Compatibility of alumina and beryllia ceramics with potassium vapor.
Alumina and beryllia ceramics compatibility with potassium vapor, discussing modes of attack and low silica level
Lindberg, R.↗
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Chemical interaction and compatibility of uranium mononitride and alumina forming austenitic stainless steel
Uranium mononitride (UN) and alumina forming austenitic (AFA) stainless steel are a potential fuel-cladding combination for the lead-cooled fast reactor (LFR). Chemical compatibility between UN and AFA steel needs to be verified before implementation in a nuclear reactor. Diffusion couple experiments at 823 K and 1023 K were conducted for nonirradiated UN samples in contact with as-cast (no thermally grown Al 2 O 3 ) and preoxidized (with thermally grown Al 2 O 3 ) AFA for 500 and 1000 h in an inert environment. Preoxidized AFA exhibited little to no interaction with all UN samples tested at both 823 K and 1023 K, displaying the stability and capability of the Al 2 O 3 layer to prevent chemical interaction and inter-diffusion with UN. Chemical interaction occurs between UN and as-cast AFA. At 1023 K, an aluminum and nitrogen rich phase (likely AlN) formed along the interface of as-cast AFA and UN samples. At 823 K the AlN phase was not prominently observed due to the reduced diffusivity of aluminum through AFA. The aluminum and nitrogen-enriched phase was also observed in a high temperature pressure-assisted test sample of UN and as-cast AFA thermally treated at 1373 K. Finally, in UN samples doped with a low weight percent of UO 2 (< 3 wt%), AlN was not detected along the interface at either temperatures, and an Al 2 O 3 layer likely formed along the interface and prevented further chemical interaction between UN and as-cast AFA.
36 MATERIALS SCIENCE↗
Developments in Processing Criteria for Iron Phosphate Waste Form Design for Treating Electrorefiner Salt Wastes
This report describes work done under a Nuclear Energy University Partnership (NEUP) project that included a collaborative effort between Pacific Northwest National laboratory, University of Nevada Reno, University to Utah, and Missouri University of Science and Technology. In this project, the main goals were the following: (1) to assess H3PO4 dechlorination parameters for halide removal from salt simulants, (2) to evaluate crucible compatibility with iron phosphate glass melts, and (3) to evaluate waste form properties within a ternary system of P2O5 (added as H3PO4), Fe2O3 and fission product simulants.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Thermal expansion compatibility of ceramic chip capacitors mounted on alumina substrates.
The thermal expansion coefficients of a representative sample of BaTiO3 and TiO2 ceramic chip capacitors and alumina substrates have been examined. These data have revealed large potential mechanical stresses under thermal cycling. A mathematical analysis of a composite model of the capacitor to predict the thermal expansion and modulus of elasticity and an analysis of the capacitor-substrate system to predict the magnitude of thermally induced stresses have been conducted. In all cases studied, thermally induced stresses great enough to cause capacitor body rupture or termination failure was predicted.
Allen, R. V.↗
CMOS-fabricated ultraviolet light modulator using low-loss alumina piezo-optomechanical photonics
Ultra-violet (UV) and near-UV wavelengths are necessary for many important optical transitions for quantum technologies and various sensing mechanisms for biological and chemical detection. However, all well-known photonic platforms have excessively high losses in the UV, which has prevented photonic integrated circuits (PICs) being used to address these and other important application spaces. Photonic waveguides using low-loss alumina cores and silicon dioxide cladding have emerged as a promising solution because of alumina’s large optical bandgap and the high quality of films enabled by atomic layer deposition. These properties allow passive, low-loss waveguide operation down to at least 266 nm using multimode widths. However, to the best of our knowledge, active alumina PICs have only been realized using thermo-optic tuning, which precludes switching speeds shorter than approximately 100 microseconds, high circuit densities, and cryogenically compatible operation. Here, we introduce a CMOS-fabricated, piezo-optomechanical PIC platform using alumina waveguides and piezoelectric aluminum nitride strain actuators. The platform allows for sub-microsecond switching times, high circuit densities, and cryogenic operation which is desired in many UV PIC applications. We demonstrate a high-performance, reconfigurable optical filter operating at wavelengths as low as 320 nm. The filter has a 6-nanosecond switching time, a loaded linewidth of 3.3 GHz, tuning rate of 28 V/linewidth, and a hold power of less than 20 nW at one linewidth detuning. This work establishes the foundations for a new class of CMOS-fabricated, rapidly reconfigurable, and low-power UV photonic circuits compatible with wavelengths as low as 225 nm.
Castillo, Zachary A. [Sandia National Laboratories↗
Investigation of Solid Particle Reactors for Nonoxidative Dehydrogenation of Ethane: Toward Solar Thermal Ethylene Production
Concentrating solar power plants can generate renewable heat at temperatures well above those of most industrial processes. Ceramic particles irradiated with concentrated sunlight can store high-quality sensible heat and transfer this to power generation systems. These concepts and materials hold great potential to also enable thermal processes in the chemical industry, but effective strategies for transferring heat from thermal energy storage media into chemical reactors are still under development. This present work evaluated the thermal and chemical compatibility of various solid particle media (including quartz, bauxite, and alumina particles) integrated directly into tube reactors and the subsequent effects on reactor performance for the nonoxidative dehydrogenation of ethane reaction. Empty tube reactors without loaded particles (representing conventional ethane cracking coils) showed significant heat transfer limitations as the tube diameter was scaled. The incorporation of media into the reactor significantly aided heat transfer to the gaseous ethane reactant and increased its conversion by as much as 10% at similar space velocities. Despite direct contact with hydrocarbon gases, alumina and quartz media showed negligible coke formation. Even during reaction in 100% ethane feed gas at 825 °C, the average selectivity of the coke product was only 0.57% when using the quartz media. These materials further demonstrated excellent thermal stability during subsequent reoxidation in air at 800 °C, which simulated the reheating of particles in a circulating particle solar receiver. Conversely, high rates of coke formation, with a product selectivity of 27.5%, were observed on sintered bauxite particles during the reaction, likely promoted by transition metal constituents. These particles fractured upon reoxidation due to exotherms generated from coke combustion. In conclusion, while the use of cofed steam could mitigate attrition of redox-active particles, the ability of inert metal oxide particles to efficiently transfer heat to concentrated ethane reactant gas while suppressing side reactions or degradation suggests that these media could effectively couple solar thermal plants to reactors for next-generation production of ethylene and other critical chemicals.
Hydrocarbons↗
Durability of YSZ Coated Ti2AlC in 1300 °C Mach 0.3 Burner Rig Tests
A thermal barrier coating system survived burner rig testing at 1300 °C for 500 h. A 160 µm thick yttria stabilized zirconia (YSZ) coating was applied to a Ti2AlC MAX phase bar sample by plasma spray physical vapor deposition (PS-PVD) and tested face-on in an atmospheric Mach 0.3 jet fuel burner, using 5-h thermal cycles. No thermal barrier coating (TBC) spallation or recession was observed, only a 2.4 mg/cm2 mass gain. The modest weight gain precluded severe volatility losses under high velocity burner conditions. The coating surface exhibited colonies of (111)flourite fiber-textured columns separated by craze patterns, with no visible moisture attack. The metastable tetragonal t' YSZ phase was obtained initially, transitioning to equilibrium teq and cubic YSZ, but with little detrimental monoclinic. The thickness of the alumina TGO was ~21 to 23 μm under the heated YSZ face and ~13 to 15 μm on the uncoated, cooler backside. The backside exhibited removal of initial transient TiO2 nodules and partial etching of the underlying Al2O3 scale by volatile hydroxides formed in high temperature, high velocity water vapor. Aerodynamic forces produced some bending of the cantilevered sample via creep. The test indicated exceptional stability of YSZ coatings on Ti2AlC under turbine conditions, with thermal expansion matching playing a key role. The purpose of this study was to demonstrate long term durability of YSZ/MAX phase system in aggressive high temperature burner rig testing. MAX phases have been keenly studied because of their unique crystal structure and intriguing properties (Refs. 1 and 2). Having Mn+1(Al,Si)(C,N)n general composition, they are defined as ceramics, but possess unusual desirable attributes such as high conductivity, thermal shock resistance, easy machinability, and deformation tolerance. The mechanical properties derive from weak M-(Al,Si) bonding in the basal plane that leads to sliding and kinking in preference to catastrophic crack growth. Like most ceramics they are phase stable at high temperatures, generally up to 1500 °C. High temperature oxidation resistance is excellent for alumina-forming Ti3AlC2, Ti2AlC, and Cr2AlC, as reviewed by Tallman, et al. (Ref. 3). Compatibility with α-Al2O3 scales is further enhanced in cyclic exposures by a close matching of thermal expansion coefficients, (Ref. 4) i.e., (~9.3, 10.2, 11.3×10–6/K for Al2O3, Ti2AlC, and YSZ, to be discussed). Turbine environments generally contain 10 percent water vapor in the combustion gases, therefore moisture effects can be a concern for some materials (Ref. 5). Furnace tests of MAX phases in high temperature steam generally showed little effect on Al2O3 scale growth (Ref. 6). However, high velocity and high pressure gas can influence scale losses by the formation of volatile reaction products, such as TiO(OH)2 and Al(OH)3 (Refs. 7 to 10). This phenomenon had been discussed for 1100 to 1300 °C high pressure burner rig tests of Ti2AlC (Ref. 11). A single cubic growth rate parameter kcubic was measurably lower than comparable furnace TGA data, but it could be matched reasonably well if corrected for a slight volatility term. In general, a two-parameter cubic-linear growth-volatility law was believed to apply. Corresponding scale volatility loss rates, directly measured at 1300 °C on a pre-oxidized sample, were moderate (0.012 mg/cm2/h) and largely attributed to removal of the initial TiO2 transient scale. A related CH4 burner study of high purity Cr2AlC MAX phase demonstrated 1200 °C durability after 500 rapid (5 min. heat and 2 min. cool) thermal shock cycling (29 h hot time) (Ref. 12). Heating and cooling rates were ~1000 and 500 °C per minute, with a gas velocity of 5 m/s, producing a 75 °C/mm gradient. A 7 μm Al2O3 surface scale and a 13 μm Cr7C3 depletion zone formed with no signs of failure. No evidence of scale volatility was evident, although weight change was not provided, the velocity was moderate, and the total hot time was not extensive. The same high gradient BRT was used to produce 1400 °C surface temperatures for a YSZ/Cr2AlC/IN738 system in the first study of MAX phases used as bond coats for thermal barrier coatings (TBC) (Ref. 25). Here TBC failure was reported after 745 cycles, with only a 1.5 μm Al2O3 scale entrained within a porous, Cr7C3 bondcoat depletion phase. YSZ thermal barrier coatings have been considered to be a compatible complement to Al-MAX phases because of thermal expansion matching and extremely low volatility in water vapor. Initial studies showed superior oxidative stability up to 1300 °C, for long times (at least 500 h) for Ti2AlC substrates and less (268 h) for Cr2AlC, while withstanding large alumina TGO scale thickness (~35 to 40 μm) (Refs. 13 and 14). By comparison, typical superalloy systems can only survive 1150 °C maximum interface temperatures for extended periods, with a maximum sustained TGO below 10 μm (Ref. 15). High temperature SiC based systems are known to form slow-growing SiO2 scales. But these are subject to rate enhancement and volatile Si(OH)4 products in the presence of water vapor, as described comprehensively by Opila, et al. (Refs. 5, 16 to 19). Net weight losses are generally observed in high velocity, high pressure burner rig studies (e.g., 0.084 mg/cm2/h at 1300 °C) (Ref. 20). Furthermore, the loss rates have been shown from chemical physics to scale with v1/2 and pH2O 2 (Ref. 16). Low activity, moisture-resistant environmental barrier coatings (EBC), such as rare earth silicates, are needed to prevent substrate recession under turbine conditions (Refs. 21 to 23).
Smialek, James L.↗
Electrical and Dielectric Characterizations of HTCC Electronic Packages for High Temperature Harsh Environment Applications
A prototype high temperature co-fired ceramic (HTCC) alumina packaging system composed of a 32-I/Os package and a compatible circuit board was previously developed and demonstrated for long term operation in 500 °C environments. The electrical / dielectric parasitic parameters of that chip level package were characterized and reported. This co-fired packaging system with platinum (Pt) conductor has successfully facilitated tests of silicon carbide (SiC) analog and digital integrated circuits (ICs) developed at NASA GRC at 500°C for up to 10,000 hours in ambient oven environment and 60 earth days in Venus surface environment with simulated temperature, pressure, and chemical constituents. Based on these previous results, this paper introduces new designs of Pt-HTCC packages with 16, 24, and 44 I/Os for packaging a new generation SiC ICs with 8, 24, 56, 62, and 72 I/Os to be tested in high temperature harsh environments. The package with 44 I/Os is specifically designed for the new SiC ICs with 56, 62, and 72-I/Os and electrical connection needs, the power pads of this package are consolidated, and an array of I/O pads distributed on separated vertical levels (inside the package) is used to control the overall package dimensions and mitigate the parasitic effects at high temperatures. This paper will present the detailed design of these chip-level packages and results of electrical and dielectric characterization of these newly fabricated chip-level Pt-HTCC packages.
High temperature↗
Electrical and Dielectric Characterizations of HTCC Electronic Packages for High Temperature Harsh Environment Applications
A prototype high temperature co-fired ceramic (HTCC) alumina packaging system composed of a 32-I/Os package and a compatible circuit board was previously developed and demonstrated for long term operation in 500 °C environments. The electrical / dielectric parasitic parameters of that chip level package were characterized and reported. This co-fired packaging system with platinum (Pt) conductor has successfully facilitated tests of silicon carbide (SiC) analog and digital integrated circuits (ICs) developed at NASA GRC at 500°C for up to 10,000 hours in ambient oven environment and 60 earth days in Venus surface environment with simulated temperature, pressure, and chemical constituents. Based on these previous results, this paper introduces new designs of Pt-HTCC packages with 16, 24, and 44 I/Os for packaging a new generation SiC ICs with 8, 24, 56, 62, and 72 I/Os to be tested in high temperature harsh environments. The package with 44 I/Os is specifically designed for the new SiC ICs with 56, 62, and 72-I/Os and electrical connection needs, the power pads of this package are consolidated, and an array of I/O pads distributed on separated vertical levels (inside the package) is used to control the overall package dimensions and mitigate the parasitic effects at high temperatures. This paper will present the detailed design of these chip-level packages and results of electrical and dielectric characterization of these newly fabricated chip-level Pt-HTCC packages.
High temperature↗
Mechanical and Structural Behavior of Granular Material Packed Beds for Space Life Support System Applications
Long-term human mission to space, such as living in International Space Station (ISS), Lunar, and Martian bases, and travel to Mars, must m ake use of Advanced Life Support Systems (ALSS) to generate and recycle critical life supporting elements like oxygen and water. Oxygen Gen eration Assembly (OGA) and Water Processor Assembly (WPA), critical c omponents of ALSS, make use of series of granular material packed beds for generation and recycling of oxygen and water. Several granular m aterials can be used for generation, recycling, processing and recovery of oxygen and water. For example, they may include soft bed media, e.g. ion exchange resins for oxygen generation assembly and hard bed media such as, activated alumina, magchem (Magnesium oxide) and activa ted carbon to remove organic species like ethanol, methanol, and urea from wastewater in Water recovery/processing assembly. These beds are generally packed using a plate-spring mechanism to provide sufficien t compaction to the bed media throughout the course of operation. This paper presents results from an experimental study of a full-scale, 3 8.1 cm (15 inches) long and 3.7 cm (1.44 inches) diameter. activated alumina bed enclosed in a cylinder determining its force-displacement behavior, friction mobilizing force, and axial normal stress distribu tion under various axially applied loads and at different levels of packing. It is observed that force-displacement behavior is non-linear for low compaction level and becomes linear with increase in compaction of the bed media. Axial normal stress distribution along the length of the bed media decreased non-linearly with increase in depth from the loading end of the granular media. This paper also presents experimental results on the amount of particulates generated corresponding to various compaction levels. Particulates generated from each of the tests were measured using standard US sieves. It was found that the p articulates and the overall displacement of the bed media increased with decrease in initial compaction of the bed media. This effect could be attributed to the greater tendency for inter-particle sliding/rub bing due to smaller internal friction angles, as seen from the shear tests, at lesser initial compacted levels. Upon unloading, it was obse rved that there was no change in displacement (especially rebounding) in the bed media. This effect could be attributed to the fact that th e porous activated alumina particles fracture/break upon increase in applied load (during loading phase) and occupy void spaces in between the material grains; thereby leading to settling of the media. The lo ad-displacement curve becomes more linear with increase in initial compaction of the bed media. It is concluded that compaction considerabl y affects the load-displacement behavior of the bed media. A series of tests were also conducted on the packed bed media to determine the f orce required to mobilize the friction between the bed media and the housing cylinder. The results from these tests showed the existence of significant friction between the bed media and the encasing stainles s steel cylinder. Further, it was found that friction effects were more pronounced for media with higher initial compaction. Internal frict ion of the granular media was measured using direct shear apparatus. It was observed that the internal friction increased with increase in initial compaction of the bed media. In this study, a computational m odel (CM) is also developed using finite element software ANSYS to verify experimental results obtained for the distribution of the axial n ormal stress and axial displacement along the length of the full-scal e activated alumina bed media. In the computational model, the granular material is considered to have appropriate failure and frictional c ontact exists between the wall and the granular media. It is observed that the model predicts results closely with the experimental method. The compational results show that the axial normal stress distribution along the length of the activated alumina media decreases non-linea rly from the loading end and is negligible beyond a certain depth. Th is can be attributed to the existence of friction between the walls and the media and that the friction takes up most of the applied load.
Malla, Ramesh B.↗
Process for High-Rate Fabrication of Alumina Nanotemplates
An anodizing process, at an early stage of development at the time of reporting the information for this article, has shown promise as a means of fabricating alumina nanotemplates integrated with silicon wafers. Alumina nanotemplates are basically layers of alumina, typically several microns thick, in which are formed approximately regular hexagonal arrays of holes having typical diameters of the order of 10 to 100 nm. Interest in alumina nanotemplates has grown in recent years because they have been found to be useful as templates in the fabrication of nanoscale magnetic, electronic, optoelectronic, and other devices. The present anodizing process is attractive for the fabrication of alumina nanotemplates integrated with silicon wafers in two respects: (1) the process involves self-ordering of the holes; that is, the holes as formed by the process are spontaneously arranged in approximately regular hexagonal arrays; and (2) the rates of growth (that is, elongation) of the holes are high enough to make the process compatible with other processes used in the mass production of integrated circuits. In preparation for fabrication of alumina nanotemplates in this process, one first uses electron-beam evaporation to deposit thin films of titanium, followed by thin films of aluminum, on silicon wafers. Then the alumina nanotemplates are formed by anodizing the aluminum layers, as described below. In experiments in which the process was partially developed, the titanium films were 200 A thick and the aluminum films were 5 m thick. The aluminum films were oxidized to alumina, and the arrays of holes were formed by anodizing the aluminum in aqueous solutions of sulfuric and/or oxalic acid at room temperature (see figure). The diameters, spacings, and rates of growth of the holes were found to depend, variously, on the composition of the anodizing solution, the applied current, or the applied potential, as follows: In galvanostatically controlled anodizing, regardless of the chemical composition of the solution, relatively high current densities (50 to 100 mA/cm2) resulted in arrays of holes that were more nearly regular than were those formed at lower current densities. . The rates of elongation of the holes were found to depend linearly on the applied current density: the observed factor of proportionality was 1.2 (m/h)/(mA/cm2). For a given fixed current density and room temperature, the hole diameters were found to depend mainly on the chemical compositions of the anodizing solutions. The holes produced in sulfuric acid solutions were smaller than those produced in oxalic acid solutions. The arrays of holes produced in sulfuric acid were more ordered than were those produced in oxalic acid. . The breakdown voltage was found to decrease logarithmically with increasing concentration of sulfuric acid. The breakdown voltage was also found to decrease with temperature and to be accompanied by a decrease in hole diameter. The hole diameter was found to vary linearly with applied potential, with a slope of 2.1 nm/V. This slope differs from slopes (2.2 and 2.77 nm/V) reported for similar prior measurements on nanotemplates made from bulk aluminum. The differences among these slopes may be attributable to differences among impurities and defects in bulk and electron-beam-evaporated aluminum specimens.
Myung, Nosang↗
Pt/HTCC Alumina based Electronic Packaging System and Integration Processes for High Temperature Harsh Environment Applications
Electronic devices capable of operation at 500°C are required for long term Venus surface missions, as well as for in situ monitoring and control of next generation aeronautical engines. High temperature sensors and electronics can also find many applications in military, and energy and automobile industries. Various silicon carbide (SiC) sensors and electronic devices have been developed for operation at 500 °C, and a compatible packaging system is needed for long term test and deployment of these high temperature devices. High temperature co-fired ceramics (HTCC) alumina with platinum (Pt) conductor was proposed for high temperature electronic packaging. A prototype Pt/HTCC alumina packaging system including chip-level package and circuit board has been briefly reported previously for long-term electrical testing of SiC integrated circuits at 500 °C, and brief testing at much higher temperatures. HTCC alumina is an excellent dielectric material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. Pt is chemically noble and can be co-fired with HTCC alumina in air ambient producing a viable electronic packaging material system for high temperature applications. This paper presents a more detailed description of this packaging system including prototype low power packages and circuit boards based on HTCC alumina and Pt metallization for 500°C and other harsh environment applications. The key technical considerations for chip-level packaging and circuit board assembly, including materials and processes for 500 °C durable wire-bonding and SiC die attach, and integration of multi-chip circuit boards, are presented. Experimental test results of this packaging approach applied to SiC integrated circuits at 500 °C and 700°C are discussed as well.
High temperature↗
Pt/HTCC Alumina based Electronic Packaging System and Integration Processes for High Temperature Harsh Environment Applications
Electronic devices capable of operation at 500°C are required for long term Venus surface missions, as well as for in situ monitoring and control of next generation aeronautical engines. High temperature sensors and electronics can also find many applications in military, and energy and automobile industries. Various silicon carbide (SiC) sensors and electronic devices have been developed for operation at 500 °C, and a compatible packaging system is needed for long term test and deployment of these high temperature devices. High temperature co-fired ceramics (HTCC) alumina with platinum (Pt) conductor was proposed for high temperature electronic packaging. A prototype Pt/HTCC alumina packaging system including chip-level package and circuit board has been briefly reported previously for long-term electrical testing of SiC integrated circuits at 500 °C, and brief testing at much higher temperatures. HTCC alumina is an excellent dielectric material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. Pt is chemically noble and can be co-fired with HTCC alumina in air ambient producing a viable electronic packaging material system for high temperature applications. This paper presents a more detailed description of this packaging system including prototype low power packages and circuit boards based on HTCC alumina and Pt metallization for 500°C and other harsh environment applications. The key technical considerations for chip-level packaging and circuit board assembly, including materials and processes for 500 °C durable wire-bonding and SiC die attach, and integration of multi-chip circuit boards, are presented. Experimental test results of this packaging approach applied to SiC integrated circuits at 500 °C and 700°C are discussed as well.
electronic packaging↗
A 96% Alumina based Packaging System for 500°C Test of SiC Integrated Circuits
With the development of silicon carbide (SiC) sensors and electronic devices for operation at 500°C, compatible packaging technologies are needed for long term high temperature test and deployment of these sensors and electronic devices. 96% Al2O3ceramic is an excellent electrically insulating material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. This paper presents a packaging system for low power integrated circuits including a prototype 8-I/O chip-level package and printed circuit board (PCB) based on 96% Al2O3ceramic substrates and Au thick-film metallization for 500°C applications. The details related to designs of packages and PCBs, packaging materials, and specific packaging step recipes including wire -bonding and die-attach, are presented. Some test results of this prototype packaging approach applied to SiC integrated circuits at 500°C are reviewed.
High Temperature, Packaging, Alumina, Thick Film↗
A 96% Alumina based Packaging System for 500°C Test of SiC Integrated Circuits
With the development of silicon carbide (SiC) sensors and electronic devices for operation at 500°C, compatible packaging technologies are needed for long term high temperature test and deployment of these sensors and electronic devices. 96% Al2O3 ceramic is an excellent electrically insulating material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. This paper presents a packaging system for low power integrated circuits including a prototype 8-I/O chip-level package and printed circuit board (PCB) based on 96% Al2O3 ceramic substrates and Au thick-film metallization for 500°C applications. The details related to designs of packages and PCBs, packaging materials, and specific packaging step recipes including wire - bonding and die-attach, are presented. Some test results of this prototype packaging approach applied to SiC integrated circuits at 500oC are reviewed.
high temperature↗
NSUF BOILER Pre-Irradiation Characterization and High Flux Isotope Reactor Experiment Design
Alumina-forming austenitic (AFA) stainless steels have emerged as a candidate alloy because of their high-temperature strength, formability, cost, and compatibility with primary coolants for lead-cooled fast reactors (LFRs). This class of steels has exceptional high-temperature oxidation performance; however, a high concentration of Ni is required to stabilize the austenite phase and to provide sufficient creep strength. AFA stainless steels are also susceptible to liquid metal embrittlement (LME). Additionally, under neutron irradiation, Ni will enrich at grain boundaries due to radiation-induced segregation (RIS). Nickel RIS can increase the LME under these coupled effects. Oak Ridge National Laboratory (ORNL) and the NSUF program have leveraged its High Flux Isotope Reactor (HFIR) and experience with complex irradiation experiments to design experiment capsules that test the aforementioned coupled effects. These capsules are designed for insertion in the central flux trap, the highest flux region, of HFIR. The experiment capsules will be filled with Pb, designed to passively melt from the gamma heating in HFIR. The specimens were fabricated into miniature tensile specimens from two different alloys, GA05-25Ni and GA05-20Ni, varying Ni concentrations. The experiment capsules are designed to achieve target temperatures of 400 °C and 650 °C with accumulated dosage of 3 dpa. This report documents the specimen alloy characterization, experimental design, and expected performance of the capsules.
21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
BOILER Experiment Material Characterization and HFIR Irradiation Status
Pre-oxidized alumina-forming austenitic (AFA) steels have been previously identified as candidate alloys for structural components in lead-cooled fast reactors (LFRs). They offer compatibility with liquid Pb, high-temperature strength, formability, and cost advantages. However, variations in Ni content can affect the formation and stability of the Al 2 O 3 layer, influencing compatibility with liquid Pb. The effect of fast neutron irradiation on Al 2 O 3 stability in liquid Pb also requires evaluation. Therefore, understanding how Ni concentrations impacts pre-oxidized AFAs under combined extremes of irradiation and liquid metal corrosion is essential before safe deployment. The Behavior Of In-situ Lead Environments & Radiation (BOILER) experiment was developed under the Nuclear Science User Facilities (NSUF) program to integrate alloy development, irradiation experiment design, and irradiated materials characterization. In this effort, two pre-oxidized AFA steels with 20 wt% and 25 wt% Ni, hereinafter referred to as GA05-20Ni and GA05-25Ni, were produced. An irradiation experiment was then planned for the High Flux Isotope Reactor (HFIR), designed for passive heating of irradiation rabbit capsules from gamma heating in the HFIR flux trap (1 × 10 15 n/cm 2 ·s, >0.1 MeV). This heating melts Pb and exposes the pre-oxidized AFA steel specimens to nominal temperatures of 400 and 650°C. Detailed neutronics and thermal analyses were performed, though based on nominal design rather than as-built, as-irradiated conditions. This report documents further characterization of the pre-oxidized AFAs in the unirradiated condition. It also includes as-built thermal analysis using measured component dimensions, updated fill gas concentrations, and actual HFIR irradiation positions. Finally, the report summarizes capsule fabrication, current irradiation status, projected completion, estimated damage accumulation, and initial plans for post-irradiation examination plans.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Microstructure and bonding between calcium aluminate cement‐containing gahnite–alumina matrix and refractory aggregates
Calcium aluminate cement enhances the thermomechanical properties of refractory castables through the formation of acicular calcium hexaluminate (CaO·6Al 2 O 3 ), Ca 2 Mg 2 Al 28 O 46 (CAM-I), and CaMg 2 Al 16 O 27 (CAM-II) phases in MgO- or MgAl 2 O 4 -containing castables. The compatibility of CA 6 with gahnite (ZnAl 2 O 4 ), and acicular Ca 2 Zn 2 Al 28 O 46 (CAZ-I) and CaZn 2 Al 16 O 27 (CAZ-II) phases formation have been previously reported. Here, in this work, the interaction between a CAC binder containing ZnAl 2 O 4 -Al 2 O 3 matrix with commonly used refractory aggregates such as tabular alumina (TA), alumina-rich (AR90, AR78) and stoichiometric (SM72) MgAl 2 O 4 spinels, and fused and dead-burned magnesia (FM, DBM, respectively) were investigated at 1650°C for 5 h. Microstructural analysis, using digital microscopy, scanning electron microscopy, and energy dispersive spectroscopy, revealed the formation of acicular CaZn 0.18 Al 11.82 O 18.91 , CAZ-I and CAZ-II grains, and strong interfacial bonding between the matrix and TA and spinel aggregates. FM and DBM were found to debond from the matrix. Thick interface layers were observed between the matrix and all the aggregates but TA. Null hypothesis significance testing (NHST) shows that the difference in the number of acicular grains between the interface zone and the bulk matrix (Z) is statistically significant for AR90/Z, SM72/Z, FM/Z, and DBM/Z interfaces, but not significant for TA/Z and AR78/Z. The role of the aggregates’ chemistry on the interfacial bonding and microstructure evolution is discussed.
Ramteke, Rajat Durgesh [Univ. of Alabama, Birmingh↗