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Microstructural and thermal properties of pure BaFe{sub 12}O{sub 19} and Sr doped barium ferrite (Ba{sub 0.9}Sr{sub 0.1}Fe{sub 12}O{sub 19}) synthesized by auto combustion method

Nanoparticles (NPs) of Pure BaFe{sub 12}O{sub 19} and Strontium doped Barium Ferrite (Ba{sub 0.9}Sr{sub 0.1}Fe{sub 12}O{sub 19}) have been successfully synthesized by Auto combustion method using citric acid as a chelating agent and calcined at 450°C for 3 hrs and 850°C for 4 hrs. Microstructural studies were carried by XRD and SEM techniques. Structural studies suggest that the crystal system remains hexagonal even with the doping of Strontium. The XRD analysis confirms the formation of the structures in the nanometer regime and the peaks are the evidence of the crystalline phase. The SEM images shows the morphology of surface of the samples. The thermal property studied by TGA shows the weight loss which is with varying the temperature and weight loss also varies with Sr doping. The TGA analysis exhibits the loss of weight at different temperatures.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

High temperature oxidation behavior of a high Al-containing ferritic heat-resistant stainless steel

Highlights: • Oxidation kinetics has been analyzed by discontinuous weighing. • Microstructure and phase composition of oxide films were investigated by SEM, EDS and XRD analysis. • The oxidation resistance of 1000 °C is obviously deteriorated comparing with that at 800 °C and 900 °C. • The oxidation mechanism has been discussed. - Abstract: The high temperature oxidation behavior of a high Al-containing ferritic heat-resistant stainless steel at temperatures of 800, 900, and 1000 °C in air were studied in isothermal oxidation tests. The results showed that the isothermal oxidation kinetic curves obtained at different temperatures followed the parabolic law, and the weight gain per unit at 1000 °C was significantly higher than that at 800 and 900 °C. The oxidation rate at 1000 °C was about three times faster than that at 800 and 900 °C. Continuous and compact multicomponent oxide films mainly composed of Cr{sub 2}O{sub 3}, Al{sub 2}O{sub 3}, spinel MnFe{sub 2}O{sub 4}, and MnCr{sub 2}O{sub 4} were obtained at 800 and 900 °C. The oxide film started delaminating at 1000 °C; the outer layer was composed of Cr{sub 2}O{sub 3}, spinel MnCr{sub 2}O{sub 4}, and MnFe{sub 2}O{sub 4}, the middle layer was composed of Fe{sub 2}O{sub 3} and Fe-Cr matrix, and the inner layer was composed of Al{sub 2}O{sub 3} and SiO{sub 2}. Oxidation resistance at 1000 °C was reduced mainly because of porous Fe{sub 2}O{sub 3} and inner oxidation of Al and Si. In addition, the oxidation mechanism was discussed based on kinetic and morphological observations.

36 MATERIALS SCIENCE↗

High Schottky barrier at grain boundaries observed in Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics

Graphical abstract: - Highlights: • NSCTO exhibits a high ε′ of 7.0–8.4 × 10{sup 3} and low tan δ of 0.030–0.041. • NSCTO exhibits a high E{sub b} of ∼2208 V cm{sup −1} and large α of 15.6. • Giant ε′ response is attributed to the electrically heterogeneous microstructure. • High Φ{sub b} values at grain boundaries are found to be 0.925–0.964 eV. • Formation of a potential barrier at grain boundaries is caused by Schottky effect. - Abstract: The dielectric properties and nonlinear current–voltage characteristics of Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics prepared by a conventional solid state reaction method were investigated. Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics exhibited a high dielectric permittivity of 7.0–8.4 × 10{sup 3} and low loss tangent (tan δ∼0.030–0.041). Non-Ohmic properties with a high breakdown voltage of ∼2208 V cm{sup −1} and large nonlinear coefficient of 15.6 were observed in Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics. Using complex impedance analysis, Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics were shown to be electrically heterogeneous consisting of semiconducting grains and insulating grain boundaries. Giant dielectric properties were described based on the electrically heterogeneous microstructure. X-ray photoelectron spectroscopy analysis suggested that the semiconductive nature of grains may be related to the presence of Cu{sup +} and Ti{sup 3+}. The formation of an electrostatic potential barrier at the grain boundaries of Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics was suggested to be caused by the Schottky effect. Interestingly, high electrostatic potential barriers at grain boundaries in Na{sub 1/2}Sm{sub 1/2}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics were calculated and found to be 0.925–0.964 eV.

36 MATERIALS SCIENCE↗

Analytical Ultrasonics in Materials Research and Testing

Research results in analytical ultrasonics for characterizing structural materials from metals and ceramics to composites are presented. General topics covered by the conference included: status and advances in analytical ultrasonics for characterizing material microstructures and mechanical properties; status and prospects for ultrasonic measurements of microdamage, degradation, and underlying morphological factors; status and problems in precision measurements of frequency-dependent velocity and attenuation for materials analysis; procedures and requirements for automated, digital signal acquisition, processing, analysis, and interpretation; incentives for analytical ultrasonics in materials research and materials processing, testing, and inspection; and examples of progress in ultrasonics for interrelating microstructure, mechanical properites, and dynamic response.

Vary, A.↗

Development and characterisations of WC–12Co microwave clad

In the present work, WC–12Co based cermet clad was developed on AISI 304 stainless steel using microwave hybrid heating technique. The experimental trials were carried out in a 1.4 kW industrial multimode microwave applicator. The paper explains the major events occurring during microwave irradiation and formation of clad. The developed clads were subsequently characterised through field emission scanning electron microscopy equipped with energy dispersive X-ray spectroscopy, X-ray diffraction, assessment of porosity and microhardness. The WC–12Co clads developed with an approximate thickness of 1 mm, illustrated excellent metallurgical bonding with substrate. The microstructure of the WC–12Co clad mainly consists of skeleton structured carbides embedded in tough metallic phase. The phase analysis of the developed clads indicate the presence of various stable and complex carbides like Co{sub 6}W{sub 6}C, Co{sub 3}W{sub 3}C and Fe{sub 6}W{sub 6}C. The uniform distribution of such carbides with skeleton-like morphology in the microstructure is indicative of high hardness of the clad. The developed clads were free from visible interfacial cracking and the clad porosity was found in the order of approximately 0.98%. The average microhardness of the WC–12Co microwave clads was observed to be 1135 ± 88 HV. - Highlights: • Microwave cladding of WC–12Co on AISI 304 stainless steel is carried out. • Skeleton-like structures of W–Co based carbides are embedded in metallic matrix. • Clad–substrate interface is free from un-melted and un-dissolved carbide particles. • Hardness of clad (1135 ± 88 HV) is 3.5 times that of the substrate (325 ± 49 HV)

36 MATERIALS SCIENCE↗

Agglomerates in Polymer Electrolyte Fuel Cell Electrodes: Part I. Structural Characterization

This two-part study characterizes the structural and transport properties of polymer electrolyte fuel cell (PEFC) cathode catalyst electrode. The agglomerates comprising the electrode are characterized with nano scale resolution X-ray computed tomography (nano-CT). A hybrid reconstruction technique is used to further refine the 3-D agglomerate microstructure and obtain 1-nm voxel resolution of the constituent catalyst, ionomer, carbon support and primary and secondary pore phases. Our analysis of nano-CT data shows that the electrode composition is heterogeneous and the agglomerates have structural heterogeneities in terms of size and composition. There is a strong correlation between the ionomer to carbon weight ratio (I/C) and agglomerate microstructure, suggesting that ionomer plays role in formation of larger agglomerates. With the hybrid reconstructions, we show that ionomer film thickness is spatially non-uniform inside the agglomerate and is strongly dependent on the I/C. Smaller agglomerate size and high I/C are shown to favor the ionomer impregnation. We demonstrate that the majority of the primary pores are smaller than 15 nm for I/C = 0.8 and higher I/C reduces the primary pore size. We also characterize the uniformity of the catalyst distribution and show that the majority of the catalyst is located away from the agglomerate surface.

agglomerate↗

Dislocation Substructures on the Functional Properties of Niobium for SRF Cavities, focusing on microstructural,microchemical, and electromagnetic characteristic for Florida State University.

Funding is being requested pursuant to a proposal that was submitted and reviewed through the Portfolio Analysis and Management System (PAMS). PAMS Proposal ID: 222686. Superconducting cavities are the integral part of many energy-efficient particle accelerators around the world. The current material of choice for superconducting cavities is niobium, which is the material with the highest transition temperature among pure metals. The performance of SRF cavities are influenced by the fabrication and processing steps. We plan to study the microstructural, microchemical and electromagnetic properties of Nb that are processed similar to the cavity processing steps to identify and mitigate the limiting factors to improve the performance of SRF cavities.

99 GENERAL AND MISCELLANEOUS↗

Focal Gray Matter Plasticity as a Function of Long Duration Head Down Tilted Bed Rest: Preliminary Results

Long duration spaceflight (i.e., 22 days or longer) has been associated with changes in sensorimotor systems, resulting in difficulties that astronauts experience with posture control, locomotion, and manual control. The microgravity environment is an important causal factor for spaceflight induced sensorimotor changes. Whether these sensorimotor changes are solely related to peripheral changes from reduced vestibular stimulation, body unloading, body fluid shifts or that they may be related to structural and functional brain changes is yet unknown. However, a recent study reported associations between microgravity and flattening of the posterior eye globe and protrusion of the optic nerve [1] possibly as the result of increased intracranial pressure due to microgravity induced bodily fluid shifts [3]. Moreover, elevated intracranial pressure has been related to white matter microstructural damage [2]. Thus, it is possible that spaceflight may affect brain structure and thereby cognitive functioning. Long duration head down tilt bed rest has been suggested as an exclusionary analog to study microgravity effects on the sensorimotor system [4]. Bed rest mimics microgravity in body unloading and bodily fluid shifts. In consideration of the health and performance of crewmembers both in- and post-flight, we are conducting a prospective longitudinal 70-day bed rest study as an analog to investigate the effects of microgravity on brain structure [5]. Here we present results of the first six subjects. Six subjects were assessed at 12 and 7 days before-, at 7, 30, and ~70 days in-, and at 8 and 12 days post 70 days of bed rest at the NASA bed rest facility in UTMB, Galveston, TX, USA. At each time point structural MRI scans (i.e., high resolution T1-weighted imaging and Diffusion Tensor Imaging (DTI)) were obtained using a 3T Siemens scanner. Focal changes over time in gray matter density were assessed using the voxel based morphometry 8 (VBM8) toolbox under SPM. Longitudinal processing in VBM8 includes linear registration of each scan to the mean of the subject and subsequently transforming all scans in to MNI space by applying the warp from the mean subject to MNI to the individual gray matter segmentations. Modulation was applied so that all images represented the volume of the original structure in native space. Voxel wise analysis was carried out on the gray matter images after smoothing, using a flexible factorial design with family wise error correction. Focal changes in white matter microstructural integrity were assessed using tract based spatial statistics (TBSS) as part of FMRIB software library (FSL). TBSS registers all DTI scans to standard space. It subsequently creates a study specific white matter skeleton of the major white matter tracts. For each subject, for each DTI metric (i.e. fractional anisotropy (FA), mean diffusivity (MD), axial diffusivity (AD), and radial diffusivity (RD)), the maximum value in a line perpendicular to the skeleton tract is projected to the skeleton. Non-parametric permutation based t-tests and ANOVA's were used for voxel-wise comparison of the skeletons. For both VBM and TBSS, comparison of pre bed rest measurements did not show significant differences. VBM analysis revealed decreased gray matter density in bilateral areas including the frontal medial cortex, the insular cortex and the caudate (see Figure) from 'pre to in bed rest'. Over the same time period, there was an increase in gray matter density in the cerebellum, occipital-, and parietal cortex, including the precuneus (see Figure). The majority of these changes did not recover from 'during to post bed rest'. TBSS analysis did not reveal significant changes in white matter microstructural integrity after correction for multiple comparisons. Uncorrected analyses (p<.015) revealed an increase in RD in the cerebellum and brainstem from pre bed rest to the first week in bed rest that did not recover post bed rest. Extended bed rest, which is an analog for microgravity, can result in gray matter changes and potentially in microstructural white matter changes in areas that are important for neuro motor behavior and cognition. These changes did not recover at two weeks post bed rest. Whether the effects of bed rest wear off at longer times post bed rest, and if they are associated with behavior are important questions that warrant further research.

Koppelmans, V.↗

Combustion synthesis and luminescence properties of yellow-emitting phosphors Ca{sub 2}BO{sub 3}Cl:Eu{sup 2+}

Graphical abstract: A yellow-emitting phosphor Ca{sub 2}BO{sub 3}Cl:Eu{sup 2+} was firstly synthesized by the solution-combustion method. The photoluminescence excitation and emission spectra, temperature dependence of luminescence intensity, and luminescence lifetime of the phosphor were investigated. Highlights: Black-Right-Pointing-Pointer Ca{sub 2}BO{sub 3}Cl:Eu{sup 2+} phosphor was synthesized by a solution-combustion method. Black-Right-Pointing-Pointer Ca{sub 2}BO{sub 3}Cl:Eu{sup 2+} showed an intense yellow emission band centered at 569 nm with the CIE coordinate of (0.453, 0.526). Black-Right-Pointing-Pointer The temperature dependent luminescence property and mechanism of Ca{sub 2}BO{sub 3}Cl:Eu{sup 2+} were studied. -- Abstract: Yellow-emitting phosphor Ca{sub 2}BO{sub 3}Cl:Eu{sup 2+} was synthesized by a solution-combustion method. The phase structure and microstructure were determined by the X-ray diffraction (XRD) and scanning electron microscope (SEM) analysis, respectively. The as-prepared Ca{sub 2}BO{sub 3}Cl:Eu{sup 2+} phosphor absorbed near ultraviolet and blue light of 320-500 nm, and showed an intense yellow emission band centered at 569 nm with the CIE coordinate of (0.453, 0.526). The lifetime of Eu{sup 2+} ions in Ca{sub 2}BO{sub 3}Cl:Eu{sup 2+} phosphor was measured, furthermore the temperature dependent luminescence property and mechanism were studied, which also testified that the present phosphor had a promising potential for white light-emitting diodes.

36 MATERIALS SCIENCE↗

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↗

Photoactive Blend Morphology Engineering through Systematically Tuning Aggregation in All-Polymer Solar Cells

Polymer aggregation plays a critical role in the miscibility of materials and the performance of all-polymer solar cells (APSCs). However, many aspects of how polymer texturing and aggregation affect photoactive blend film microstructure and photovoltaic performance are poorly understood. Here the effects of aggregation in donor–acceptor blends are studied, in which the number-average molecular weights (Mns) of both an amorphous donor polymer, poly[4,8-bis(5-(2-ethylhexyl)thiophen-2-yl)benzo[1,2-b;4,5-b]dithiophene-2,6-diyl-alt-(4-(2-ethylhexyl)-3-fluorothieno[3,4-b]thiophene-)-2-carboxylate-2-6-diyl)] (PBDTT-FTTE) and a semicrystalline acceptor polymer, poly{[N,N'-bis(2-octyldodecyl)naphthalene-1,4,5,8-bis(dicarboximide)-2,6-diyl]-alt-5,5'-(2,2'-bithiophene)} (P(NDI2OD-T2)) are systematically varied. The photovoltaic performance is correlated with active layer microstructural and optoelectronic data acquired by in-depth transmission electron microscopy, grazing incidence wide-angle X-ray scattering, thermal analysis, and optical spectroscopic measurements. Coarse-grained modeling provides insight into the effects of polymer aggregation on the blend morphology. Notably, the computed average distance between the donor and the acceptor polymers correlates well with solar cell photovoltaic metrics such as short-circuit current density (Jsc) and represents a useful index for understanding/predicting active layer blend material intermixing trends. Importantly, these results demonstrate that for polymers with different texturing tendencies (amorphous/semicrystalline), the key for optimal APSC performance, photovoltaic blend morphology can be controlled via both donor and acceptor polymer aggregation.

bio-inspired↗

Physicochemical evolution of uranium nitride kernel microstructure with varying carbon distribution for advanced TRISO fuel forms

Uranium nitride (UN) has emerged as a fuel candidate for advanced nuclear reactor concepts due to its superior uranium density, thermal conductivity, and high melting temperature. However, the fabrication route for converting UO 2 to UN is complex and difficult to standardize. Although the chemistry of this conversion process is well-studied, more insight into the physicochemical dynamics of this conversion using advanced characterization techniques can help further our understanding of this material system. This work leveraged thermogravimetric analysis (TGA), X-ray diffraction (XRD), and nondestructive 3D X-ray computed tomography (XCT) to characterize dynamic microstructural changes in the UO 2 → UCO → UN fabrication pathway for two kernels with a varying carbon distribution in the starting composition. TGA and XRD were used to quantify changes in the mass, density, and chemical composition of the two kernels, while three-dimensional image processing and segmentation of XCT data were used to quantify the volume, surface area, and spatial distribution of features within each kernel for multiple steps along the fabrication pathway. The analysis indicates distinct differences between the two kernels that are correlated to downstream conversion efficiency. In conclusion, this work is among the first to perform 3D quantification of physicochemical evolution during UN conversion, providing quantitative correlation between processing, properties, and expected fuel performance.

Nuclear fuel↗

Gas atomized precursor alloy powder for oxide dispersion strengthened ferritic stainless steel

Gas atomization reaction synthesis (GARS) was employed as a simplified method for producing precursor powders for oxide dispersion strengthened (ODS) ferritic stainless steels (e.g., Fe-Cr-Y-(Ti,Hf)-O), departing from the conventional mechanical alloying (MA) process. During GARS processing a reactive atomization gas (i.e., Ar-O 2 ) was used to oxidize the powder surfaces during primary break-up and rapid solidification of the molten alloy. This resulted in envelopment of the powders by an ultra-thin (t < 150 nm) metastable Cr-enriched oxide layer that was used as a vehicle for solid-state transport of O into the consolidated microstructure. In an attempt to better understand the kinetics of this GARS reaction, theoretical cooling curves for the atomized droplets were calculated and used to establish an oxidation model for this process. Subsequent elevated temperature heat treatments, which were derived from Rhines pack measurements using an internal oxidation model, were used to promote thermodynamically driven O exchange reactions between trapped films of the initial Cr-enriched surface oxide and internal Y-enriched intermetallic precipitates. This novel microstructural evolution process resulted in the successful formation of nano-metric Y-enriched dispersoids, as confirmed using high energy X-ray diffraction and transmission electron microscopy (TEM), equivalent to conventional ODS alloys from MA powders. The thermal stability of these Y-enriched dispersoids was evaluated using high temperature (1200°C) annealing treatments ranging from 2.5 to 1,000 hrs of exposure. In a further departure from current ODS practice, replacing Ti with additions of Hf appeared to improve the Y-enriched dispersoid thermal stability by means of crystal structure modification. Additionally, the spatial distribution of the dispersoids was found to depend strongly on the original rapidly solidified microstructure. To exploit this, ODS microstructures were engineered from different powder particle size ranges, illustrating microstructural control as a function of particle solidification rate. The consolidation of ultra-fine powders (dia. ≤ 5μm) resulted in a significant reduction in dispersoid size and spacing, consistent with initial scanning electron microscopy studies on as-atomized cross-sectioned particles that suggested that these powders solidified above the threshold velocity to effectively solute trap Y within the α-(Fe,Cr) matrix. Interestingly, when the solidification velocity as a function of particle size was extracted from the aforementioned theoretical particle cooling curves, it could be offered as supporting evidence for these microstructure observations. Thermal-mechanical treatments also were used to create and evaluate the stability of a dislocation substructure within these alloys, using microhardness and TEM analysis of the alloy sub-grain and grain structure. Moreover, elevated temperature tensile tests up to 800°C were used to assess the initial mechanical strength of the ODS microstructure.

36 MATERIALS SCIENCE↗

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↗

Spectro-Microscopic Analysis of Soot Particle Composition and Source Attribution

Ambient soot particles significantly impact Earth’s radiative balance, human health, and atmospheric visibility. Their microstructural properties depend on formation and aging mechanisms, which vary by emission source and atmospheric processes. Hence, accurately identifying sources of soot enhances our understanding of their physicochemical properties and atmospheric implications. This study used a multi-modal approach to characterize and attribute sources of submicron soot particles collected in Israel during new particle formation events, biomass burning episodes, and background atmospheric conditions. Synchrotron-based X-ray microscopy was used to map soot (elemental carbon), organic carbon, and inorganic species. Implemented atomic force microscopy showed highly diverse phase states, with soot consistently exhibiting a solid-like phase. Automated µ-Raman analysis was subsequently performed on ~690 particles, identifying three soot classes based on spectral features corresponding to the "Defect" (D) and "Graphite" (G) bands of soot. We applied two-peak and five-peak fitting approaches to deconvolute the “Defect” peaks (D1, D2, D3, and D4) and G band from average Raman, revealing varying degrees of graphitic order. The degree of graphitic order was determined from metrics such as the D3 peak area, often observed when soot was internally mixed with organic material. Raman spectral features, along with temporal variations in particle classes contributions, suggest that Particle Type 1 corresponds to traffic related soot and Particle Type 2 to less graphitic soot from biomass burning, while Particle Type 3 is associated with more heterogeneous particulate representative of soot-OC mixtures emitted during new particle formation and biomass burning episodes.

Rivera-Adorno, Felipe (ORCID:0000000273557999)↗

Interaction Between Liquid Silver and Graphene-Coated SiC Substrate

Wettability between liquid Ag and graphene-coated SiC single crystal has been investigated by dispensed drop method at T = 970 °C under vacuum accompanied with subsecond recording of the drop/substrate images (100 frames per second) by high-speed high-resolution CCD camera. Non-contact heating method coupled with capillary purification of the Ag drop procedure has been applied. Scanning electron microscopy combined with EDS analysis and scanning probe microscopy combined with Raman spectroscopy techniques has been utilized for microstructure and surface characterization of samples before and after high-temperature wetting tests. Immediately after its detachment from the capillary, the Ag drop showed non-wetting behavior (θ > 90°) forming a high contact angle of θ = 114°. Surface characterization of the drop surface after wettability tests evidenced the presence of graphene and Si transferred from the substrate to the top of Ag drop. These findings suggest chemical interaction phenomena occurring at the interface. Locally, an intimate contact between liquid Ag and SiC substrate was allowed by the appearance of discontinuities in the graphene layer basically produced by thermomechanical stress. Local dissolution of carbon into liquid Ag and its reorganization (by segregation, nucleation and growth) as secondary graphene layer at the Ag surface was also observed.

36 MATERIALS SCIENCE↗

Evaluation of P{sub 2}O{sub 5} distribution inside the main clinker minerals by the application of EPMA method

The formation of Portland clinker phases has taken place in thermodynamically non-equilibrium state between macro-oxides CaO, SiO{sub 2}, Al{sub 2}O{sub 3}, Fe{sub 2}O{sub 3} and MgO from raw meal and P{sub 2}O{sub 5} from bone meal. The paper deals with the study of clinker minerals as solid solutions with P{sub 2}O{sub 5} during the clinkerization of raw mixture containing bone meal (BM). The ash of BM has contributed as a raw material to the formation of different clinker phases. Electron probe microanalysis (EPMA) method was used to determine the preferential distribution of P{sub 2}O{sub 5} inside calcium silicate phases and its influence upon C{sub 2}S/C{sub 3}S ratio. Basing on these results, composition of solid solution of C{sub 2}S and C{sub 3}S was established.

36 MATERIALS SCIENCE↗

Ceramics from self-sustained reactions: Recent advances

Specific applications of self-sustained reactions to fabricate advanced ceramics, along with details such as synthesis conditions, mechanism of microstructure formation, and material properties, are overviewed. The latest achievements in the field include analysis of three such synthetic routes: reactive spark plasma sintering, combustion synthesis with mechanical stimulation, and solution combustion synthesis. Examples of fabrication of high-temperature nanostructured ceramics and composites, as well as non-equilibrium ceramic phases are also discussed.

36 MATERIALS SCIENCE↗