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At least 433 records · Page 24

Iodine Waste Form Corrosion: PNNL Summary Testing Report

A test method to correlate the laboratory corrosion behavior of iodine-containing waste forms (IWFs) to a conceptual long-term corrosion models is required. Several candidate methods have been evaluated previously, and each method presents unique challenges and limitations. Dynamic leach tests have emerged as the preferred candidate test method to evaluate IWFs and parameterize an eventual long-term corrosion model. This report was prepared in support of this effort to define the test suite to evaluate the corrosion of IWFs, with the goal of defining and parameterizing a conceptual long-term corrosion model. A review was presented highlighting the high degree of variability between the IWF corrosion data that is available in the literature and the need for a standardized test suite. The targeted test suite is composed of a single interval screening test, a dynamic leach test, and post-test solid characterization of the monolithic IWF samples. The data presented serves two purposes: to expand the range of IWFs evaluated with the test suite to assess method variability and to further understand the corrosion of IWFs to best inform conceptual long-term corrosion model development. A series of IWF types were included in the testing, including hot isostatically pressed Ag-mordenite, silver functionalized silica-based aerogels, iodosodalites (hot isostatic pressing, sintered, glass bonded ceramic), iodoapatite, tellurite glass and glass composite materials.

42 ENGINEERING↗

Nitridation of silicon

Silicon powders with three levels of impurities, principally Fe, were sintered in He or H2. Non-densifying mechanisms of material transport were dominant in all cases. High purity Si showed coarsening in He while particle growth was suppressed in H2. Lower purity powder coarsened in both He and H2. The same three Si powders and Si /111/ single crystal wafers were nitrided in both N2 and N2/H2 atmospheres. Hydrogen increased the degree of nitridation of all three powders and the alpha/beta ratio of the lower purity powder. Some Si3N4 whiskers and open channels through the surface nitride layer were observed in the presence of Fe, correlating with the nitridation-enhancing effects of Fe. Thermodynamic calculations showed that when SiO2 is present on the Si, addition of H2 to the nitriding atmosphere decreases the amount of SiO2 and increases the partial pressure of Si-containing vapor species, that is, Si and SiO. Large amounts of NH3 and SiH4 were also predicted to form.

Shaw, N. J.↗

Development of improved coating for advanced carbon-carbon components

Reaction sintered silicon nitride (RSSN) was studied as a substitute coating material on the carbon-carbon material (RCC) presently used as a heat shield on the space shuttle, and on advanced carbon-carbon (ACC), a later development. On RCC, RSSN showed potential in a 538 C (1000 F) screening test in which silicon carbide coated material exhibits its highest oxidation rate; RSSN afforded less protection to ACC because of a larger thermal expansion mismatch. Organosilicon densification and metallic silicon sealing methods were studied as means of further increasing the oxidation resistance of the coating, and some improvement was noted when these methods were employed.

Yamaki, Y. R.↗

Hafnia-rich mixed oxide ceramics of the system HfO2-ZrO2-TiO2 for heaters and heat exchangers in electrothermal thrusters: The effects of titania on selected electrical and mechanical properties of Hafnia-rich mixed oxides in the system Hafnia-Zirconia-Titania, volume 1

A study of the effects of titania on selected properties of hafnia-rich mixed oxides in the system hafnia-zirconia-titania (HZT) was made in the region 5 to 20 mol percent titania. The studied properties included electrical conductivity, thermal expansion, and fracture strength and toughness. The effects of titania on the properties were studied for the reduced state as well as the oxidized state of the sintered mixed oxides. X-ray analysis showed that the materials were not always single phase. The oxidized compositions went from being monoclinic solid solutions at low titania additions to having three phases (two monoclinic and a titanate phase) at high additions of titania. The reduced compositions showed an increasing cubic phase presence mixed with the monoclinic phase as titania was added. The electrical conductivity increased with temperature at approximately 0.1 mhos/cm at 1700 C for all compositions. The thermal expansion coefficient decreased with increasing titania as did the monoclinic to tetragonal transformation temperature. The fracture strength of the oxidized bars tended to decrease with the addition of titania owing to the presence of the second phase titania. The fracture strength of the reduced bars exhibited a minimum corresponding to a two-phase region of monoclinic and cubic phases. When the second phases were suppressed, the titania tended to increase the fracture strength slightly in both the oxidized and reduced states. The fracture toughness followed similar trends.

Staszak, Paul Russell↗

Improved silicon nitride for advanced heat engines

Silicon nitride is a high temperature material currently under consideration for heat engine and other applications. The objective is to improve the net shape fabrication technology of Si3N4 by injection molding. This is to be accomplished by optimizing the process through a series of statistically designed matrix experiments. To provide input to the matrix experiments, a wide range of alternate materials and processing parameters was investigated throughout the whole program. The improvement in the processing is to be demonstrated by a 20 percent increase in strength and a 100 percent increase in the Weibull modulus over that of the baseline material. A full characterization of the baseline process was completed. Material properties were found to be highly dependent on each step of the process. Several important parameters identified thus far are the starting raw materials, sinter/hot isostatic pressing cycle, powder bed, mixing methods, and sintering aid levels.

Yeh, H. C.↗

Thermal barrier coating life-prediction model development

The program focuses on predicting the lives of two types of strain-tolerant and oxidation-resistant thermal barrier coating (TBC) systems that are produced by commercial coating suppliers to the gas turbine industry. The plasma-sprayed TBC system, composed of a low-pressure plasma-spray (LPPS) or an argon shrouded plasma-spray (ASPS) applied oxidation resistant NiCrAlY or (CoNiCrAlY) bond coating and an air-plasma-sprayed yttria partially stabilized zirconia insulative layer, is applied by both Chromalloy, Klock, and Union Carbide. The second type of TBS is applied by the electron beam-physical vapor deposition (EB-PVD) process by Temescal. The second year of the program was focused on specimen procurement, TMC system characterization, nondestructive evaluation methods, life prediction model development, and TFE731 engine testing of thermal barrier coated blades. Materials testing is approaching completion. Thermomechanical characterization of the TBC systems, with toughness, and spalling strain tests, was completed. Thermochemical testing is approximately two-thirds complete. Preliminary materials life models for the bond coating oxidation and zirconia sintering failure modes were developed. Integration of these life models with airfoil component analysis methods is in progress. Testing of high pressure turbine blades coated with the program TBS systems is in progress in a TFE731 turbofan engine. Eddy current technology feasibility was established with respect to nondestructively measuring zirconia layer thickness of a TBC system.

Strangman, T. E.↗

Advances in lightweight nickel electrode technology

Studies are currently underway to further the development of lightweight nickel electrode technology. Work is focused primarily on the space nickel-hydrogen system and nickel-iron system but is also applicable to the nickel-cadmium and nickel-zinc systems. The goal is to reduce electrode weight while maintaining or improving performance, thereby increasing electrode energy density. Two basic electrode structures are being investigated. The first is the traditional nickel sponge produced from sintered nickel-carbonyl powder. The second is a new material for this application which consists of a non-woven mat of nickel fiber. Electrodes are being manufactured, tested, and evaluated at the electrode and cell level.

Coates, Dwaine↗

Tribological and mechanical comparison of sintered and hipped PM212: High temperature self-lubricating composites

Selected tribological, mechanical and thermophysical properties of two versions of PM212 (sintered and hot isostatically pressed, HIPped) are compared. PM212, a high temperature self-lubricating composite, contains 70 wt percent metal bonded chromium carbide, 15 wt percent CaF2/BaF2 eutectic and 15 wt percent silver. PM212 in the sintered form is about 80 percent dense and has previously been shown to have good tribological properties from room temperature to 850 C. Tribological results of a fully densified, HIPped version of PM212 are given. They are compared to sintered PM212. In addition, selected mechanical and thermophysical properties of both types of PM212 are discussed and related to the tribological similarities and differences between the two PM212 composites. In general, both composites display similar friction and wear properties. However, the fully dense PM212 HIPped composite exhibits slight lower friction and wear than sintered PM212. This may be attributed to its generally higher strength properties. The sintered version displays stable wear properties over a wide load range indicating its promise for use in a variety of applications. Based upon their properties, both the sintered and HIPped PM212 have potential as bearing and seal materials for advanced high temperature applications.

Dellacorte, Christopher↗

Grain orientation in high Tc superconductors by molten salt powder synthesis

The molten salt or the flux method is used to fabricate a grain oriented YBa2Cu3O(7-x) (123) superconductor. Here we suggest a two-stage approach in using the 'green phase', Y2BaCuO5 (211), as seed crystals in the formation of YBa2Cu3O(7-x). The process uses Y2BaCuO5 formed by molten salt synthesis. The Y2BaCuO5 phase was observed to be stable in water and in most of the salt systems. Salt processing can form a small quantity of anisotropic particles of Y2BaCuO5. This material can form the 123 phase when tape cast and sintered in the presence of the required levels of Ba and Cu.

Gopalakrishnan, Sudhakar↗

Tribological and mechanical comparison of sintered and HIPped PM212 - High temperature self-lubricating composites

Selected tribological, mechanical and thermophysical properties of two versions of PM212 (sintered and hot isostatically pressed, HIPped) are compared. PM212, a high temperature self-lubricating composite, contains 70 wt percent metal bonded chromium carbide, 15 wt percent CaF2/BaF2 eutectic and 15 wt percent silver. PM212 in the sintered form is about 80 percent dense and has previously been shown to have good tribological properties from room temperature to 850 C. Tribological results of a fully densified, HIPped version of PM212 are given. They are compared to sintered PM212. In addition, selected mechanical and thermophysical properties of both types of PM212 are discussed and related to the tribological similarities and differences between the two PM212 composites. In general, both composites display similar friction and wear properties. However, the fully dense PM212 HIPped composite exhibits slight lower friction and wear than sintered PM212. This may be attributed to its generally higher strength properties. The sintered version displays stable wear properties over a wide load range indicating its promise for use in a variety of applications. Based upon their properties, both the sintered and HIPped PM212 have potential as bearing and seal materials for advanced high temperature applications.

Dellacorte, Christopher↗

Synthesis and behavior of bulk iron nitride soft magnets via high-pressure spark plasma sintering

Abstract In this study, dense bulk iron nitrides (Fe x N) were synthesized for the first time ever using spark plasma sintering (SPS) of Fe x N powders. The Fe 4 N phase of iron nitride in particular has significant potential to serve as a new soft magnetic material in both transformer and inductor cores and electrical machines. The density of SPSed Fe x N increased with SPS temperature and pressure. The microstructure of the consolidated bulk Fe x N was characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. XRD revealed a primary phase of Fe 4 N with secondary phases of Fe 3 N and metallic iron. Finite element analysis (FEA) was also applied to investigate and explain localized heating and temperature distribution during SPS. The effects of processing on interface bonding formation and phase evolution were investigated and discussed in detail to provide insight into fundamental phenomena and microstructural evolution in SPSed Fe x N. Graphic abstract

36 MATERIALS SCIENCE↗

Nuclear Rocket Ceramic Metal Fuel Fabrication Using Tungsten Powder Coating and Spark Plasma Sintering

Nuclear thermal propulsion is an enabling technology for crewed Mars missions. An investigation was conducted to evaluate spark plasma sintering (SPS) as a method to produce tungsten-depleted uranium dioxide (W-dUO2) fuel material when employing fuel particles that were tungsten powder coated. Ceramic metal fuel wafers were produced from a blend of W-60vol% dUO2 powder that was sintered via SPS. The maximum sintering temperatures were varied from 1,600 to 1,850 C while applying a 50-MPa axial load. Wafers exhibited high density (>95% of theoretical) and a uniform microstructure (fuel particles uniformly dispersed throughout tungsten matrix).

Barnes, M. W.↗

Improved silicon nitride for advanced heat engines

The AiResearch Casting Company baseline silicon nitride (92 percent GTE SN-502 Si sub 3 N sub 4 plus 6 percent Y sub 2 O sub 3 plus 2 percent Al sub 2 O sub 3) was characterized with methods that included chemical analysis, oxygen content determination, electrophoresis, particle size distribution analysis, surface area determination, and analysis of the degree of agglomeration and maximum particle size of elutriated powder. Test bars were injection molded and processed through sintering at 0.68 MPa (100 psi) of nitrogen. The as-sintered test bars were evaluated by X-ray phase analysis, room and elevated temperature modulus of rupture strength, Weibull modulus, stress rupture, strength after oxidation, fracture origins, microstructure, and density from quantities of samples sufficiently large to generate statistically valid results. A series of small test matrices were conducted to study the effects and interactions of processing parameters which included raw materials, binder systems, binder removal cycles, injection molding temperatures, particle size distribution, sintering additives, and sintering cycle parameters.

Yeh, H. C.↗

High Velocity Burner Rig Oxidation and Thermal Fatigue Behavior of Si3N4- and SiC Base Ceramics to 1370 Deg C

One SiC material and three Si3N4 materials including hot-pressed Si3N4 as a baseline were exposed in a Mach-1-gas-velocity burner rig simulating a turbine engine environment. Criteria for the materials selection were: potential for gas-turbine usage, near-net-shape fabricability and commercial/domestic availability. Cyclic exposures of test vanes up to 250 cycles (50 hr at temperature) were at leading-edge temperatures to 1370 C. Materials and batches were compared as to weight change, surface change, fluorescent penetrant inspection, and thermal fatigue behavior. Hot-pressed Si3N4 survived the test to 1370 C with slight weight losses. Two types of reaction-sintered Si3N4 displayed high weight gains and considerable weight-change variability, with one material exhibiting superior thermal fatigue behavior. A siliconized SiC showed slight weight gains, but considerable batch variability in thermal fatigue.

Sanders, W. A.↗

Machine-learning-based, online estimation of ceramic’s microstructure upon the laser spot brightness during laser sintering

The ceramic microstructure strongly influences its properties. During manufacturing, the online monitoring of microstructure is critical to ensure the desired material properties. So far, the microstructure on the relevant scale is usually characterized offline using scanning electron microscopy (SEM), which is time and cost-consuming. In this work, we demonstrate a cost-effective, machine learning (ML)-based approach to simulate the SEM micrographs in real-time from the laser spot brightness. We experimentally observed a strong correlation between the laser spot brightness and the corresponding microstructure at the exact locations. The brightness values obtained from thermal emission images and the corresponding SEM micrographs were used in the training datasets. The ML algorithm was a style-based conditional generative adversarial network (CGAN). After training, the ML model could generate high-fidelity microstructure images within 0.1 seconds based on in-situ captured brightness at the laser sintering spot. We used the average grain sizes as the metric to evaluate the accuracy of the ML-predicted micrographs. Here, the ML-predicted microstructures were in good agreement, with less than 5% in difference from the real SEM images. In conclusion, we demonstrate the cost-effective, online microstructure estimation during laser sintering with a simple setup (a camera, a regular computer, and the ML model).

08 HYDROGEN↗

Coupling of Spark Plasma Sintering with Advanced Modeling to Enable Process Scale-Up: LDRD Final Project Poster

Electric-field assisted sintering (EFAS) manufacturing techniques reduce energy usage requirements, fabricate near-net-shape parts, and produce bulk nanostructured materials through rapid heating and cooling rates achievable through Joule heating. Process parameters of pulsed DC voltage and constant pressure are applied through stainless steel rams and graphite tooling to the ceramic yttrium oxide powder to be sintered. Our high-fidelity modeling code application advances manufacturing for extreme environments by enabling process-informed design and improving microstructure consistency through multiphysics multiscale process-structure-property-performance correlation simulations.

36 MATERIALS SCIENCE↗