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At least 91 records · Page 5

Study on Microstructures and Mechanical Properties of Foam Titanium Carbide Ceramics Fabricated by Reaction Sintering Process

Foam titanium carbide (TiC) ceramics with a three-dimensional network structure were fabricated by the reaction sintering process, in which polyurethane foam was taken as the template, and TiO{sub 2} and phenolic resin were used as the reactants. Phase, microstructures and fracture morphologies of foam TiC ceramics were characterized by x-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The results show that when the mass ratios of phenolic resin and TiO{sub 2} (F/T) are (0.8-1.2): 1, foam TiC ceramics with pure TiC phase can be formed. As the F/T ratios increase, crystal lattice parameters of fabricated foam TiC ceramics become bigger. When the value of F/T decreases from 1.2 to 0.8, grain size of TiC grows larger and microstructures get denser; meanwhile, the compressive strength increases from 0.10 to 1.05 MPa. Additionally, either raising the sintering temperatures or extending holding time can facilitate the completion of the reaction process and increase the compressive strength.

36 MATERIALS SCIENCE↗

Initiating the Validation of CCIM Processability for Multi-phase all Ceramic (SYNROC) HLW Form: Plan for Test BFY14CCIM-C

This plan covers test BFY14CCIM-C which will be a first–of–its-kind demonstration for the complete non-radioactive surrogate production of multi-phase ceramic (SYNROC) High Level Waste Forms (HLW) using Cold Crucible Induction Melting (CCIM) Technology. The test will occur in the Idaho National Laboratory’s (INL) CCIM Pilot Plant and is tentatively scheduled for the week of September 15, 2014. The purpose of the test is to begin collecting qualitative data for validating the ceramic HLW form processability advantages using CCIM technology- as opposed to existing ceramic–lined Joule Heated Melters (JHM) currently producing BSG HLW forms. The major objectives of BFY14CCIM-C are to complete crystalline melt initiation with a new joule-heated resistive starter ring, sustain inductive melting at temperatures between 1600 to 1700°C for two different relatively high conductive materials representative of the SYNROC ceramic formation inclusive of a HLW surrogate, complete melter tapping and pouring of molten ceramic material in to a preheated 4 inch graphite canister and a similar canister at room temperature. Other goals include assessing the performance of a new crucible specially designed to accommodate the tapping and pouring of pure crystalline forms in contrast to less recalcitrant amorphous glass, assessing the overall operational effectiveness of melt initiation using a resistive starter ring with a dedicated power source, and observing the tapped molten flow and subsequent relatively quick crystallization behavior in pans with areas identical to standard HLW disposal canisters. Surrogate waste compositions with ceramic SYNROC forming additives and their measured properties for inductive melting, testing parameters, pre-test conditions and modifications, data collection requirements, and sampling/post-demonstration analysis requirements for the produced forms are provided and defined.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Numerical modelling of evaporation in a ceramic layer in the tape casting process

Evaporation of water from a ceramic layer is a key phenomenon in the drying process for the manufacturing of tape cast ceramics. This process contains mass, momentum and energy exchange between the porous medium and the free–flow region. In order to analyze such interaction processes, a Representative Elementary Volume (REV)–scale model concept is presented for coupling non–isothermal multi–phase compositional porous–media flow and single–phase compositional laminar free–flow. The preliminary results show the typical expected evaporation behaviour from a porous medium initially saturated with water, and its transport to the free–flow region according to the existent results from the literature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

The effects of carbonaceous inclusions and their distributions on dynamic failure processes in boron carbide ceramics

Commercially available boron carbide ceramics typically have heterogeneous microstructures that contain distributions of processing-induced inclusions. The inclusions that are rich in carbon (i.e., carbonaceous) govern the underlying mechanisms of brittle fracture through wing crack formation, and thus dictate the mechanical response of the ceramic. In this study, we investigate the dynamic failure of five boron carbide ceramic materials with different inclusion populations. All of the materials were prepared by hot-pressing; four of these boron carbides contained different sizes and concentrations of carbonaceous inclusions, while one contained no carbonaceous inclusions. The heterogeneity distributions were characterized in some detail for statistical analysis using scanning electron microscopy and quantitative image analysis. A modified compression Kolsky bar setup with in situ ultra-high-speed microscopic imaging (10 million frames per second) was then used to study the influence of the inclusion distributions on the dynamic failure processes in these materials, at nominal high strain rates of 10 2 -10 3 s -1 . The in situ ultra-high-speed microscopy highlighted the link between micro and macroscale failure processes and demonstrated that the carbonaceous inclusions are indeed the preferential sites for nucleation of wing cracks, as previously hypothesized based on post-mortem observations. The relative orientation of an inclusion with respect to the compression axis was shown to affect the likelihood that it would participate in crack nucleation. In conclusion, all of the ceramics were also found to have orientation-dependent peak compressive stress, regardless of the presence of carbonaceous inclusions, suggesting that grain orientation distributions are also important.

36 MATERIALS SCIENCE↗

New Materials and an Efficient Processing Approach for Materials for Harsh Environments – Continuous Electric Field Assisted Sintering

Electric-field assisted sintering (EFAS) is an advanced manufacturing method for the consolidation and processing of ceramic and metal materials. It is a particularly excellent candidate for efficient materials processing as it has greater than 90% energy cost savings and improved CO2 emissions compared to traditional sintering in a furnace. This is due to direct rapid heating of the materials and molds leveraging an electrification phenomenon called Joule heating where electrical current is passed through the sample/mold assemblies causing direct heating. The technique does have limitations though as it is traditionally a batch-process and suffers from scale up difficulties. To overcome this, researchers at Idaho National Laboratory changed the form factor of traditional EFAS instruments to develop and construct a continuous rolling electric-field assisted sintering (CEFAS) device. Its unique design creates highly localized electrical, thermal, and mechanical process parameters for continuous samples of limitless length. Advanced core shell powder materials were also created using fluidized powder bed atomic layer deposition of core/shell solid oxide electrochemical electrode/electrolyte BaCe0.7Zr0.1Y0.1Yb0.1O3 (BCZYYb) and yttrium doped BaZrO3 (BZY) to be a feedstock for the new CEFAS instrument. The innovative core/shell powder is hypothesized to have high protonic conductivity with enhanced environmental resistance. The completed project covers innovations in process control and design enabled by control theory, finite element modeling and mechanical design, three dimensionally printed carbon-carbon composite manufacturing and utilization, and green materials processing techniques.

36 MATERIALS SCIENCE↗

Additive manufacturing of mullite ceramic by digital light processing

Mullite material was successfully additively manufactured using digital light processing (DLP). The printed geometry involves a one-step process of pyrolysis, de-binding, and sintering under a plain atmosphere to achieve an average of 76 % ceramic yield and linear shrinkage of 12 %. Furthermore, the thermal profile was carefully controlled to obtain consistent phases in which the XRD shows a mullite phase. Here, in addition, the Weibull analysis was conducted on the sintered flexural specimens, showing a Weibull modulus (m) of 13.05 with a characteristic strength (σ 0 ) of 94.96 MPa. Synchrotron microtomography was performed on the sintered specimens, which showed two distinct porosity distributions (small and large). Large porosity (non-spherical elongated) is the primary cause of decreased material strength, while small porosity (spherical) is the sintering product. The measured thermal conductivity of the specimens was in the range of 2.7–3.1 W/m∙k and decreased with an increase in temperature. Lastly, large-scale prototypes were printed concurrently with a fine resolution of 25 μm without any compromise on the predetermined design and structure.

Additive manufacturing↗

In Situ Microstructure Characterization of Potassium Di-Phosphate (KDP) Densification during Cold Sintering

In order for ceramic additive manufacturing (AM) to achieve its full potential, it is increasingly important to develop a more rigorous understanding of fundamental phenomena that govern the kinetics and thermodynamics of ceramic AM processes. In the case of additive build processes, such as direct ink write and ceramic extrusion, methods for densifying the resulting green-body product need to be considered to complement the efficiencies of ceramics AM, itself. One densification route, at least for monolithic components, built layer-by-layer, is offered by the recently developed cold sintering process, whereby high-density final product is achieved through addition of a small amount of liquid solvent and application of modest uniaxial compressive stress at relatively low temperature. In situ small-angle X-ray scattering methods and X-ray diffraction have been applied to characterize and quantify the pore morphology evolution during cold sintering for a model system: potassium di-phosphate, KH 2 PO 4 (KDP). It is shown that both temperature and applied stress affect the densification rate, but stress has a stronger effect on the evolving morphology. A regime with an approximate linear densification rate can be identified, yielding an effective densification activation energy of ≈90 kJ/mol.

36 MATERIALS SCIENCE↗

Improving protonic ceramic electrochemical cell performance via a dual-phase reaction-sintered bilayer electrolyte

Protonic ceramic electrochemical cells (PCCs) are promising energy conversion devices, but their fabrication remains challenging. In particular, the typical electrolytes for PCCs such as BaCe 0.7 Zr 0.1 Y 0.1 Yb 0.1 O 3−δ (7111) and BaCe 0.4 Zr 0.4 Y 0.1 Yb 0.1 O 3−δ (4411) suffer from intrinsic barium evaporation issues during high-temperature sintering. This tendency towards barium loss, combined with their highly refractory nature, leads to a tradeoff between sinterability and chemical stability. To address this tradeoff, we propose a bilayer electrolyte combining layers of 4411 and 7111 materials that is designed to enhance sinterability and conductivity through dual-phase reactive sintering. Our findings demonstrate that the bilayer structure exhibits shrinkage behavior closely matched to that of the fuel electrode substrate, with a higher shrinkage compared to a single-layer 4411 electrolyte. Utilizing this bilayer electrolyte structure, our PCCs achieve a peak power density of 637 mW∙cm −2 in fuel-cell mode and a current density of 1060 mA∙cm −2 at 1.3 V in electrolysis mode at 600 °C. Our PCCs demonstrate high Faradaic efficiency of 83% at 1.3 V and 500 °C. Hybrid distribution of relaxation times (DRT) polarization mapping further reveals that the bilayer structure reduces Ohmic and polarization resistance in both fuel-cell and electrolysis modes.

ceramic processing↗

Processing and 3D printing of SiCN polymer-derived ceramics

Preceramic polymer resins are attractive for the 3D printing of net-shaped ceramic components. Recently various processes have been demonstrated for 3D printing of polymer-derived ceramics (PDCs). Ultimately in these processes, the process outcomes strongly depend on the process parameters. In particular, for PDCs the ceramic density, and ceramic yield are affected by the catalyst concentration and cross-linking duration. Here, we use thermal analysis and FTIR to quantify the interrelation of the process parameters on the process outcome for polysilazanes and demonstrate 3D printing of PDC components based on the best-identified process parameters. Furthermore, the results of this work can be used as guidelines for future additive manufacturing of PDCs.

36 MATERIALS SCIENCE↗

An Industrial Membrane System Suitable for Distributed Used Oil Re-refining

Under this SBIR project, Media and Process Technology Inc (MPT) has achieved ~60% cost reduction and system foot print of its ceramic membrane product, which leads to successful commercialization of its industrial ceramic membrane process to large scale applications. Ceramic membrane is known for its rugged materials and performance reliability; however, it has been limited in niche applications due to its cost and footprint. The low-cost ceramic membrane thus developed under this project has been field tested successfully in our semi-works production facility for used oil re-refining. Our membrane subsystem of our re-refining production capacity was tripled through the installation of this low-cost high packing density of ceramic membranes. In addition, we have successfully field tested/demonstrated with a pilot unit in two large scale applications for refinery FCC slurry upgrading and decoker/amine scrubber wastewater treatment. Commercialization of these two applications in oil refineries are currently actively pursued by our commercialization partner. With regard to the membrane product sales, we have produced >500 m 2 ceramic membranes for two full-scale installations for industrial oil/water separations in 2017, which is equivalent to ~50% of the annual US ceramic membrane market size. We will continue to push our low-cost high packing density ceramic membrane developed from this project for large scale applications, which are not currently occupied by existing ceramic membranes.

02 PETROLEUM↗

New composite separator pellet to increase power density and reduce size of thermal batteries

We show that it is possible to manufacture strong macroporous ceramic films that can be backfilled with electrolyte to form rigid separator pellets suitable for use in thermal batteries. Several new ceramic manufacturing processes are developed to produce sintered magnesium oxide foams with connected porosities of over 80% by volume and with sufficient strength to withstand the battery manufacturing steps. The effects of processing parameters are quantified, and methods to imbibe electrolyte into the ceramic scaffold demonstrated. Preliminary single cell battery testing show that some of our first generation pellets exhibit longer voltage life with comparable resistance at the critical early times to that exhibited by a traditional pressed pellets. Although more development work is needed to optimize the processes to create these rigid separator pellets, the results indicate the potential of such ceramic separator pellets to be equal, if not superior to, current pressed pellets. Furthermore, they could be a replacement for critical material that is no longer available, as well as improving battery separator strength, decreasing production costs, and leading to shorter battery stacks for long-life batteries.

25 ENERGY STORAGE↗

Characterization of Ceramic Material Produced From a Cold Crucible Induction Melter Test

This report summarizes the results from characterization of samples from a melt processed surrogate ceramic waste form. Completed in October of 2014, the first scaled proof of principle cold crucible induction melter (CCIM) test was conducted to process a Fe-hollandite-rich titanate ceramic for treatment of high level nuclear waste. X-ray diffraction, electron microscopy, inductively coupled plasma-atomic emission spectroscopy (and inductively coupled plasma-mass spectroscopy for Cs), and product consistency tests were used to characterize the CCIM material produced. Core samples at various radial locations from the center of the CCIM were taken. These samples were also sectioned and analyzed vertically. Together, the various samples were intended to provide an indication of the homogeneity throughout the CCIM with respect to phase assemblage, chemical composition, and chemical durability. Characterization analyses confirmed that a crystalline ceramic with desirable phase assemblage was produced from a melt using a CCIM. Hollandite and zirconolite were identified in addition to possible highly-substituted pyrochlore and perovskite. Minor phases rich in Fe, Al, or Cs were also identified. Remarkably only minor differences were observed vertically or radially in the CCIM material with respect to chemical composition, phase assemblage, and durability. This recent CCIM test and the resulting characterization in conjunction with demonstrated compositional improvements support continuation of CCIM testing with an improved feed composition and improved melter system.

36 MATERIALS SCIENCE↗