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At least 181 records · Page 10

Preparation, mechanical properties, and toughening mechanisms of SiCw/SiCp‐reinforced zirconia‐toughened alumina ceramics

ABSTRACT Zirconia‐toughened alumina (ZTA) ceramics with high mechanical properties were sintered by hot‐pressing method using SiC particles (SiCp) and SiC whiskers (SiCw) as the reinforcing agents simultaneously. The influences of sintering temperature, SiCp, and SiCw contents on the microstructure and mechanical properties of ZTA ceramics were investigated. It was found that both SiCp and SiCw could contribute to grain refinement significantly and promote the mechanical properties of the ceramics. However, the excess addition of SiCp or SiCw led to the formation of pores with large sizes and degraded the mechanical properties instead. When 13 wt% SiCp was introduced, the maximum flexural strength of 1180.0 MPa and fracture toughness of 15.9 MPa·m 1/2 were obtained, whereas the maximum flexural strength of 1314.0 MPa and fracture toughness of 14.7 MPa·m 1/2 were achieved at 20 wt% SiCw. Interestingly, the simultaneous addition of SiCp and SiCw could further improve the mechanical properties, and the highest flexural strength of 1334.0 MPa and fracture toughness of 16.0 MPa·m 1/2 were achieved at a SiCw/SiCp ratio of 16/4. The reinforcement mechanisms in the ceramics mainly included the phase transformation toughening of ZrO 2 , the crack deflection and bridging of SiCp and SiCw, and the pull‐out of SiCw.

Liu, Longyang↗

The evolution of grain boundary energy in textured and untextured Ca–doped alumina during grain growth

The role of anisotropic grain boundary energy in grain growth is investigated using textured microstructures that contain a high proportion of special grain boundaries. Textured and untextured Ca–doped alumina was prepared by slip casting inside and outside a high magnetic field, respectively. At 1600°C, the textured microstructure exhibits faster growth than the untextured microstructure and its population of low–angle boundaries increases. Atomic force microscopy (AFM) is employed to measure the geometry of thermal grooves to assess the relative grain boundary energy of these systems before and after growth. In the textured microstructure, the grain boundary energy distribution narrows and shifts to a lower average energy. Conversely, the energy distribution broadens for the untextured microstructure as it grows and exhibits abnormal grain growth. Further analysis of the boundary networks neighboring abnormal grains reveals an energy incentive that facilitates their growth. These results suggest that coarsening is not the only dominant grain growth mechanism and that the system can lower its energy effectively by replacing high energy boundaries with those of low energy. The faster growth of lower energy boundaries suggests that isotropic simulations do not adequately account for anisotropic grain growth mechanisms or anisotropic mobility.

36 MATERIALS SCIENCE↗

Vapor phase deposition of alumina on interior surfaces of tritium storage containers

Efficient tritium management and containment are critical challenges for nuclear fusion. To mitigate issues related to permeation into structural materials and isotopic exchange with protium, permeation barriers must be applied to the nonplanar internal surfaces of tritium handling components. In this study, we developed an atomic layer deposition (ALD) system to deposit films on canisters used to store and transport tritium. Growth conditions for deposition of Al 2 O 3 were mapped spatially along the length of a canister using silicon witness samples characterized by ellipsometry, atomic force microscopy, and x-ray reflectivity (XRR). We identified ALD process windows for growth at temperatures between 100 and 140 °C. Furthermore, we compared films grown on our Si witness samples to those grown on polished stainless steel 316 (SS316). X-ray photoelectron spectroscopy indicates two distinct chemical states for the alumina, while XRR confirms that the overall growth rate is similar to the 1.1 Å/cycle that we observed on the Si witness samples.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Corrosion of Chromia-Forming and Alumina-Forming Ferritic Stainless Steels under Dual Atmosphere Exposure Conditions

The surface morphology and chemistry of oxide scales formed on select chromia-forming and alumina-forming ferritic steels have been studied after exposure to a dual atmosphere of hydrogen and air. Localized Fe-rich oxide nodules with surface whiskers/platelets form at the onset of corrosion. The initiation and growth of localized nodules and breakdown of passivation are attributed to the presence of hydrogen, inclusion of iron oxide in the passivating scale, and subsequent growth of iron-rich oxide due to the establishment of redox (H 2 -H 2 O) atmosphere and modification of oxide defect chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Simons Observatory: broadband metamaterial antireflection cuttings for large-aperture alumina optics

Here we present the design, fabrication, and measured performance of metamaterial antireflection cuttings (ARCs) for large-format alumina filters operating over more than an octave of bandwidth to be deployed at the Simons Observatory (SO). The ARC consists of subwavelength features diced into the optic’s surface using a custom dicing saw with near-micrometer accuracy. The designs achieve percent-level control over reflections at angles of incidence up to 20°. The ARCs were demonstrated on four 42 cm diameter filters covering the 75 to 170 GHz band and a 50 mm diameter prototype covering the 200 to 300 GHz band. The reflection and transmission of these samples were measured using a broadband coherent source that covers frequencies from 20 GHz to 1.2 THz. These measurements demonstrate percent-level control over reflectance across the targeted pass-bands and a rapid reduction in transmission as the wavelength approaches the length scale of the metamaterial structure where scattering dominates the optical response. The latter behavior enables use of the metamaterial ARC as a scattering filter in this limit.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Ultra-high Q alumina optical microresonators in the UV and blue bands

UV and visible photonics enable applications ranging from spectroscopic sensing to communication and quantum information processing. Photonics structures in these wavelength regimes, however, tend to experience higher loss than their IR counterpart. Particularly in the near-UV band, on-chip optical microresonators have not yet achieved a quality factor beyond 1 million. Here, we report ultra-low-loss photonic waveguides and resonators patterned from alumina thin films prepared by a highly scalable atomic layer deposition process. We demonstrate ultra high Q factor of 1.5×10 6 at 390 nm, a record value at UV bands, and 1.9×10 6 at 488.5 nm.

He, Chengxing (ORCID:0000000347166078)↗

Solid-state ionics: The key to the discovery and domination of lithium batteries: some learnings from β-alumina and titanium disulfide

We report solid state ionics, the study of fast ion transport in solids, expanded explosively after the discovery of sodium ion transport in b-alumina 50 years ago and has revolutionized energy storage. Lithium ion batteries have come from a dream with titanium disulfide to enabling the communications revolution and are enabling renewable energy. Much can be learnt from these early studies, that will allow the attainment of a fossil-free society and a sustainable environment.

36 MATERIALS SCIENCE↗

pH-Driven Restructuring of Hydration Layers and Cation Ad-sorption at the Alumina-Water Interface

Oxide-water interfaces underpin ion separation, catalysis, and electrochemical energy technologies, where the electrical double layer (EDL) controls adsorption, transport, and reactivity. Yet, the molecular-scale link between pH-dependent surface protonation, hydration-layer structure, and counter-ion adsorption remains poorly defined. Here, we combine in situ crystal truncation rod (CTR) and resonant anomalous X-ray reflectivity (RAXR) with streaming potential measurements and ab initio molecular dynamics (AIMD) simulations to resolve the chemical and structural evolution of the EDL at the single-crystal alumina (012)-water interface in 10 mM Rb+ over pH 3-12. CTR measurements reveal two distinct adsorbed water layers at ~2.2 and ~3.5 Å above the surface that each shift toward the substrate at transition pHs near 6.5 and 10.6, respectively, directly reflecting changes in primary hydration layer structure in response to the deprotonation of bridging and terminal aluminol groups. RAXR shows a 10-fold increase in Rb+ coverage and a decrease in mean adsorption height from ~3.5 to ~2.7 Å with increasing pH, indicating enhanced counter-ion binding accompanied by Stern layer contraction. Streaming potential measurements demonstrate that the zeta potential, i.e., potential at the hydrodynamic shear plane, is positive at pH 3 and becomes negative at pH ≥3.5. This negative charge magnitude increases with increasing pH, consistent with progressive surface deprotonation at higher pH. AIMD identifies inner- and outer-sphere Rb+ complexes whose adsorption heights and coordination geometries depend sensitively on the protonation state of surface oxygens, providing atomistic support for the experimentally inferred trends. These measurements establish two discrete, site-specific pH transitions in hydration-layer structure that track aluminol (de)protonation and quantitatively link them to a pH-driven contraction of the Stern layer (increasing Rb+ coverage and decreasing adsorption height). This provides a direct structural basis for connecting surface acid-base chemistry to ion binding distances at an oxide-water interface.

Electrical double layer (EDL), Surface protonation↗

Progress on Design and Production of Oxide Dispersion–Strengthened Alumina-Forming Austenitic Alloys for Nuclear Applications

Alumina-forming austenitic (AFA) alloys are a promising class of nuclear materials due to their high-temperature oxidation/corrosion resistance and mechanical properties. Unfortunately, these alloys are limited in use for core material applications, specifically in their use as nuclear fuel cladding. Improving these alloys through a fine dispersion of oxide precipitates and thus increasing the effective irradiation sink strength of the alloy system may mitigate many of the degradation phenomena expected during alloy deployment (such as high-temperature helium embrittlement for lead-cooled fast reactor applications). This work package has started using a combination of conventional and advanced manufacturing approaches to the fabrication of oxide dispersion–strengthened (ODS) AFA materials. As such, this report summarizes progress to date in the fabrication of new compositions of these ODS AFA materials with a focus on reactor-specific design and a multifaceted manufacturing approach. Two different compositions of AFA gas-atomized powders were procured, and 200 g of each have been prepared using mechanical alloying with the expectation of high-temperature consolidation in Q1 of FY24. In addition, an approach to use reactive cover gases to promote additional precipitate formation has been developed for implementation in FY24 as a direct comparison with conventionally manufactured alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Status report on HFIR irradiation of optimized alumina forming alloys

Properties of FeCrAl alloys under neutron irradiation are of interest because of these materials’ potential application as accident-tolerant fuel cladding in nuclear systems. In parallel, alumina-forming austenitic (AFA) alloys are of interest for use as structural materials in advanced nuclear systems for their potential higher resistance to embrittlement and high-temperature steam oxidation resistance. An irradiation campaign for fiscal year 2024 has been developed under the Advanced Fuels Campaign to perform irradiation testing of various FeCrAl and AFA alloys in Oak Ridge National Laboratory’s High Flux Isotope Reactor (HFIR). The goals of this irradiation campaign are to (1) study the impact of minor alloying elements on the neutron-irradiated mechanical properties of FeCrAl alloys and (2) collect neutron-irradiated mechanical properties on AFA alloys for comparison with those of FeCrAl alloys. This campaign will include both tensile and fracture toughness specimens tested following HFIR irradiation at temperatures representative of normal operating conditions in light-water reactors. The pre-irradiation characterization to date, the irradiation plan for the FeCrAl and AFA specimens, and the subsequent post-irradiation experimental test plan are presented in this report, along with the status of HFIR builds and scheduled insertion dates.

36 MATERIALS SCIENCE↗

Nanostructured Alumina Forming Austenitic Alloy (NAFA) Production Using Mechanical Alloying and High-Temperature Consolidation

Alumina-forming austenitic (AFA) alloys are a promising class of nuclear materials because of their high-temperature oxidation/corrosion resistance and mechanical properties. Unfortunately, these alloys are limited in use for core material applications, and they are specifically limited for use as nuclear fuel cladding because of their high Ni-transmutation and helium generation rate in-service. Improving these alloys through a fine dispersion of oxide precipitates and thus increasing the effective irradiation sink strength of the alloy system may mitigate many of the degradation phenomena expected during alloy deployment. These phenomena include high-temperature helium embrittlement and cavity swelling for lead-cooled fast reactor applications. This work effort uses combination of conventional and advanced manufacturing approaches are being used to fabricate nanostructured AFA (NAFA) materials. As the first objective of this initiative, a conventional AFA was modified using mechanical alloying and extrusion to alter the precipitation characteristics to include a fine dispersion of nanoscale oxides intended to serve as traps for irradiation-induced point defects and transmuted He within the lattice. This analysis compared the efficacy of the conventional mechanical alloying and extrusion approach with the unalloyed AFA consolidated approach using hot isostatic pressing (HIP). It was found that, although the mechanical alloying approach is successful in producing a fine distribution of oxides within the first nanostructured AFA (NAFA-1), the distribution is heterogeneous because of the mild milling parameters used to prevent cold welding of powder to the spherical milling media. The additional dispersion of oxides, coupled with a higher volume fraction of other secondary phases in the NAFA-1, produces higher alloy strengths that range up to 600°C in comparison to the unalloyed HIP AFA, thus exceeding the operating temperature of lead-cooled fast reactors. However, the strength of the NAFA-1 is lower than that of the HIP AFA at 800°C, which is presumed to be a function of increased secondary phases from the nonoptimized AFA chemistry. Future work is planned on a newly procured NAFA-2 chemistry that is more suitable for advanced reactor applications exploring new manufacturing routes.

36 MATERIALS SCIENCE↗

Microwave-assisted dehydrogenation of fossil fuels using iron-based alumina nanocomposites

Hydrogen is mainly produced via steam reforming of methane and gasification of coal, with enormous CO 2 emissions in both cases. Microwave-assisted thermocatalytic decomposition (pyrolysis) is of interest as a method for hydrogen production from fossil fuels with no CO 2 emissions. For successful implementation of this technology, it is necessary to develop decomposition catalysts that are also good microwave absorbers and can be produced from inexpensive materials via a robust synthetic route. Recently, iron-based alumina nanocomposites, fabricated by solution combustion synthesis (SCS), have shown promising microwave-absorbing and catalytic properties in the pyrolysis of plastics. The reported project explored the feasibilities of improving such catalysts and using them for the microwave-assisted pyrolysis of liquid fossil fuels, viz., diesel fuel, gasoline, and crude oil. The research focused on how SCS parameters affect the material properties and pyrolysis performance.

02 PETROLEUM↗

Nanostructured Alumina Forming Austenitic Alloy (NAFA) Production using Advanced Manufacturing

Alumina-forming austenitic (AFA) alloys are well known for their exceptional corrosion-resistant properties due to the formation of a dense oxide scale beneficial in their application as a nuclear material. However, use of the alloys in core material applications is limited due to the high nickel-transmutation and helium generation rate in service, leading to swelling and reduced lifetimes. Enhancing the sink strength to pin gas bubbles and increasing gas management of the material may mitigate many of the degradation phenomena expected during alloy deployment (such as high-temperature helium embrittlement and cavity swelling for lead-cooled fast-reactor applications). Nanostructured materials are usually produced using a time-consuming and expensive batch process like mechanical alloying to achieve the fine homogenous distribution of nanoprecipitates throughout the matrix material. Integrating the nanoprecipitates in modern additive manufacturing processes has proven difficult, as the required nano-sizes or number densities cannot be achieved simultaneously. Efforts to increase the number density of precipitates by adding more precipitate-forming rare-earth elements led to agglomeration of such elements, while the nano-sized precipitates did not form in sufficient quantity when not enough rare-earth element was use. In this work a novel approach to advanced manufacturing and the fabrication of Nanostructured AFA (NAFA) materials was chosen. A dual precipitate-forming NAFA steel with a chemistry more suitable for advanced reactor applications was produced to create an environmentally resistant, high-sink-strength austenitic alloy for advanced reactor cladding applications.

36 MATERIALS SCIENCE↗

Nanostructured Alumina-Forming Austenitic Alloy (NAFA) Production Using Advanced Manufacturing

Alumina-forming austenitic (AFA) alloys are well known for their exceptional corrosion-resistant properties due to the formation of a dense oxide scale beneficial in their application as a nuclear material. However, use of the alloys in core material applications is limited due to the high nickel-transmutation and helium generation rate in service, leading to swelling and reduced lifetimes. Enhancing the sink strength to pin gas bubbles and increasing gas management of the material may mitigate many of the degradation phenomena expected during alloy deployment (such as high-temperature helium embrittlement and cavity swelling for lead-cooled fast-reactor applications). Nanostructured materials are usually produced using a time-consuming and expensive batch process like mechanical alloying to achieve the fine homogenous distribution of nanoprecipitates throughout the matrix material. Integrating the nanoprecipitates in modern additive manufacturing processes has proven difficult, as the required nano-sizes or number densities cannot be achieved simultaneously. Efforts to increase the number density of precipitates by adding more precipitate-forming rare-earth elements led to agglomeration of such elements, while the nano-sized precipitates did not form in sufficient quantity when not enough rare-earth element was use. In this work a novel approach to advanced manufacturing and the fabrication of Nanostructured AFA (NAFA) materials was chosen. A dual precipitate-forming NAFA steel with a chemistry more suitable for advanced reactor applications was produced to create an environmentally resistant, high-sink-strength austenitic alloy for advanced reactor cladding applications.

36 MATERIALS SCIENCE↗

Block Copolymer-Templated Synthesis of Fe–Ni–Co-Modified Nanoporous Alumina Films

Despite intense interest in the catalytic potential of transition metal oxide heterostructures, originating from their large surface area and tunable chemistry, the fabrication of well-defined multicomponent oxide coatings with controlled architectures remains challenging. Here, we demonstrate a simple and effective swelling-assisted sequential infiltration synthesis (SIS) strategy to fabricate hierarchically porous multicomponent metal-oxide electrocatalysts with tunable bimetallic composition. A combination of solution-based infiltration (SBI) of transition metals, iron (Fe), nickel (Ni), and cobalt (Co), into a block copolymer (PS73-b-P4VP28) template, followed by vapor-phase infiltration of alumina using sequential infiltration synthesis (SIS), was employed to synthesize porous, robust, conformal and transparent multicomponent metal-oxide coatings like Fe/AlO x , Fe+Ni/AlO x , and Fe+Co/AlO x . Electrochemical assessments for the oxygen evolution reaction (OER) in a 0.1 M KOH electrolyte demonstrated that the Fe+Ni/AlO x composite exhibited markedly superior catalytic activity, achieving an impressive onset potential of 1.41 V and a peak current density of 3.29 mA/cm 2 . This superior activity reflects the well-known synergistic effect of alloying transition metals with a trace of Fe, which facilitates OER kinetics. Overall, our approach offers a versatile and scalable path towards the design of stable and efficient catalysts with tunable nanostructures, opening new possibilities for a wide range of electrochemical energy applications.

conformal films↗

Chromium oxide coatings improve thermal emissivity of alumina

Chromium oxide coatings improve thermal radiation characteristics of alumina-coated heater-cathode systems in vacuum tubes. Chromium oxide is applied either as a surface layer or as a doping material. The new coatings eliminate the high temperature migration problems of carbon surface treatments.

Upshaw, V.↗