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DOE OSTI2023

Decoding the Atomic Structure of Ga 2 Te 5 Pulsed Laser Deposition Films for Memory Applications Using Diffraction and First-Principles Simulations

Neuromorphic computing, reconfigurable optical metamaterials that are operational over a wide spectral range, holographic and nonvolatile displays of extremely high resolution, integrated smart photonics, and many other applications need next-generation phase-change materials (PCMs) with better energy efficiency and wider temperature and spectral ranges to increase reliability compared to current flagship PCMs, such as Ge 2 Sb 2 Te 5 or doped Sb 2 Te. Gallium tellurides are favorable compounds to achieve the necessary requirements because of their higher melting and crystallization temperatures, combined with low switching power and fast switching rate. Ga 2 Te 3 and non-stoichiometric alloys appear to be atypical PCMs; they are characterized by regular tetrahedral structures and the absence of metavalent bonding. The sp 3 gallium hybridization in cubic and amorphous Ga 2 Te 3 is also different from conventional p-bonding in flagship PCMs, raising questions about its phase-change mechanism. Furthermore, gallium tellurides exhibit a number of unexpected and highly unusual phenomena, such as nanotectonic compression and viscosity anomalies just above their melting points. Using high-energy X-ray diffraction, supported by first-principles simulations, we will elucidate the atomic structure of amorphous Ga 2 Te 5 PLD films, compare it with the crystal structure of tetragonal gallium pentatelluride, and investigate the electrical, optical, and thermal properties of these two materials to assess their potential for memory applications, among others.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Photo-Switching of Protein Dynamical Collectivity

We examine changes in the picosecond structural dynamics with irreversible photobleaching of red fluorescent proteins (RFP) mCherry, mOrange2 and TagRFP-T. Measurements of the protein dynamical transition using terahertz time-domain spectroscopy show in all cases an increase in the turn-on temperature in the bleached state. The result is surprising given that there is little change in the protein surface, and thus, the solvent dynamics held responsible for the transition should not change. A spectral analysis of the measurements guided by quasiharmonic calculations of the protein absorbance reveals that indeed the solvent dynamical turn-on temperature is independent of the thermal stability/photostate however the protein dynamical turn-on temperature shifts to higher temperatures. This is the first demonstration of switching the protein dynamical turn-on temperature with protein functional state. The observed shift in protein dynamical turn-on temperature relative to the solvent indicates an increase in the required mobile waters necessary for the protein picosecond motions, that is, these motions are more collective. Melting-point measurements reveal that the photobleached state is more thermally stable, and structural analysis of related RFP’s shows that there is an increase in internal water channels as well as a more uniform atomic root mean squared displacement. These observations are consistent with previous suggestions that water channels form with extended light excitation providing O2 access to the chromophore and subsequent fluorescence loss. We report that these same channels increase internal coupling enhancing thermal stability and collectivity of the picosecond protein motions. The terahertz spectroscopic characterization of the protein and solvent dynamical onsets can be applied generally to measure changes in collectivity of protein motions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Structural, Thermal, and Mechanical Characterization of a Thermally Conductive Polymer Composite for Heat Exchanger Applications

Polymer composites are being considered for numerous thermal applications because of their inherent benefits, such as light weight, corrosion resistance, and reduced cost. In this work, the microstructural, thermal, and mechanical properties of a 3D printed polymer composite with high thermal conductivity are examined using multiple characterization techniques. Infrared spectroscopy and X-ray diffraction reveal that the composite contains a polyphenylene sulfide matrix with graphitic fillers, which is responsible for the high thermal conductivity. Furthermore, differential scanning calorimetry determines that the glass transition and melting point of the composite are 87.6 °C and 285.6 °C, respectively. Thermogravimetric analysis reveals that the composite is thermally stable up to ~400 °C. Creep tests are performed at different isotherms to evaluate the long-term performance of the composite. The creep result indicates that the composite can maintain mechanical integrity when used below its glass transition temperature. Nanoindentation tests reveal that modulus and hardness of the composite is not significantly influenced by heating or creep conditions. These findings indicate that the composite is potentially suitable for heat exchanger applications.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Thermal History of Matrix Forsterite Grains from Murchison Based on High-resolution Tomography

Protoplanetary disks are dust- and gas-rich structures surrounding protostars. Depending on the distance from the protostar, this dust is thermally processed to different degrees and accreted to form bodies of varying chemical compositions. The primordial accretion processes occurring in the early protoplanetary disk such as chondrule formation and metal segregation are not well understood. One way to constrain them is to study the morphology and composition of forsteritic grains from the matrix of carbonaceous chondrites. Here, we present high-resolution ptychographic X-ray nanotomography and multimodal chemical microtomography (X-ray diffraction and X-ray fluorescence) to reveal the early history of forsteritic grains extracted from the matrix of the Murchison CM2.5 chondrite. Here,. the 3D electron density maps revealed, at unprecedented resolution (64 nm), spherical inclusions containing Fe–Ni, very little silica-rich glass and void caps (i.e., volumes where the electron density is consistent with conditions close to vacuum) trapped in forsterite. The presence of the voids along with the overall composition, petrological textures, and shrinkage calculations is consistent with the grains experiencing one or more heating events with peak temperatures close to the melting point of forsterite (~2100 K), and subsequently cooled and contracted, in agreement with chondrule-forming conditions.

58 GEOSCIENCES↗

DOE OSTI2023

AlGaN High Electron Mobility Transistor for High-Temperature Logic

Here we report on AlGaN high electron mobility transistor (HEMT)-based logic development, using combined enhancement- and depletion-mode transistors to fabricate inverters with operation from room temperature up to 500°C. Our development approach included: (a) characterizing temperature-dependent carrier transport for different AlGaN HEMT heterostructures, (b) developing a suitable gate metal scheme for use in high temperatures, and (c) over-temperature testing of discrete devices and inverters. Hall mobility data (from 30°C to 500°C) revealed the reference GaN-channel HEMT experienced a 6.9x reduction in mobility, whereas the AlGaN channel HEMTs experienced about a 3.1x reduction. Furthermore, a greater aluminum contrast between the barrier and channel enabled higher carrier densities in the two-dimensional electron gas for all temperatures. The combination of reduced variation in mobility with temperature and high sheet carrier concentration showed that an Al-rich AlGaN-channel HEMT with a high barrier-to-channel aluminum contrast is the best option for an extreme temperature HEMT design. Three gate metal stacks were selected for low resistivity, high melting point, low thermal expansion coefficient, and high expected barrier height. The impact of thermal cycling was examined through electrical characterization of samples measured before and after rapid thermal anneal. The 200-nm tungsten gate metallization was the top performer with minimal reduction in drain current, a slightly positive threshold voltage shift, and about an order of magnitude advantage over the other gates in on-to-off current ratio. After incorporating the tungsten gate metal stack in device fabrication, characterization of transistors and inverters from room temperature up to 500°C was performed. The enhancement-mode (e-mode) devices’ resistance started increasing at about 200°C, resulting in drain current degradation. This phenomenon was not observed in depletion-mode (d-mode) devices but highlights a challenge for inverters in an e-mode driver and d-mode load configuration.

42 ENGINEERING↗

DOE OSTI2023

Investigation of Lubricant Additive Interactions on Gasoline Particulate Filters

To understand how the composition of novel lubricant additives and their ash interact with gasoline particulate filters (GPFs), an accelerated aging protocol was conducted using three lubricant additive formulations and two GPF types. The additive packages (adpaks) consisted of Ca+Mg detergent in a 3:1 or 0:1 ratio and an anti-wear component—either zinc dialkyl dithiophosphate (ZDDP) or a novel phosphonium-phosphinate ionic liquid (IL) substitute. The particulate sampling captured amount/compositions of particulate matter (PM) generated, total particulate number, and size distribution. Five ash loadings were completed. GPF position and adpak composition affected the backpressure, ash composition, ash morphology, and captured mass. The particulate sampling indicated that the ash component consisted primarily of particles less than 50 nm in size and that the Mg-only adpak resulted in more particulate of 50–400 nm in size. Postmortem materials characterization indicated GPFs in the underfloor position had deeper penetration of ash into the walls compared to the close-coupled position. Additionally, the Mg-only adpak had a higher filter collection efficiency (>90%) and the ash particles consisted of a higher concentration of dense ash material. In contrast, four of the 3:1 Ca:Mg lubricant adpaks resulted in a collection efficiency of only 40–50%. Although the collection efficiency was higher with the Mg-only adpak, the ash layer in the GPF was not thicker, nor was the penetration into the wall more significant, and surprisingly the full useful life (FUL) backpressure was lower than with Ca:Mg adpaks. The higher density of the Mg-derived ash was the only detectable difference. A possible explanation of this observation is that Mg ash has a lower melting point and is more susceptible to densification during combustion or GPF regeneration. The substitution of IL in place of the ZDDP did not lead to any notable changes in collection efficiency or location of the ash.

42 ENGINEERING↗

DOE OSTI2022

Feedstock to Function (F2F) v1

The Feedstock to Function (F2F) tool was designed to help scientists and companies explore viable biofuels and bioproducts early in the R&D cycle to support more productive experimentation, while reducing early-stage exploration from months/years to days/weeks (feedstock-to-function.lbl.gov). The tool focuses on using machine learning to predict biomass-derived molecule properties, while evaluating the cost, benefits, and risks of promising molecules for sustainable aviation fuels. The tool successfully predicts (within 15% of experimental values) high-throughput aviation properties for over 10,000 molecules while enabling users to explore new possibilities and opportunities rapidly and effortlessly. It also links to lightweight life-cycle analysis and techno-economic tools for cost and emissions analyses. Predicted molecule properties include melting point, boiling point, flash point, yield sooting index, and heat of combustion. To date, F2F is more expansive and outperforms several other molecule property prediction models while enabling users (scientists, companies, and policy makers) to explore new possibilities and opportunities rapidly and effortlessly. F2F provides the foundation for developing an adaptive computational tool that predicts properties, cost, benefits, and risk of promising new and uncertified alternative jet fuel pathways and their blending effects.

Rapp, Vi↗

DOE OSTI2021

Controlled Conversion of Sodium Metal From Nuclear Systems to Sodium Chloride

A series of three bench-scale experiments was performed to investigate the conversion of sodium metal to sodium chloride via reactions with non-metal and metal chlorides. Specifically, batches of molten sodium metal were separately contacted with ammonium chloride and ferrous chloride to form sodium chloride in both cases along with iron in the latter case. Additional ferrous chloride was added to two of the three batches to form low melting point consolidated mixtures of sodium chloride and ferrous chloride, whereas consolidation of a sodium-chloride product was performed in a separate batch. Samples of the products were characterized via X-ray diffraction to identify attendant compounds. The reaction of sodium metal with metered ammonium chloride particulate feeds proceeded without reaction excursions and produced pure colorless sodium chloride. The reaction of sodium metal with ferrous chloride yielded occasional reaction excursions as evidenced by temperature spikes and fuming ferrous chloride, producing a dark salt-metal mixture. This investigation into a method for controlled conversion of sodium metal to sodium chloride is particularly applicable to sodium containing elevated levels of radioactivity—including bond sodium from nuclear fuels—in remote-handled inert-atmosphere environments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Low-temperature bonding with spaced nanorods and eutectic alloys

Bonded surfaces are formed by adhering first nanorods and second nanorods to respective first and second surfaces. The first shell is formed on the first nanorods and the second shell is formed on the second nanorods, wherein at least one of the first nanorods and second nanorods, and the first shell and the second shell are formed of distinct metals. The surfaces are then exposed to at least one condition that causes the distinct metals to form an alloy, such as eutectic alloy having a melting point below the temperature at which the alloy is formed, thereby bonding the surfaces upon which solidification of the alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Battery with aluminum-containing cathode

A battery includes an anode chamber configured to contain an anolyte and including an anode, a cathode chamber configured to contain a catholyte including a cathode, and a separator between the anode chamber and the cathode chamber. The anode includes sodium, and the cathode includes aluminum. The battery is configured to be operated above a melting point of the anolyte and the catholyte, such that the anolyte is a molten anolyte and the catholyte is a molten catholyte.

25 ENERGY STORAGE↗

DOE OSTI2020

System and method for forming material substrate printer

A method is disclosed for manufacturing a part via an additive manufacturing process. A solution is used which has a volatile component within which is suspended particles of a powdered material. The solution is heated until it at least one of begins boiling or is about to begin boiling. The heated solution is then deposited at least at one location on a substrate to help form a layer of the part. The volatile component then evaporates, leaving only the particles of powdered material. The particles are then heated to the melting point. The deposition and heating operations are repeated to successively form a plurality of layers for the part. The evaporation of the volatile component helps to cool the part.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Corrosion and creep resistant high Cr FeCrAl alloys

An alloy includes in weight % based upon the total weight of the alloy: 28-35% Cr; 2.5-4% Al; 0.8-2% Nb; 5.5-7.5% W; 0-0.5% Mo; 0-0.3% Ti; 0.1-0.3% Zr; 0.1-1% Si; 0-0.07% Y; 0-2% Mn; 0-1% Ni; 0-0.05% C; 0-0.015% B; 0-0.02% N; 0.02-0.04 Ce; balance Fe. The alloy includes a recrystallized, equi-axed grain structure, and forms an external alumina scale, and has strengthening particles including Fe2M (M: Nb, W, Mo, and Ti) type C14 Laves-phase, and a BCC ferritic matrix microstructure from room temperature to melting point with less than 1% FCC-phase, less than 1% martensite phase, less than 0.5 wt. % of carbides (MC and M23C6), and at least 1% tensile elongation at room temperature. The alloy provides a creep resistance of greater than 3000 to 15000 h creep rupture life at 750° C. and 50 MPa, or greater than 500 to 5000 h creep rupture life at 700° C. and 100 MPa.

Yamamoto, Yukinori↗

DOE OSTI2022

Plasma confinement system with outer electrode having liquifiable material and methods for use

An example plasma confinement system includes an inner electrode having a rounded first end that is disposed on a longitudinal axis of the plasma confinement system and an outer electrode that at least partially surrounds the inner electrode. The outer electrode includes a solid conductive shell and an electrically conductive material disposed on the solid conductive shell and on the longitudinal axis of the plasma confinement system. The electrically conductive material has a melting point within a range of 170° C. to 800° C. at 1 atmosphere of pressure. Related plasma confinement systems and methods are also disclosed herein.

Shumlak, Uri↗

DOE OSTI2022

System and method for forming material substrate printer

Demuth, James A.↗

DOE OSTI2022

Fault Characterization and Diagnostics Supporting Condition-Based Operation and Maintenance of Gas Turbine Engines

Condition-Based Operation and Maintenance (CBOM) is the state-of-the-art in maintenance approaches for gas turbine engines. CBOM applies engine sensor information to the optimization of future operation and maintenance procedures; this technique reduces costs for engine operators by minimizing unplanned outages and catastrophic engine degradation. However, due to the complexities of gas turbine operation and the lack of available engine sensors, further development is required to fully realize the benefits of CBOM. In the turbine section, rotating components interact with high temperature flows, which creates intense thermal and mechanical stresses. As a result, there are numerous mechanisms of component degradation in the turbine section. Furthermore, turbine components – like stator vanes and rotor blades – are among the most expensive in the engine because they are complex to design and manufacture. For these reasons, this dissertation addresses two main questions: (i) which parameters or faults within the turbine section are most important to monitor, and (ii) how can these parameters or faults be monitored in an engine-relevant environment? Although many turbine parameters and faults have been investigated in the open literature, there are some faults that are still not well understood. Rotor-casing eccentricity, which causes a non-constant blade tip clearance around the annulus, has not been investigated in terms of its effects on turbine efficiency. Therefore, the first study in this dissertation quantifies overall and local turbine efficiency for varying levels of rotor-casing eccentricity. Results showed negligible variations to overall turbine efficiency, meaning rotor-casing eccentricity only becomes relevant to CBOM when its severity causes rotordynamic issues. Purge flow is critical to turbine hardware longevity because it prevents ingestion of hot main gas path (MGP) flow into the under-platform regions. Despite its importance, there are currently no methods for monitoring purge flow performance in an engine environment. Therefore, the second study in this dissertation develops a predictive model for sealing effectiveness using inputs from two fast-response pressure sensors. Results exhibited low prediction errors across a full range of purge flow rates, which supports the viability of the modelling approach for CBOM. The final two studies in this dissertation address blade coolant flow monitoring. This cooling flow is responsible for protecting the turbine blades from the MGP flow, which exits the combustor at temperatures greater than the blade melting point. These studies showed that temperature measurements on the blade surface can be used to accurately predict blade coolant flow rate, and that defining the candidate features relative to the coolant trajectory is important for maintaining accuracy as coolant flow rate degradation occurs. This work enables blade coolant flow monitoring, which is currently not possible through existing condition monitoring techniques.

condition-based, gas turbines, diagnostics,↗

DOE OSTI2023

Moldable photovoltaic solar cell module

A moldable photovoltaic module is provided. The module includes a flexible polymeric flex-circuit substrate having an electrically conductive printed wiring pattern and solder pads defined on it. Small photovoltaic cells are affixed to the flex-circuit substrate by back-surface contacts in electrical contact with the solder pads. At least one thermoformable polymeric film is joined to the flex-circuit substrate. Each said solder pad comprises a solder composition that, after an initial melt, has a melting point that lies above at least a portion of the temperature range for thermoforming the polymeric film.

14 SOLAR ENERGY↗

DOE OSTI2023

Ab Initio Evaluation of Plutonium Dioxide $S(α,β)$ and Thermal Neutron Cross Sections

Plutonium Dioxide (PuO 2 ) is an advanced fuel-cycle nuclear fuel material for thermal and fast reactors, with a melting point at 3261.8 K and thermal conductivity above 3 Wm -1 K -1 for temperatures below 1500 K. Plutonium from spent UO 2 is reprocessed to form chemically stable mixed oxide (MOX) fuel. In contrast to metallic fuels, the low PuO 2 conductivity results in high thermal gradients between fuel center and surface, resulting in structural annealing and efficient fission product migration over burnup. Crystal binding affects the doppler broadening of epithermal resonances for nuclear fuels and scattering behavior of thermal neutrons. Currently, there is no ENDF/B Thermal Scattering Law, i.e., $S(α,β)$, evaluation for PuO 2 , only free atom cross sections for Plutonium and Oxygen, respectively, which neglect lattice contributions to total cross section. Herein, ab initio lattice dynamics (AILD) techniques are employed to calculate the phonon density of states (DOS) using spin-orbit-coupling density functional theory (DFT) to predict the PuO2 paramagnetic ground-state structure. These results highlight the evaluation of $S(α,β)$ for Plutonium and Oxygen, respectively in PuO 2 and consequential generation of thermal neutron scattering cross sections for high fidelity criticality safety analysis and reactor calculations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Methods for manufacturing electrochemical sensors, and related electrochemical sensors

Methods for manufacturing an electrochemical sensor include forming at least one electrode by printing at least one conductive ink on a surface of at least one substrate. The conductive ink may comprise, e.g., a platinum-group metal, another transition-group metal with a high-temperature melting point, a conductive ceramic material, glass-like carbon, or a combination thereof. The electrochemical sensor may be free of another material over the at least one electrode. An electrochemical sensor, formed according to such methods, may be configured for use in harsh environments (e.g., a molten salt environment). Electrodes of the electrochemical sensor comprise conductive material formed from a printed, conductive ink. In some embodiments, at least a portion of the electrochemical sensor is free of silver, gold, copper, silicon, and polymer materials, such portion being that which is to be exposed to the harsh environment during use of the electrochemical sensor.

Shaltry, Michael R.↗