS SCIENCE↗

DOE OSTI2020

High sensitivity pump–probe measurements of magnetic, thermal, and acoustic phenomena with a spectrally tunable oscillator

We describe an optical pump/probe system for sensitive measurements of time-resolved optical measurements of material dynamics. The instrument design is optimized for time-resolved magneto-optic Kerr effect (TR-MOKE) measurements of dynamics in magnetic materials. The system also allows for time-domain thermoreflectance (TDTR) measurements of thermal transport properties and picosecond acoustic measurements of film thickness and/or elastic constants. The system has several advantages over the conventional designs for TRMOKE and/or TDTR systems. Measurements of pump-induced changes to the probe beam intensity are shot-noise limited. The system’s design allows for MOKE and/or thermoreflectance measurements of both sides of a sample. Pumping and probing the sample on opposite sides allows nanoscale flash diffusivity measurements of transport properties. The wavelengths of the pump and probe beams are straightforward to tune between 350–525 nm and 690–1050 nm. A tunable wavelength allows for optical resonances in a wide array of materials to be excited and/or probed. Finally, the setup is calibrated to allow for the real and imaginary components of Kerr signals to be separately quantified.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

Bendability parameter for twisted ribbons to describe longitudinal wrinkling and delineate the near-threshold regime

We propose a dimensionless bendability parameter, ε -1 =[(h/W) 2 ⁢T -1 ] -1 , for wrinkling of thin, twisted ribbons with thickness h, width W, and tensional strain T. Bendability permits efficient collapse of data for wrinkle onset, wavelength, critical stress, and residual stress, demonstrating longitudinal wrinkling's primary dependence on this parameter. This parameter also allows us to distinguish the highly bendable range (ε -1 >20) from moderately bendable samples (ε -1 ϵ(0,20]). We identify scaling relations to describe longitudinal wrinkles that are valid across our entire set of simulated ribbons. When restricted to the highly bendable regime, simulations confirm theoretical near-threshold (NT) predictions for wrinkle onset and wavelength.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Minimum Quench Energy of Nb 3 Sn Wires With High Specific Heat Tape

A major problem of state-of-the-art Nb3Snaccelerator magnets is their long training due to thermo-mechanical perturbations. Increasing the specific heat, Cp, of the Rutherford cable would reduce and/or eliminate training by limiting the coils temperature rise. This paper studies feasibility of increasing the Cp of Rutherford-type cables by using thin composite Cu/Gd 2 O 3 and Cu/Gd 2 O 2 S tapes produced by HyperTech Research, Inc. The tape can be either wrapped around the cable, placed on the cable wide faces under the insulation, and/or inserted as a core. Wire samples outfitted with these high-Cp ribbons, or tapes, were prepared and tested at FNAL for their Minimum Quench Energy (MQE). At 90%Ic and 15 T, the average gain of MQE of the Nb 3 Sn wire soldered to the Cu/Gd 2 O 2 S 55 μm thick ribbon was 2.5, and further increased at larger transport currents.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

Functionalized Polymer Thin Films for Plutonium Capture and Isotopic Screening from Aqueous Sources

The rapid screening of plutonium from aqueous sources remains a critical challenge for nuclear nonproliferation efforts. The determination of trace-level Pu isotopes in water requires offsite sample preparation and analysis; therefore, new methods that combine plutonium purification, concentration, and isotopic screening in a fieldable detection system will provide an invaluable tool for nuclear safeguards. This contribution describes the development and characterization of thin polymer-ligand films for the isolation and concentration of waterborne Pu for direct spectroscopic analyses. Submicron thin films were prepared through spin coating onto Si wafers and consisted of combinations of polystyrene (PS) with dibenzoylmethane, thenoyltrifluoroacetone, and di(2-ethylhexyl)phosphoric acid (HDEHP). Pu uptake studies from solutions at pH from 2.3 to 6.3 indicated that only films containing HDEHP exhibited significant recovery of Pu. High alpha spectroscopy peak energy resolutions were achieved for PS-HDEHP films over a range of film thicknesses from 30 to 250 nm. Furthermore, a separate study was performed to evaluate uptake from a primarily Pu(V) solution where it was observed that doubling the HDEHP loading in the film increased uptake of Pu by an order of magnitude. X-ray photoelectron spectroscopy (XPS) analysis revealed that HDEHP was highly concentrated within the first few nanometers of the film at the higher loading. XPS analysis also revealed that, in the presence of water, HDEHP was stripped from the surface layer of the film at circumneutral pH. While significant losses of ligand were seen in all samples, higher loadings of HDEHP resulted in measurable amounts of ligand retained after a 12-h soak in water. Findings of this study are being used to guide the development of thin-film composite membrane-based detection methods for the rapid, fieldable analysis of Pu in water.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Multiport high-pressure synchrotron x-ray microscopy cell (CRADA Final Report)

The LBNL team developed a multiport cell allowing for fluid flow, with electrical contacts for sample bias, and with reference electrodes. The cell is currently installed and operating in beam-line 11.0.2 of the ALS, the Berkeley Synchrotron. The cell is closed by a membrane consisting of several stacked layers of graphene (1 to 3). The graphene membrane is supported on a 100 nm thick Si3N4 membrane covered with a 20 nm thin gold film for improved adhesion of the graphene and to ensure electrical conductivity. The Si3N4 film is perforated with a periodic array of holes 1 to 2 micrometers diameter. The cell can withhold an internal pressure (gas or liquid) of up to 10 atmospheres for in situ/operando studies using X-ray Photoelectron emission (XPS), and X-ray Absorption Spectroscopy (XAS). It is also ideal for tip-enhanced nano-Infrared Spectroscopy studies of molecules at the interface between the graphene and the liquid or gas filling the cell. Materials studied in the LBNL laboratory are in the form of nanoparticles, or thin films (few nm) deposited on the side of the graphene membrane facing the solution or gas inside the cell.

36 MATERIALS SCIENCE↗

DOE OSTI2025

A Modified Model Dielectric Function for Analyzing Optical Spectra of InGaN Nanofilms on Sapphire Substrates

Due to a lower InN bandgap energy Eg~0.7 eV, InxGa1−xN/Sapphire epifilms are considered valuable in the development of low-dimensional heterostructure-based photonic devices. Adjusting the composition x and thickness d in epitaxially grown films has offered many possibilities of light emission across a wide spectral range, from ultraviolet through visible into near-infrared regions. Optical properties have played important roles in making semiconductor materials useful in electro-optic applications. Despite the efforts to grow InxGa1−xN/Sapphire samples, no x- and d-dependent optical studies exist for ultrathin films. Many researchers have used computationally intensive methods to study the electronic band structures Ejk→, and subsequently derive optical properties. By including inter-band transitions at critical points from Ejk→, we have developed a semiempirical approach to comprehend the optical characteristics of InN, GaN and InxGa1−xN. Refractive indices of InxGa1−xN and sapphire substrate are meticulously integrated into a transfer matrix method to simulate d- and x-dependent reflectivity RE and transmission TE spectra of nanostructured InxGa1−xN/Sapphire epifilms. Analyses of RE and TE have offered accurate x-dependent shifts of energy gaps for InxGa1−xN (x = 0.5, 0.7) in excellent agreement with the experimental data.

Talwar, Devki N. (ORCID:0000000202723195)↗

DOE OSTI2026

Multiscale Cryo Electron Microscopy Reveals Interfacial Degradation and Stabilization in Battery Electrodes

Electrochemical interfaces are dynamic systems, evolving based on their local environment and reactant surface structures. The electrode-electrolyte interface in Li-ion batteries can be protective, limiting parasitic reactions with the electrolyte to passivate the surface [1]. Additionally, this interphase has an impact on the Li-ion transport through that layer based on its composition, bonding environment, and thickness. These parameters are challenging to collect and may vary depending on the electrode surface site investigated relative to its spatial position in a coin cell. This study will detail a multiscale cryogenic electron microscopy approach where millimeter-scale cross-sections through the coin cell batteries were made using a cryogenic stage within a fs-laser plasma focused ion beam (laser PFIB) with complementary energy dispersive X-ray spectroscopy able to detect variations in the composition at electrode interfaces [2]. Microscale cross-sectioning and lamella sample preparation of battery electrodes was conducted at the Center for Integrated Nanotechnologies using a Ga-ion focused ion beam (FIB) with air-free and cryo-transfer [3], followed by nanoscale mapping of composition and bonding within the CEI through cryo-scanning transmission electron microscopy (cryo-STEM) electron energy loss spectroscopy [4]. This multiscale approach enabled identification of millimeter-scale features of a battery stack with visualization of degradation in electrodes such as cracks in cathode particles, gas evolution, and SEI evolution; microscale interfacial characteristics, such as heterogeneity in the SEI or barrier layer and identification of electrolyte networks to the electrode surfaces; and nanoscale measurement of the CEI thickness, mapping of transition metal bonding within the cathode particles to identify loss of active materials, and identification of beneficial electrolyte additives incorporated into the CEI structure. This multiscale approach allows for a statistical understanding of the primary mechanisms and parasitic degradation pathways that impact performance by limiting the ion transport pathways within Li+ batteries.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Microstructure and hardness evolution induced by annealing of ion irradiated LiTaO 3

We report the evolution of the microstructure and mechanical properties of low-energy heavy-ion-irradiated LiTaO 3 crystals annealed at various temperatures was investigated by transmission electron microscopy (TEM) observations and nanoindentation tests to extend the applications of irradiated LiTaO 3 crystals. Before annealing, randomly distributed voids formed in an approximately 200 nm thick region at the end of the ion irradiation range, which was attributed to preferential absorption of interstitials by the amorphous-crystalline interface. After annealing, a new directional diffusion path of defects was identified, resulting in a void string. Furthermore, void string diffusion to the free surface was also found during the annealing temperature increase process, which offers a potential application in designing custom sized-thickness exfoliation at the nanoscale. Meanwhile, two competing processes were identified during the annealing process: epitaxial recrystallization from the amorphous-crystalline interface and grain nucleation process in the amorphous region, which formed phases different from the matrix crystal structure, resulting in an interaction between them. Furthermore, the hardness of irradiated samples was also found to be affected by the annealing process; in particular, a hardness decrease induced by the interstitial Fe ions in the recrystallized region was also confirmed, which can improve the processability of samples for further application.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Emergence of exchange bias and giant coercive field enhancement by internal magnetic frustration in La 0.67 Sr 0.33 MnO 3 thin films

We have studied the influence of controlled defects on the magnetic properties of La 0.67 Sr 0.33 MnO 3 (LSMO) thin films. We used 100 nm thick epitaxial LSMO films, which were grown on SrTiO 3 substrates and introduced stoichiometry changes and defects using oxygen ion irradiation through nanoporous alumina masks. Oxygen irradiation through the mask creates cascades of defects in spatially-modulated regions in the plane of the LSMO film. The magnetic properties of the samples were compared before and after the irradiation. We have found that irradiation reduces the ferromagnetic ordering temperature, decreases the total magnetization, enhances the coercivity, and induces exchange bias below 50 K. The coercivity enhancement is dramatically higher below 50 K and can be associated with exchange bias. These results can be explained by the formation of Mn-rich antiferromagnetic or ferrimagnetic phases within the bombarded regions that are exchange coupled to the non-irradiated - ferromagnetic host.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Densification, microstructure, and mechanical properties of Mo–30W alloys fabricated from conditioned powders

Refractory alloys, such as molybdenum-based systems, are attracting growing interest for applications in extreme environments, such as in the nuclear and aerospace industries. Recent advances in sintering technologies, coupled with mechanical alloying, have enabled the tailored design of these alloys by leveraging powder characteristics to control final microstructures and mechanical properties. In this study, Mo-30W alloys were fabricated using electric field-assisted sintering (EFAS) from ball-milled powders with and without hydrogen treatment to investigate the influence of surface oxides on material properties and sintering behavior. The results revealed that samples processed from as-ball-milled powder contained a high density of oxides within the microstructure, whereas oxide presence was significantly reduced in samples fabricated from hydrogen-treated powders. Interestingly, the two powder types led to opposite trends in grain size distribution: samples from untreated powders exhibited grain refinement from sample periphery to the center, while samples from hydrogen-treated powders showed grain coarsening toward the center. This behavior is attributed to temperature gradients present during sintering due to electrical percolation pathway differences during Joule heating. The powder surface oxides may have influenced the temperature distribution and grain evolution. Microhardness profiles measured along both axial and thickness directions were consistent with the grain size distribution. Furthermore, oxide films on powder surfaces have delayed densification by hindering particle necking and atomic diffusion during sintering.

36 - MATERIALS SCIENCE↗

DOE OSTI2023

Enhanced Switching Reliability of Hf 0.5 Zr 0.5 O 2 Ferroelectric Films Induced by Interface Engineering

Ferroelectric materials have been widely researched for applications in memory and energy storage. Among these materials and benefiting from their excellent chemical compatibility with complementary metal–oxide–semiconductor (CMOS) devices, hafnia-based ferroelectric thin films hold great promise for highly scaled semiconductor memories, including nonvolatile ferroelectric capacitors and transistors. However, variation in the switched polarization of this material during field cycling and a limited understanding of the responsible mechanisms have impeded their implementation in technology. Here, we show that ferroelectric Hf 0.5 Zr 0.5 O 2 (HZO) capacitors that are nearly free of polarization “wake-up”─a gradual increase in switched polarization as a function of the number of switching cycles─can be achieved by introducing ultrathin HfO 2 buffer layers at the HZO/electrodes interface. High-resolution transmission electron microscopy (HRTEM) reveals crystallite sizes substantially greater than the film thickness for the buffer layer capacitors, indicating that the presence of the buffer layers influences the crystallization of the film (e.g., a lower ratio of nucleation rate to growth rate) during postdeposition annealing. This evidently promotes the formation of a polar orthorhombic (O) phase in the as-fabricated buffer layer samples. Synchrotron X-ray diffraction (XRD) reveals the conversion of the nonpolar tetragonal (T) phase to the polar orthorhombic (O) phase during electric field cycling in the control (no buffer) devices, consistent with the polarization wake-up observed for these capacitors. The extent of T–O transformation in the nonbuffer samples is directly dependent on the duration over which the field is applied. Here these results provide insight into the role of the HZO/electrodes interface in the performance of hafnia-based ferroelectrics and the mechanisms driving the polarization wake-up effect.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Secondary electron emission of reticulated foam materials

Complex material surfaces can reduce secondary electron emission (SEE) and sputtering via geometric trapping. In this work, the SEE yields for a range of open-cell reticulated carbon foam geometries are characterized using scanning electron microscopy. The total reduction in the SEE yield from carbon foams with a 3% volume fill density and 10–100 pores per inch (PPI) is shown to be between 23.5% and 35.0%. Contributions of a foam backplate are assessed by experimentally and analytically defining the critical parameter, transparency. The transparency of a foam is quantified and is shown to affect the primary electron angular dependence on the SEE yield. For the same thickness of 6 mm, it is found that higher PPI decreases foam transparency from 32% to 0% and reduces the SEE yield. The SEE yield from carbon foams is also shown to have weaker dependence on the morphology of the surface compared with fuzzes and velvets and less variation across individual sample surfaces due to the rigidity of their ligament structures and isotropic geometries.

Physics↗

DOE OSTI2022

Managing Sn-Supply to Tune Surface Characteristics of Vapor-Diffusion Coating of Nb₃Sn

Nb₃Sn promises better RF performance (Q and E_{acc}) than niobium at any given temperature because of superior superconducting properties. Nb₃Sn-coated SRF cavities are now produced routinely by growing a few microns thick Nb₃Sn films inside Nb cavities via the tin vapor diffusion technique. Sn evaporation and consumption during the growth process notably affect the quality of the coating. Aiming at favorable surface characteristics that could enhance the RF performance, many coatings were produced by varying Sn sources and temperature profiles. Coupon samples were examined using different material characterization techniques, and a selected few sets of coating parameters were used to coat 1.3 GHz single-cell cavities for RF testing. The Sn supply’s careful tuning is essential to manage the microstructure, roughness, and overall surface characteristics of the coating. We summarize the material analysis of witness samples and discuss the performance of several Nb₃Sn-coated single-cell cavities linked to Sn-source characteristics and observed Sn consumption during the film growth process.

Pudasaini, U.↗

DOE OSTI2021

Managing Sn-supply to tune surface characteristics of vapor-diffusion coating of Nb3Sn

Pudasaini, U.↗

DOE OSTI2020

Vertical Structure of Radiative Heating Rates of the MJO during DYNAMO

The vertical structure of radiative heating rates over the region of the tropi-cal Indian Ocean associated with the MJO during the DYNAMO/ARM MJO Investigation Experiment is presented. The mean and variability of heating rates during active, suppressed, and disturbed phases are determined from the Paci?c Northwest National Laboratory combined remote sensing retrieval (CombRet) from Gan Island, Maldives (0.69? S, 73.15? E). TOA and surface ?uxes from the CombRet product are compared with collocated three-hourly CERES SYN1deg Ed4A satellite retrievals. The ?uxes are correlated in time with correlation coef?cients around 0.9, yet CombRet time-mean OLR is 15 W m-2 larger. Previous work has suggested that CombRet under-samples high clouds, due to attenuation by low-level clouds and reduced instrument sensitivity with altitude. However, mean OLR differs between CombRet and CERES for all values of OLR, not just the lowest values corresponding to widespread high clouds. The discrepancy peaks for mid-range OLR, sugges-tive of precipitating, towering cumulus convective clouds, rather than strati-form cirrus clouds. Biases in the cloud-top height of thick clouds substantially contribute to the overestimate of OLR by CombRet. CombRet data is used to generate composite shortwave and longwave atmospheric heating rate pro-?les as a function of the local OLR. Though there is considerable variability in CombRet not directly related to OLR, the time-height structure of mean heating rate composites generated using OLR as the interpolant is broadly representative of tropical convective variability on intraseasonal time scales.

Shell, Karen M.↗