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DOE OSTI2020

Defect accommodation in off-stoichiometric (SrTiO 3 ) n SrO Ruddlesden–Popper superlattices studied with positron annihilation spectroscopy

he low dielectric loss underlying the record performance of strained (SrTiO 3 ) n SrO Ruddlesden–Popper films as tunable microwave dielectrics was postulated to arise from (SrO) 2 faults accommodating local non-stoichiometric defects. Here, we explore the effect of non-stoichiometry on (SrTiO 3 ) n SrO using positron annihilation lifetime spectroscopy on a composition series of 300 nm thick n = 6 (Sr 1+δ TiO 3 ) n SrO thin films. These films show titanium-site vacancies across the stoichiometry series, with evidence that TiO x vacancy complexes dominate. Little change in defect populations is observed across the series, indicating the ability of Ruddlesden–Popper phases to accommodate ± 5% off-stoichiometry. This ability for defect accommodation is corroborated by scanning transmission electron microscopy with electron energy loss spectroscopy.

Physics↗

NASA NTRS1991

Selective and low temperature synthesis of polycrystalline diamond

Polycrystalline diamond thin films have been deposited on single-crystal silicon substrates at low temperatures (not above 600 C) using a mixture of hydrogen and methane gases by high-pressure microwave plasma-assisted chemical vapor deposition. Low-temperature deposition has been achieved by cooling the substrate holder with nitrogen gas. For deposition at reduced substrate temperature, it has been found that nucleation of diamond will not occur unless the methane/hydrogen ratio is increased significantly from its value at higher substrate temperature. Selective deposition of polycrystalline diamond thin films has been achieved at 600 C. Decrease in the diamond particle size and growth rate and an increase in surface smoothness have been observed with decreasing substrate temperature during the growth of thin films. As-deposited films are identified by Raman spectroscopy, and the morphology is analyzed by scanning electron microscopy.

Ramesham, R.↗

NASA NTRS2008

Effect of Weld Tool Geometry on Friction Stir Welded Ti-6Al-4V

In this study, flat 0.250" thick Ti-6Al-4V panels were friction stir welded (FSWed) using weld tools with tapered pins. The five different pin geometries of the weld tools included: 0 degree (straight cylinder), 15 degree, 30 degree, 45 degree, and 60 degree angles on the frustum. All weld tools had a smooth 7 degree concave shoulder and were made from microwave sintered tungsten carbide. For each weld tool geometry, the FSW process parameters were optimized to eliminate internal defects. All the welds were produced in position control with a 2.5 degree lead angle using a butt joint configuration for the panels. The process parameters of spindle rpm and travel speed were varied, altering the hot working conditions imparted to the workpiece. Load cells on the FSWing machine allowed for the torque, the plunge force, and the plow force to be recorded during welding. Resulting mechanical properties were evaluated from tensile tests results of the FSWjoints. Variations in the material flow were investigated by use of microstructural analysis including optical microscopy (OM), scanning electron microscopy (SEM), and orientation image mapping (aIM).

Querin, Joseph A.↗

NASA NTRS1990

Silicon carbon alloy thin film depositions using electron cyclotron resonance microwave plasmas

Amorphous and microcrystalline silicon carbon films (a-SiC:H, micro-c-SiC:H) have been deposited using SiH4, CH4 and H2 mixed gas ECR (electron cyclotron resonance) plasmas. The optical bandgap of a-SiC:H films is not dependent on the hydrogen dilution in the ECR plasma. The deposition rate of a-SiC:H films is found to be strongly dependent on the ECR magnetic field and the hydrogen dilution. The hydrogen dilution effect on the deposition rate indicates that the etching in ECR hydrogen plasmas plays an important role in the deposition of a-SiC:H films. The optical constants n and k of ECR-deposited a-SiC:H films in the wavelength region of 0.4 to 1.0 micron are determined to be 2.03-1.90 and 0.04-0.00, respectively. The microstructures of ECR-deposited micro-c-SiC:H films are shown by X-ray diffraction and SEM (scanning electron microscopy) to be composed of 1000-A alpha-SiC microcrystallites and amorphous network structures.

Shing, Y. H.↗

DOE OSTI2023

Abstract for CRADA between NETL and the University of Massachusetts Lowell (AGMT-1275)

The demand for printed electronics over conventional electronics is growing each year due to their low costs, low material waste during manufacturing, and compatibility with flexible substrates. The development of inks for printed electronics is a challenge because each printing technology requires different viscosities and curing behaviors to create devices with controlled structures at the micron scale, or smaller. Carbon is a great candidate for fabricating printed electronics devices because it is inexpensive and earth abundant, easily functionalized to impart miscibility with solvent systems, and has electrical properties that can be tuned from insulating to conducting. Despite these advantages, carbons are rarely used for printed electronics because there is a scarcity of inks available for non-contact printing technologies. To address these challenges, the National Energy Technology Laboratory (NETL) will collaborate with the University of Massachusetts Lowell (Participant) through its Printed Electronics Research Collaborative (PERC) to develop engineered carbons and ink formulations optimized specifically for printing radio- and microwave-frequency electronic devices using ink jet, aerosol jet, syringe dispensing, and other additive manufacturing techniques. NETL will process coal, petroleum, and other carbon feedstocks to make engineered carbons with the appropriate composition, microstructure, surface functionalization, and particle morphologies needed to stabilize ink suspensions and impart useful electronic properties to printed devices. The University of Massachusetts Lowell will utilize these engineered carbons to determine which solvent systems and ink additives are needed to achieve the appropriate viscosity, stability, and printability to make useful ink formulations. The University of Massachusetts Lowell will then utilize these inks to manufacture printed resistors and conductors using inkjet, aerosol jet, and syringe dispensing printing methods and will characterize device performance using four-point probe resistivity measurements, contact angle measurements to assess wettability, adhesion evaluation to various substrates, and focused ion beam and scanning electron microscopy for surface and density investigations of printed devices.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Hyperspectral X-ray Imaging: Progress Towards Chemical Analysis in the SEM

The Hyperspectral X-ray Imaging (HXI) project will enable non-destructive chemical-state determination of nano-scale samples in the electron microscope for nuclear safeguards applications. To efficiently measure chemical state through electron-excited X-ray emission requires a combination of wide spectral bandwidth, high resolution, and high count rate capability. We are building a next-generation X-ray detector based on an array of transition edge sensors (TESs) to make these measurements possible and routine in the scanning electron microscope (SEM). Leveraging the large pixel densities afforded by microwave multiplexing readout and continuous, uninterrupted operation of a cryogen-free dilution refrigerator, this instrument will have efficiency to allow chemical species identification of nano-scale samples in hours instead of days to weeks. We describe prototype pixel designs for this HXI instrument, comprising three pixel types that will make up the hybrid TES array. Engineering design of the integrated HXI cryostat and SEM system is in progress, with full detector commissioning expected in Spring 2021 followed closely by full-scale integration with the SEM. Furthermore, we also report on the commissioning of a complementary TES-based X-ray emission spectroscopy platform for bulk samples to build a spectral library for HXI sample identification.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Solution combustion synthesis of iron-based alumina nanocomposites for clean production of hydrogen from fossil fuels

Iron-based alumina nanocomposites are promising materials for microwave-assisted thermocatalytic dehydrogenation of fossil fuels, which has been proposed for the production of hydrogen with no CO2 emissions. Solution combustion synthesis (SCS) is an attractive technique for the fabrication of these materials because it has been used for synthesis of many nanoscale oxides. However, SCS can be carried out using different organic fuels and different heating equipment, and it is important to determine which fuel and heating mode generate materials with the best properties for dehydrogenation, such as maximized specific surface area. In the present work, the iron-based alumina nanocomposites were obtained by SCS using two different fuels (citric acid and glycine) and two different heating modes (a hotplate and a muffle furnace). The precursors/oxidizers were iron nitrate and aluminum nitrate. They were mixed with the fuel according to stoichiometry and dissolved in water. Heating the solution resulted in combustion synthesis. The products were characterized by X-ray diffraction analysis, Brunauer-Emmett-Teller surface area analysis, laser diffraction particle size analysis, scanning electron microscopy, and energy dispersive X-ray spectroscopy. The experiments have shown that the specific surface area of the iron-based alumina nanocomposites obtained by SCS can be dramatically increased by using citric acid instead of glycine, and additionally by using a muffle furnace instead of a hotplate.

Solution combustion synthesis, Nanoscale metal oxi↗

DOE OSTI2024

Probabilistic Analysis of Long-Term Degradation of Microwave Cavity Flow Sensor

We are investigating a microwave resonant cavity transducer for flow sensing in the vessel of a high temperature fluid advanced reactor (AR), such as a molten salt cooled reactor (MSCR) or a sodium fast reactor (SFR). This transducer is a hollow metallic cylindrical cavity, with the flat wall of the cylinder flexible enough to undergo microscopic deflection due to dynamic fluid pressure. Membrane deflection leads to a shift in the resonant frequency, which can be detected with a spectrum analyzer. We have performed a proof-of-concept experiment of flow sensing with the transducer in liquid sodium at 340°C in impinging liquid jet geometry. The transducer remained in liquid sodium for 70 days. After removal, no structural damage was observed, and the expected transducer response was verified in a water test. Because long-term (multi-year) experimental tests of transducer resilience to harsh environment are not practical, we have developed a probabilistic model of creep to estimate transducer resilience to the harsh environment. The probabilistic model considers diffusion creep under the condition of high temperature and low stress, where the stress and temperature are allowed to be random variables with Gaussian distributions. Using the probabilistic model, we estimate inelastic membrane deflections due to creep for several temperature ranges. We conclude that for temperatures less than 650°C, creep has negligible long-term effect on the transducer performance. Since a yellowish residue was observed on the transducer surface after 70 days of immersion in liquid sodium, we have investigated possible evidence of corrosion. Chromium depletion is a typical indicator of the corrosion process in stainless steel. Scraping off a residue from the transducer and performing scanning electron microscopy (SEM) with energy dispersive analysis (EDS) did not find any chromium in the residue. Approximately 60% of the residue consisted of copper, which can be attributed to contamination of sodium due to powder residue from machining of copper and brass components of the transducer.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗