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At least 55 records · Page 3

Furnace Cyclic Oxidation Behavior of Multi-Component Low Conductivity Thermal Barrier Coatings

Ceramic thermal barrier coatings will play an increasingly important role in advanced gas turbine engines because of their ability to further increase engine operating temperatures and reduce cooling, thus helping achieve future engine low emission, high efficiency and improved reliability goals. Advanced multi-component zirconia-based thermal barrier coatings are being developed using an oxide defect clustering design approach to achieve the required coating low thermal conductivity and high temperature stability. Although the new composition coatings were not yet optimized for cyclic durability, an initial durability screening of the candidate coating materials was conducted using conventional furnace cyclic oxidation tests. In this paper, furnace cyclic oxidation behavior of plasma-sprayed zirconia-based defect cluster thermal barrier coatings was investigated at 1163 C using 45 min hot cycles. The ceramic coating failure mechanisms were studied using scanning electron microscopy (SEM) combined with X-ray diffraction (XRD) phase analysis after the furnace tests. The coating cyclic lifetime is also discussed in relation to coating processing, phase structures, dopant concentration, and other thermo-physical properties.

Zhu, Dong-Ming↗

Graphite Oxidation Rate Study on ET-10 and ETU-10 Grades - Task 4: QA Support and Testing for Structural Graphite Oxidation

INL performed targeted oxidation tests to measure oxidation rates for samples of ET-10 and ETU-10 graphite under CRADA No. 21CRA22 Mod. 3, Annex A, “Tritium Testing to Support Kairos Power Advanced Reactor Demonstration” (04/02/2024). All testing was conducted within INL’s Carbon Characterization Laboratory (CCL) using test standard ASTM D7542-21 "Standard Test Method for Air Oxidation of Carbon and Graphite in the Kinetic Regime" [ASTM International, 2021]. Kairos Power provided all test specimens through its graphite vendor Ibiden, Inc. to INL and ASTM specimen specified dimensions. Information within this report only provides the Arrhenius oxidation rate plots as a function of temperature for each graphite grade tested. The raw mass loss per time data will be provided on the Nuclear Data Management and Analysis System (NDMAS) portal located on the INL information system.

36 MATERIALS SCIENCE↗

The Effect of Hydrogen Annealing and Sulfur Content on the Oxidation Resistance of PWA 1480

For many decades the dramatic effect of trace amounts of reactive elements on alumina and chromia scale adhesion has been recognized and widely studied. Although various theories have been used to account for such behavior, the connection between scale adhesion and sulfur segregation was initially reported by Smeggil et al. This study found strong surface segregation of sulfur from very low levels in the bulk which could then be curtailed by the addition of reactive elements. It was assumed that the reactive elements, which are strong sulfide formers, acted by getting sulfur in the bulk thus precluding sulfur segregation and weakening of the oxide-metal bond. Subsequent studies confirmed that adhesion could be produced by reducing the sulfur impurity level, without reactive elements. The understanding of this phenomenon has been applied to modern single crystal superalloys, where the addition of Y, although very effective, is problematic. Also problematic is definition of the level of sulfur that is acceptable and below which no further adhesion benefit is reached. Published works have indicated a broad transition defined by various materials and oxidation tests. The present study describes the oxidation behavior of one superalloy (PWA 1480) as a function of various sulfur contents produced by hydrogen annealing for various temperatures, times, and sample thicknesses. The purpose is to define more precisely a criterion for adhesion based on total sulfur reservoir and segregation potential.

Smialek, James L.↗

AGR Program TRISO Fuel Topical Report Dialog

AGR Program Overview and Current Activities Fission Product Transport Data Short-Lived Fission Product Release Fuel Performance Margin Data Oxidation Testing Data

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Oxide morphology and spalling model for NiAl

A scanning electron microscope equipped with an energy dispersive spectrographic unit was used to study in detail the Al2O3 oxide morphology and oxide-metal interface of a nickel-rich NiAl alloy (Ni-42 at% Al) with a view toward providing information relevant to spalling theories in the MCrAlY system. In addition, the kinetics of spalling was studied for critical evaluation of one of the step-process spall models and for collection of pertinent experimental data. Cyclic oxidation tests were run in 1-atm air at about 1100 C, and isothermal specimens were examined from 2 min to 200 hr of exposure. It is shown that oxide spalling occurs primarily at the oxide-metal interface in an intergranular mode, that crystallographic Kirkendall voids arise as a result of oxidation, and that the fractional area of spalled oxide varies widely in cyclic tests but increases with the square of oxide thickness for isothermal tests. A spall model is developed in the form of a summation series.

Smialek, J. L.↗

Metal–Oxide Interface Sites Created Using Atomic Layer Deposition and Tested for CO Oxidation

The performance of catalysts made out of Pt supported on TiO 2 thin films grown on SBA-15 (a silica mesoporous material) by atomic layer deposition (ALD) was characterized systematically by combining in situ infrared absorption spectroscopy (IR) with other techniques including electron microscopy and adsorption−desorption isothermal measurements. The titania films in the resulting high-surface-area catalysts were evenly distributed throughout the inner surface of the SBA-15 mesopores, and their thickness could be controlled at a submonolayer level, with 3 to 4 TiO 2 ALD cycles needed for the complete coverage of the silica sites. The titania films could be deposited either before or after adding the metal (Pt), which was dispersed in the form of small nanoparticles (NPs) approximately 4−6 nm in diameter, in order to exert some control on the density and nature of the Pt/TiO 2 interface sites. One important lesson deriving from this work is that such an order of deposition leads to significantly different catalysts in spite of the fact that most of their structural properties are similar. If the Pt is deposited on the titania films, the resulting metal NPs are slightly smaller than those grown on silica and display CO adsorption sites with lower surface Pt coordination numbers. On the other hand, when TiO 2 is deposited on the Pt/SBA-15 starting material, some titania grows on the metal and partially blocks its surface while also creating new interface sites where CO binds more weakly and displays lower C−O stretching frequencies. In terms of catalytic performance, the results from in situ IR CO site titration and kinetic measurements combined suggest a mechanism where CO first adsorbs on Pt atop sites and then migrates to Pt/TiO 2 interface sites, where oxidation takes place. Both types of sites appear to be similar in all the catalysts tested, but catalytic performance could be optimized by tuning their surface densities. Maximum catalytic activity was obtained when the TiO2 films were deposited first and with TiO 2 coverages of at least half a monolayer, that is, after at least 2 ALD cycles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE Advanced Gas Reactor Fuel Development and Qualification Program Overview

AGR-3/4 post-irradiation examination and data analysis AGR-5/6/7 PIE and safety testing Supplemental fuel microanalysis and method development Fuel oxidation testing Air/moisture Ingress Experiment (AMIX) system development (deployed in FY23) Single particle testing in FITT Data management and analysis Fuel performance modeling

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

High Temperature Lightweight Self-Healing Ceramic Composites for Aircraft Engine Applications

The present research effort was undertaken to develop a new generation of SiC fiber- reinforced engineered matrix composites (EMCs) with sufficient high temperature plasticity to reduce crack propagation and self-healing capabilities to fill surface-connected cracks to prevent the oxygen ingress to the fibers. A matrix engineered with these capabilities is expected to increase the load bearing capabilities of SiCSiC CMCs at high temperatures. Several matrix compositions were designed to match the coefficient of thermal expansion (CTE) of the SiC fibers using a rule of mixture (ROM) approach. The CTE values of these matrices were determined and it was demonstrated that they were generally in good agreement with that of monolithic SiC between room temperature and 1525 K. The parameters to hot press the powders were optimized, and specimens were fabricated for determining bend strength, CTE, oxidation and microstructural characteristics of the engineered matrices. The oxidation tests revealed that some of the matrices exhibited catastrophic oxidation, and therefore, these were eliminated from further consideration. Two promising compositions were down selected based on these results for further development. Four-point bend tests were conducted on these two promising matrices between room temperature and 1698 K. Although theses matrices were brittle and failed at low stresses at room temperature, they exhibited high temperature ductility and higher stresses at the higher temperatures. The effects of different additives on the self-healing capabilities of these matrices were investigated. The results of preliminary studies conducted to slurry and melt infiltration trials with CrSi2 are described.

Silicides↗

UK-US Collaboration on Fossil Energy R&D: Steam Side Oxidation

In recent years, interest in increasing the efficiency of power plants based on steam generation has led to the need to develop and qualify materials capable of operating at steam temperatures and pressures significantly higher than those employed in current power plants. The overall focus of this international program is on using ferritic-martensitic steels to the maximum possible temperature, before switching to austenitic steels and/or Ni-based alloys. The relatively low Cr content of these alloys raises concerns regarding their resistance to steam oxidation at these higher temperatures. Earlier work in this collaboration addressed the reliability of data from atmospheric pressure, laboratory-based steam oxidation tests. This raised issues regarding how representative the laboratory-grown oxides were compared to those formed on service-exposed material and how the tests could be made more reliable by introducing added complexity. In general laboratory-scale exposures are conducted under isothermal conditions at ambient or slightly elevated pressure, using a relatively low flow rate of steam. The coupons used in these tests are normally flat cuboids which have been ground to homogenise the surface and remove any pre-existing features. However, there is a concern that these samples and exposures are not representative of service conditions, and so it is necessary to quantify the influence of transient conditions, such as heat flux, pressure and sample geometry/surface conditions. To address such concerns a new collaborative program of work was initiated to determine the influence of these added features on oxidation kinetics and oxide scale morphology. The overall aim was to improve the understanding of alloy performance in ultrasupercritical (USC) steam conditions and qualify suitable test procedures.

20 FOSSIL-FUELED POWER PLANTS↗

Prediction of oxidation performance of reinforced carbon-carbon material for Space Shuttle leading edges

A method was developed for predicting oxidation performance, in an earth atmospheric entry environment, of reinforced carbon-carbon material, coated for oxidation resistance. A model was developed which describes oxidation control mechanisms, and the equations defining these mechanisms were derived. These relations were used to correlate oxidation test data, and to infer pertinent rate constants. Predictions were made of material oxidation performance in a representative entry environment, and the predictions were compared with ground test data. Results indicate that the method can be successfully used for predicting material oxidation performance.

Medford, J. E.↗

Uranium nitride (UN) pellets with controllable microstructure and phase – fabrication by spark plasma sintering and their thermal-mechanical and oxidation properties

Dense uranium mononitride (UN) pellets with controlled microstructures and tailored grain size from large-grained to a few microns are synthesized by spark plasma sintering (SPS) combined with high energy ball milling. The impacts of the sintering conditions on fuel microstructure, grain size, physical density, and phase behavior are systematically investigated, and the thermal-mechanical properties and oxidation behavior of the SPS densified UN pellets are characterized. Higher sintering temperatures and longer ball milling durations and thus finer starting UN powders promote sintering and densification, and dense UN pellets above 95% theoretical density can be achieved by SPS at 1873 K for 10 min. UN phase purity is maintained in the SPS-densified pellets sintered at a lower temperature and short duration. A phase heterogeneity with secondary UO 2 or uranium sesquinitride (U 2 N 3 ) occurs for the UN pellets sintered at higher temperatures using finer UN powders. The hardness and fracture toughness of the SPS-densified UN pellets increase with smaller grain sizes and higher densities to 7.9 GPa and 3.5 MPa m 1/2 , respectively. Furthermore, both small (1–2 μm) and large grain-sized (30–50 µm) UN pellets exhibit good thermal conductivity. Dynamic oxidation testing by a thermogravimetric analyzer in air shows that the onset temperature for oxidation varies with microstructure and phase heterogeneity of the SPS densified UN pellets. Particularly, the smaller-grained (micron-sized) UN pellets containing uranium oxides and U 2 N 3 display lower weight gain and significantly-reduced oxidation kinetics, and full oxidation completes at a temperature above 1173 K when tested with a ramp rate of 10 K/min.

36 MATERIALS SCIENCE↗

Energy efficient engine, high pressure turbine thermal barrier coating. Support technology report

This report describes the work performed on a thermal barrier coating support technology task of the Energy Efficient Engine Component Development Program. A thermal barrier coating (TBC) system consisting of a Ni-Cr-Al-Y bond cost layer and ZrO2-Y2O3 ceramic layer was selected from eight candidate coating systems on the basis of laboratory tests. The selection was based on coating microstructure, crystallographic phase composition, tensile bond and bend test results, erosion and impact test results, furnace exposure, thermal cycle, and high velocity dynamic oxidation test results. Procedures were developed for applying the selected TBC to CF6-50, high pressure turbine blades and vanes. Coated HPT components were tested in three kinds of tests. Stage 1 blades were tested in a cascade cyclic test rig, Stage 2 blades were component high cycle fatigue tested to qualify thermal barrier coated blades for engine testing, and Stage 2 blades and Stage 1 and 2 vanes were run in factory engine tests. After completion of the 1000 cycle engine test, the TBC on the blades was in excellent condition over all of the platform and airfoil except at the leading edge above midspan on the suction side of the airfoil. The coating damage appeared to be caused by particle impingement; adjacent blades without TBC also showed evidence of particle impingement.

Duderstadt, E. C.↗

Oxidation and low cycle fatigue life prediction

When a metallic material is exposed to a high temperature in an ambient atmosphere, oxidation takes place on the metallic surface. The formed oxides (both surface and grain boundary oxides) are mechanically brittle so that if the stress is high enough the oxides will be cracked. The grain boundary oxide formation in TAZ-8A nickel-base superalloy was studied. The effect of oxide crack nucleus on low cycle fatigue life will be analyzed. The TAZ-8A was subjected to high temperature oxidation tests in air under the stress-free condition. The oxidation temperatures were 600, 800, and 1000 C. The oxidation time varies from 10 to 1000 hours.

Oshida, Y.↗

Enriched aluminide coatings for dispersion strengthened nickel materials

Improved aluminide/barrier coating combinations for dispersion strengthened nickel materials were investigated. The barrier materials involved alloys with refractory metal content to limit interdiffusion between the coating and the substrate, thereby minimizing void formation. Improved aluminide coatings involved the dispersion of aluminum-rich compounds. Coatings were tested in argon at 1533 K (2300 F) for 100 hours and in cyclic oxidation at 1422 K (2100 F). Two coatings on TDNiCr completed 300 hours of oxidation testing, none on TDNi. Selected coating combinations were evaluated in Mach 1 burner rig testing using JP-4 fuel and air at 1422 K (2100 F) and 1477 K (2200 F) for 350 and 100 hours, respectively. Static oxidation in 1-hour cycles was conducted at 1533 K (2300 F) for 100 hours. For comparison purposes a physical vapor deposition (PVD) NiCrAlY coating was tested concurrently. Only the NiCrA1Y coating survived the 1477 K (2200 F)/100-hour burner rig test and 275 hours of the 350-hour 1422 K (2100 F) test. Elevated temperature exposure reduced room temperature tensile properties but had little effect on elevated temperature properties.

Levinstein, M. A.↗

Dynamic oxidation behavior of TD-NiCr alloy with different surface pretreatments

Oxidation tests of TD-NiCr alloy with different surface pretreatments were conducted in a Mach-5 arc-jet at 1200 C and 0.002 lb/sec flowing air environment. The mechanisms responsible for the observed oxidation behavior are examined. The presence of atomic oxygen in the air stream plays a significant role in determining the oxidation characteristic of the alloy. The rate of Cr2O3 vaporization by formation of volatile CrO3 is greatly enhanced by the flowing conditions. The typical microstructure of oxides formed in the dynamic tests consists of an external layer of NiO with a porous mushroom-type morphology, an intermediate layer of NiO and Cr2O3 oxide mixture, and a continuous inner layer of Cr2O3 in contact with the Cr-depleted alloy substrate. Three basic processes underlying the formation of mushroom-type NiO are identified and discussed. The oxidation rate is determined by the rate of vaporization of NiO. Surface pretreatment has a significant effect on the oxidation behavior of the alloy in the early stage of oxidation, but becomes less important as exposure time increases. Mechanical polishing induces surface recrystallization, but promotes the concurrence of external growth of NiO and internal oxidation of the alloy in the dynamic atmosphere.

Young, C. T.↗

Development and Characterization of Hot-Pressed Matrices for Engineered Ceramic Matrix Composites (E-CMCs)

The present research effort was undertaken to develop a new generation of SiC fiber-reinforced engineered ceramic matrix composites (E-CMCs). In contrast to traditional CMCs with a brittle SiC matrix, an E-CMC is designed to consist of a matrix engineered to possess sufficient high temperature plasticity to minimize crack propagation, relatively high fracture toughness, and self-healing capabilities to prevent oxygen ingress to the BN-coated fibers through surface-connected cracks. The present paper discusses the bend strength, isothermal oxidation, microstructures and self-healing properties of several silicide-behaved engineered matrices. Based on the oxidation tests, where it was observed that some of the matrices exhibited either catastrophic oxidation ("pesting") or spalling of the oxide scale, two engineered matrices, CrSi2/SiC/Si3N4 and CrMoSi/SiC/Si3N4, were down-selected for further investigation. Four-point bend tests were conducted on these two engineered matrices between room temperature and 1698 degrees Kelvin. Although these matrices were brittle at low temperatures, it was observed that the bend strengths and bend ductility increased at high temperatures as the silicide particles became more ductile, which was qualitatively consistent with the theoretically expected behavior that crack blunting at these particles should increase the matrix strength. Additional studies were conducted to study the effects of different additives on the self-healing properties of the engineered matrices, which helped to identify the most effective additives.

Composite Materials↗

An oxidation and erosion test facility for cooled panels

The Panel Oxidation and Erosion Testbed (POET) facility under construction at GASL to provide the required test environment is described. The POET facility comprises three major element including a vitiated air heater, a supersonic nozzle, and a test section. A hydrogen-fueld vitiated air heater will provide the oxidizing and erosive environment. The flow through the test section characterized by low supersonic speed and Mach number of 1.4 will maximize the local heat transfer rate and the local surface shear stress.

Swartwout, W. H.↗