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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Effects of chemistry and microstructure on corrosion performance of Zircaloy-2-based BWR cladding - 2016-0066

In boiling water reactors (BWRs), Zircaloy-2 is typically the material of choice for fuel cladding. With increased focus on fuel performance and reliability, consistent cladding corrosion performance under varying BWR conditions has become an acknowledged requirement for modern BWR fuel. To support optimization of corrosion performance, modifications to alloy chemistry and manufacture conditions can be made, supported by ex-reactor corrosion testing and demonstrated through in-reactor operation. In this work, the combined effects of alloy chemistry and fabrication process were investigated. The effect of alloy chemistry is often complicated by variation within a production ingot. In this work, additional measurements were intentionally taken at the tube-shell stage (before cold pilgering) so that chemistry more representative of the final cladding could be obtained and the effect of iron, nickel, and tin could be examined more closely. Although chemistry range of Zircaloy-2 was the primary focus, the effect of iron above the ASTM limit in a new alloy was also explored. Three types of cladding fabrication processes were considered. Two types included a heat treatment applied after the first cold pilgering and annealing, and the treatment was limited to the outer portion of the cladding and differed in the temperature of the heat treatment; the third type had no special heat treatments after the first cold pilgering and annealing. The weight gain of the three types of cladding with varying compositions under two corrosion test conditions (400 deg. C steam and 410/520 deg. C two-stage steam) are discussed in terms of the initial second-phase particle sizes obtained from transmission electron microscopy examinations. Based on poolside inspections and hot-cell examinations, the in-reactor corrosion performance of the two cladding types up to typical discharge exposures are discussed in the terms of corrosion margin, microstructure evolution, and correlation with ex-reactor corrosion test data. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2013

Mechanical Properties of Nuclear Fuel Surrogates using Picosecond Laser Ultrasonics

Detailed understanding between microstructure evolution and mechanical properties is important for designing new high burnup nuclear fuels. In this presentation we discuss the use of picosecond ultrasonics to measure localize changes in mechanical properties of fuel surrogates. We develop measurement techniques that can be applied to investigate heterogeneous elastic properties caused by localize changes in chemistry, grain microstructure caused by recrystallization, and mechanical properties of small samples prepared using focused ion beam sample preparation. Emphasis is placed on understanding the relationship between microstructure and mechanical properties

25 ENERGY STORAGE↗
DOE OSTI2024

Phase-field modeling for restructuring in the dark zone of high burnup UO 2

This report summarizes the mesoscale modeling work performed in fiscal year 2024 under the Nuclear Energy Advanced Modeling and Simulation (NEAMS) program to capture the microstructural evolution and restructuring observed in the dark regions of high burnup UO 2 nuclear fuel. This is the first attempt to realistically simulate the restructuring behavior observed in different region of a high burnup fuel. We employ a grand-potential based phase-field model to concurrently evaluate the formation of subgrains and growth of fission bubbles within the fuel. A energy-based subgrain formation criteria is introduced to simulate the restructuring process. Effect of different initial conditions and different modeling parameters are studies systematically to capture how each of these parameters influence the characteristics of the restructured fuel. It is observed that the subgrain formation begins around existing fission gas bubbles and then proceeds towards triple junctions, grain boundaries and grain interiors. It is demonstrated that restructuring is influenced by a combination of initial dislocation densities, subgrain formation rate, and temperature. Rate of restructuring increases with increase in fuel temperature. A restructuring bias is observed within the microstructure due to variation in defect accumulation among different grains. Furthermore, bubble sizes and distribution does not have a significant effect on rate of restructuring. The predicted microstructures resembles the characteristics of the restructured regions as observed in experiments. Finally, a correlation is presented that demonstrates the evolution of the restructuring volume fraction as a function of local effective burnup. This work provides a first of its kind restructuring model for darkzone that can be used by BISON for performance prediction of high burnup UO 2 fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

The Effects of Specimen Geometry on the Plastic Deformation of AA 2219-T8 Aluminum Alloy Under Dynamic Impact Loading

The effects of specimen geometry on shear strain localization in AA 2219-T8 aluminum alloy under dynamic impact loading were investigated. The alloy was machined into cylindrical, cuboidal and conical (frustum) test specimens. Both deformed and transformed adiabatic shear bands developed in the alloy during the impact loading. The critical strain rate for formation of the deformed band was determined to be 2500 s{sup −1} irrespective of the specimen geometry. The critical strain rate required for formation of transformed band is higher than 3000 s{sup −1} depending on the specimen geometry. The critical strain rate for formation of transformed bands is lowest (3000 s{sup −1}) in the Ø5 mm × 5 mm cylindrical specimens and highest (> 6000 s{sup −1}) in the conical specimens. The cylindrical specimens showed the greatest tendency to form transformed bands, whereas the conical specimen showed the least tendency. The shape of the shear bands on the impacted plane was also observed to be dependent on the specimen geometry. Whereas the shear bands on the compression plane of the conical specimens formed elongated cycles, two elliptical shaped shear bands facing each other were observed on the cylindrical specimens. Two parallel shear bands were observed on the compression planes of the cuboidal specimens. The dynamic stress–strain curves vary slightly with the specimen geometry. The cuboidal specimens exhibit higher tendency for strain hardening and higher maximum flow stress than the other specimens. The microstructure evolution leading to the formation of transformed bands is also discussed in this paper.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Polycrystal Plasticity: Comparison Between Grain - Scale Observations of Deformation and Simulations

Here, the response of polycrystals to plastic deformation is studied at the level of variations within individual grains, and comparisons are made to theoretical calculations using crystal plasticity (CP). We provide a brief overview of CP and a review of the literature, which is dominated by surface observations. The motivating question asks how well does CP represent the mesoscale behavior of large populations of dislocations (as carriers of plastic strain). The literature shows consistently that only moderate agreement is found between experiment and calculation. We supplement this with a current example of microstructure evolution in the interior of a copper sample subjected to tensile deformation. Nondestructive measurements of orientation fields were performed using the near-field high-energy X-ray diffraction microscopy (nf-HEDM) technique at the Advanced Photon Source (APS). Starting at highly ordered grains, a single two-dimensional slice of microstructure containing ~150 grains was followed through multiple strain states, where it tracked lattice rotations and defect accumulation of up to 14% elongation. In accord with the literature, at the scale of individual grains, comparison of observations with CP models indicates reasonable qualitative agreement but significant variations between simulation and experiment are apparent. The conclusion is that in order to be able to quantify the effects of microstructure on the distributions of slip, orientation change, and damage accumulation, the empirically derived constitutive relations used in continuum-scale simulations need to be improved. Equally important will be the development of large-scale simulations of polycrystals that directly model dislocations.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Evolution of dislocation substructures in metals via high-strain-rate nanoindentation

Deformation at high strain rates often results in high stresses on many engineering materials, potentially leading to catastrophic failure without proper design. High-strain-rate mechanical testing is thus needed to improve the design of future structural materials for a wide range of applications. Although several high-strain-rate mechanical testing techniques have been developed to provide a fundamental understanding of material responses and microstructural evolution under high-strain-rate deformation conditions, these tests are often very time consuming and costly. In this work, we utilize a high-strain-rate nanoindentation testing technique and system in combination with transmission electron microscopy to reveal the deformation mechanisms and dislocation substructures that evolve in pure metals from low (10 –2 s –1 ) to very high indentation strain rates (10 4 s –1 ), using face-centered cubic aluminum and body-centered cubic molybdenum as model materials. The results help to establish the conditions under which micro- and macro-scale tests can be compared with validity and also provide a promising pathway that could lead to accelerated high-strain-rate testing at substantially reduced costs.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Radiation damage of a two-dimensional carbon fiber composite (CFC)

Carbon fiber composites (CFC) are, among other applications, already in use as low-impedance collimating elements for intercepting TeV-level protons machines, like the CERN Large Hadron Collider. Towards a comprehensive understanding of these materials’ properties and behavior, a series of radiation damage campaigns have been undertaken in order to quantitively investigate the response of AC-150 K CFC to high proton fluences. The CFCs dimensional changes, stability, micro-structural evolution, and structural integrity below and above 5 × 10 20 p/cm 2 fluence threshold were studied. The irradiating particles were protons of kinetic energies in the range of 130–200 MeV. The effects of the irradiation temperature (~90–180°C and 280–500°C) combined with the proton fluence on the dimensional stability and the microstructural evolution of this anisotropic two-dimensional composite structure were studied using precision dilatometry and X-ray diffraction. Our results shed light on the fluence-based limitations for these composite materials. Furthermore, we compare these results with reference unirradiated graphite, and we discuss the similarities and differences in the dimensional changes and post-irradiation annealing properties.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Mirostructure Characterization of Friction Consolidated Copper-Nickel using a Machine Learning Approach: Developing Process to Microstructure Associations

Friction consolidation (FC) is a solid phase processing approach where discrete material forms such as powders, chips, nuggets, etc. are densified via shear deformation. The precursors are placed in a billet container and brought in contact with a rotating tool that applying the desirable amount of normal force. Under the combined action of the rotation and normal pressure, the discrete precursor is consolidated through porosity reduction and shear deformation. FC is increasingly being studied as an attractive approach to manufacturing fully dense parts from powder forms owing to its ability to mix, alloy and consolidate difficult-to-process precursors in minimal number of process steps. Material consolidation and deformation in shear consolidation processes have been studied extensively previously for different material combinations previously. However, despite the extensive research in this area, understanding of the mechanistic processes in pore consolidation, deformation-induced mixing and material solubility during FC is still evolving. Material development using solid phase processing approaches such as FC is often performed based on research experience/education, which can be biased. Conventional analysis and simulation tools in this area tend to be successful only when material thermodynamic pathways and microstructural evolution sequences resulting from processing are clearly defined or known. They are not as effective for emerging advanced manufacturing technologies where material evolution pathways are not well established. The ability to predict optimal process parameters based on material chemistry and bulk properties is essential to accelerate materials design and processing, as are an understanding of the relevant structure-processing-property relationships. These structure-processing-property-performance relationships are at the core of materials science research. Microstructure characterization provides the link to these four core areas, often through visualizing material microstructure using imaging techniques. However, linking microstructure image data (i.e., micrographs) to variables of interest (e.g., processing parameters, material chemistry) in a reproducible, generalizable, and quantitative manner is a significant challenge. Typically, quantitatively linking image data to processing history relies on significant domain knowledge and manual or subject matter expert (SME)-heuristic based image analysis. Such an approach to image analysis has the potential to be biased, inefficient, and difficult to replicate.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The effect of boron addition on the deformation behavior and microstructure of β-solidify TiAl alloys

Highlights: • Borides could promote the DRX formation to soften TiAl alloys. • Boron addition increases firstly and then stabilizes the deformation activate energy. • The stable region expands with boron increasing in processing maps. • The DRX critical strain increases firstly and then decreases with boron increasing. • DRX softening and strengthening from solid solution and borides influence deformation behavior. - Abstract: The effect of boron addition on the deformation behavior and microstructure of Ti-43Al-6Nb-1Mo -1Cr alloys have been studied in this paper. Boron addition would induce Ti{sub 2}Al(P6{sub 3}/mmc) phase with hexagonal structure formation on the interfaces between TiB and γ phase. TiB would be the obstacles for dislocations slipping and increase the stacking fault energy. Ti{sub 2}Al could also provide the chemical foundation for DRXed γ nucleation and disappear after thermal deformation. Both these two phase could promote DRXed grains nucleation to soften the alloys during thermal deformation. With the strengthen effect of boron solid solution and TiB obstacles, the microstructure evolution, phase transformation and deformation behavior are also discussed and concluded as follow.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Effects of Cold Rolling on Microstructure and Mechanical Properties of Fe-30Mn-3Si-4Al-0.093C TWIP Steel

The effects of cold rolling on microstructure evolution and the associated mechanical properties of Fe-30Mn-3Si-4Al-0.093C twinning-induced plasticity (TWIP) steel are examined in this work with reduction rates of 10%, 20%, 30%, 40%, 50%, 60%, and 70%. Through texture analysis and transmission electron microscopy (TEM) observations, it is suggested that slip, mechanical twinning, the interaction between dislocation/twin boundaries (TB), and shear band have influenced the observed mechanical behavior and development of texture. Special components of weak initial textures are preferential for mechanical twinning, resulting in an increase in strain hardening rate. By mechanical twinning, the {111}<112> orientation is rotated into a position at the vicinity of the {110}<001> Goss orientation, and the {552}<115> (Cu-twin) texture is transformed to the {110}<001> orientation. The evolution of texture is closely related to the onset of shear banding resulting from deformation twinning. The sample with 10% cold reduction exhibits a favorable combination of yield strength and ductility, indicating a considerable capacity for energy absorption. With increasing rolling reductions, the deformation of the samples becomes inhomogeneous due to the high anisotropy of the microstructure. The localized shear bands resulting from the excessive cold rolling are detrimental to the ductility of the present TWIP steel.

Shen, Yongfeng↗
DOE OSTI2023

Annealing influence on the microstructure of irradiated U-Mo monolithic fuel foils

In this study we compared the microstructure evolution of U-Mo fuel foils produced with and without heat treatment at low burn-up via advanced post-irradiation examination. The aim of this study is to observe after irradiation the ways in which the fabrication processes have influenced fuel behavior at early-stage irradiation, as for very low burn up microstructural studies are lacking. In this work it was observed that the larger grain size detected in the heat-treated samples before irradiation led to decreased grain refinement after irradiation. Grain refinement was associated with the presence of small nano-size bubbles and precipitates. This phenomenon is hypothesized to influence early fuel swelling during reactor irradiation. Grain refinement was also observed to increase in regions where γ-U decomposition was present. Thus, it was enhanced in the samples fabricated without heat treatment. The heat treatment also increased the thickness of the U-Mo/Zr interface, namely of the UZr 2 layer. However, the influence of this layer on fuel performance needs further investigation. On one side, it may contribute to better mechanical bonding; on the other, it may influence swelling and blistering in the interaction layer as porosity increases when this layer is increased. This was observed especially in the presence of increased area containing low Mo concentration, and thus containing a higher fraction of the α-U phase, which is highly susceptible to irradiation induced swelling. Strong evidence of reverse transformation under irradiation (α-U + γ'-U2Mo → bcc γ-U) was observed in these samples. While the precipitates (carbides and oxide) seem to be unaffected by the irradiation at these low burnups. However, further analyses are necessary at higher burn-up to assess the exact impact different heat treatments have on fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Effects of in-process cryocooling on metallurgical and mechanical properties of friction stir processed Al7075 alloy

Highlights: • For in-process cryocooling (IPC) during FSP, an efficient cooling fixture was designed & fabricated. • FSP of Al7075 alloy with IPC setup suppressed precipitate coarsening as well as grain growth. • Nanosize η′ precipitates (20–30 nm) in IPC condition increased work hardening capacity & strength. • Simultaneous improvement in ductility & strength occurred for sample FSPed with IPC. - Abstract: Friction stir processing (FSP) of heat treatable aluminum alloys is reported to deteriorate strength and hardness properties in spite of huge grain size refinement. The improvement in strength due to the grain size refinement after FSP could not be able to offset the reduction in strength due to coarsening or dissolution of the strengthening precipitate(s). To overcome this, the present work investigates an effective way of heat rejection from the FSP zone to control the precipitate evolution besides the grain size refinement during FSP of Al7075 alloy. The FSP was carried out with standardized process parameters (i.e. 720 rpm, 65 mm/min traverse speed) under two different cooling environments: (i) at normal air cooling and (ii) by rushing a chilled mixture (−30 °C) of liquid nitrogen and methanol through the bottom of the backing plate. Microstructural evolution was examined through optical, scanning and transmission electron microscopy and electron backscatter diffraction to confirm the grain size and morphology of precipitate(s) formed. The in-process cryocooling during the FSP led to 65 and 72% improvement in the Vickers hardness and tensile strength, respectively, in comparison to the solutionized base metal. The results have been analyzed in terms of precipitate interface characteristics and its strengthening effect, Hall–Petch strengthening due to grain size reduction and tradeoff between them.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Evolution of sputtered tungsten coatings at high temperature

Sputtered tungsten (W) coatings were investigated as potential high temperature nanophotonic material to replace bulk refractory metal substrates. Of particular interest are materials and coatings for thermophotovoltaic high-temperature energy conversion applications. For such applications, high reflectance of the substrate in the infrared wavelength range is critical in order to reduce losses due to waste heat. Therefore, the reflectance of the sputtered W coatings was characterized and compared at different temperatures. In addition, the microstructural evolution of sputtered W coatings (1 and 5 μm thick) was investigated as a function of anneal temperature from room temperature to 1000 °C. Using in situ x-ray diffraction analysis, the microstrain in the two samples was quantified, ranging from 0.33% to 0.18% for the 1 μm sample and 0.26% to 0.20% for the 5 μm sample, decreasing as the temperature increased. The grain growth could not be as clearly quantified due to the dominating presence of microstrain in both samples but was in the order of 20 to 80 nm for the 1 μm sample and 50 to 100 nm for the 5 μm sample, as deposited. Finally, the 5 μm thick layer was found to be rougher than the 1 μm thick layer, with a lower reflectance at all wavelengths. However, after annealing the 5 μm sample at 900 °C for 1 h, its reflectance exceeded that of the 1 μm sample and approached that of bulk W found in literature. Overall, the results of this study suggest that thick coatings are a promising alternative to bulk substrates as a low cost, easily integrated platform for nanostructured devices for high-temperature applications, if the problem of delamination at high temperature can be overcome.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Lattice rotations in precipitate free zones in an Al-Mg-Si alloy

Highlights: • Recovery processes in precipitate free zones differ from those in grain interiors. • Most precipitate free zones contain few dislocations, after deformation. • Deformation can induce large misorientations in precipitate free zones. • Some deformed precipitate free zones contain nanoscale grains. - Abstract: Scanning precession electron diffraction and automated crystal orientation mapping in a transmission electron microscope (TEM) have been applied to quantitatively study the crystal orientation of precipitate free zones (PFZs) of four GB regions in an AA6060 alloy in peak aged condition (temper T6) after uniaxial compression to 20% engineering strain. The PFZ width in the alloy was found to be w = 170 ± 40 nm. The results show that some PFZs develop significant misorientations relative to their parent grain, and represent, to the best knowledge of the authors, the first quantitative evidence of this. This misorientation may either be constant inside a particular PFZ, making it appear like a band or a very elongated subgrain, or be partitioned in discrete regions with a diameter comparable to the PFZ width, making the former PFZ into a collection of small grains. The band-like PFZ observed in this work had a misorientation relative to its parent grain of ≈ 7°, while the grain-like PFZ had grains with misorientations between ≈ 12° and ≈ 20° relative to its parent grain. The other PFZs that were observed had only limited misorientations relative to their parent grains, and had either dislocations perpendicular to the GB plane or a dislocation wall at the transition region. A general TEM study of the material at various engineering strains was also conducted and suggests that grain-like PFZs are more frequent for larger strains, indicating that the different PFZ features are likely due to different strain localisation in individual PFZs. This localisation is expected to be influenced by the orientation of the loading axis relative to crystal orientations and GB planes. It is also suggested that the different PFZ features engender different work hardening rates and possibly affect nucleation of intergranular fracture. The results support previous studies on the microstructure evolution of PFZs in age-hardenable aluminium alloys during deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Correlation between Grain Size Distribution and Grain Boundary Character in Polycrystalline Uranium Dioxide

Thermo-mechanical behavior of oxide nuclear fuels is extremely important to overall fuel element performance. Critical to the understanding of Pellet-Cladding Mechanical Interactions (PCMI) are elasticity, plasticity and creep, as this interaction with the cladding can lead to fuel rod fracture and in turn affect its thermal performance significantly. In addition, sub-grain scale mechanical behavior, e.g. elastic anisotropy, as well as dislocation-driven plasticity and creep, can also play a significant role on microstructure evolution of the fuel elements and their cladding, failure of which would severely reduce the useful service life of the elements and allow the release of fission products out into the working fluid of the reactor. Therefore, careful measurements of mechanical properties are key to validate robust fuel performance codes able to predict this PCMI behavior from inputs at the micro-scale, e.g., MARMOT, and to quantify its effects on other aspects of fuel behavior. In uranium dioxide (UO{sub 2}), the thermomechanical response at the meso-scale depends strongly on crystallography of individual grains, and available datasets are far from complete in terms of temperature, stress, and stoichiometry in parameter space. Therefore, details of the fuel microstructure, such as porosity distribution and location, as well as grain boundary (GB) character, distribution, and location are needed to create accurate multiscale models to predict the fuel's evolution in-pile, and in turn aid in the design and development of more efficient fuels that can last longer cycles.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2013

The role of alumina on performance of alkali-activated slag paste exposed to 50 °C

The strength and microstructural evolution of two alkali-activated slags, with distinct alumina content, exposed to 50 °C have been investigated. These two slags are ground-granulated blast furnace slag (containing 13% (wt.) alumina) and phosphorous slag (containing 3% (wt.) alumina). They were hydrated in the presence of a combination of sodium hydroxide and sodium silicate solution at different ratios. The microstructure of the resultant slag pastes was assessed by X-ray diffraction, differential thermogravimetric analysis, and scanning electron microscopy. The results obtained from these techniques reveal the presence of hexagonal hydrates: CAH{sub 10} and C{sub 4}AH{sub 13} in all alkali-activated ground-granulated blast-furnace slag pastes (AAGBS). These hydrates are not observed in pastes formed by alkali-activated ground phosphorous slag (AAGPS). Upon exposure to 50 °C, the aforementioned hydration products of AAGBS pastes convert to C{sub 3}AH{sub 6}, leading to a rapid deterioration in the strength of the paste. In contrast, no strength loss was detected in AAGPS pastes following exposure to 50 °C. -- Highlights: •Strength of alkali-activated slag (AAS) pastes after exposure to 50 °C is studied. •AAS pastes with high alumina content lose strength after the exposure. •C{sub 4}AH{sub 13} and CAH{sub 10} form in these AAS pastes. •Conversion of these calcium alumina hydrates is associated with the strength loss. •AAS pastes with low alumina content maintain its strength after the exposure.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Alternative High-Performance Ceramic Waste Forms

This final report (M5NU-12-NY-AU # 0202-0410) summarizes the results of the project titled “Alternative High-Performance Ceramic Waste Forms,” funded in FY12 by the Nuclear Energy University Program (NEUP Project # 12-3809) being led by Alfred University in collaboration with Savannah River National Laboratory (SRNL). The overall focus of the project is to advance fundamental understanding of crystalline ceramic waste forms and to demonstrate their viability as alternative waste forms to borosilicate glasses. We processed single- and multiphase hollandite waste forms based on simulated waste streams compositions provided by SRNL based on the advanced fuel cycle initiative (AFCI) aqueous separation process developed in the Fuel Cycle Research and Development (FCR&D). For multiphase simulated waste forms, oxide and carbonate precursors were mixed together via ball milling with deionized water using zirconia media in a polyethylene jar for 2 h. The slurry was dried overnight and then separated from the media. The blended powders were then subjected to melting or spark plasma sintering (SPS) processes. Microstructural evolution and phase assemblages of these samples were studied using x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion analysis of x-rays (EDAX), wavelength dispersive spectrometry (WDS), transmission electron spectroscopy (TEM), selective area x-ray diffraction (SAXD), and electron backscatter diffraction (EBSD). These results showed that the processing methods have significant effect on the microstructure and thus the performance of these waste forms. The Ce substitution into zirconolite and pyrochlore materials was investigated using a combination of experimental (in situ XRD and x-ray absorption near edge structure (XANES)) and modeling techniques to study these single phases independently. In zirconolite materials, a transition from the 2M to the 4M polymorph was observed with increasing Ce content. The resulting powders were consolidated via SPS. Ce was reduced to the trivalent oxidation state and the zirconolite was converted into undesirable perovskite. The zirconolite polymorphs found in the synthesized powders were recovered after a post-SPS heat treatment in air. These results demonstrated the potential of processing in controlling the phase assemblage in these waste forms. Hollandites with Cr 3+ trivalent cations were identified as potential hosts for Cs immobilization and are being investigated for Cs retention properties. Series of compositions Ba 1.15-x Cs 2x Cr 2.3 Ti 5.7 O 16 , with increasing Cs loadings, were prepared by sol-gel process and characterized for structural parameters. Structural characterization was performed by a combination of powder XRD and neutron powder diffraction. Phase pure hollandite adapting monoclinic symmetry (I2/m) was observed for 0 ≤ x ≤ 0.55. These results were used to develop a new structural model to interpret Cs immobilization in these hollandites. Performance of these waste forms were evaluated for chemical durability and radiation resistance. Product consistency testing (PCT) and vapor hydration testing (VHT) were used for testing of chemical durability. Radiation resistance was tested using He + ions to simulate $\alpha$ particles and heavy ions such as Au 3+ to simulate a recoil. These results showed that these waste forms were chemically durable. The waste forms also amorphized to various degrees on exposure to simulated radiation.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗