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DOE OSTI2020

Primary Radiation Damage Formation in Solids

The processes that give rise to changes in the microstructure and the physical and mechanical properties of solid metals and ceramics exposed to energetic particles are initiated by essentially elastic collisions between atoms in what has been called an atomic displacement cascade. These processes are similar in metals and ceramics, with some differences related to the ionic and covalent bonding in ceramics compared to metallic bonding. The formation and evolution of primary radiation damage mechanisms are described to provide an overview of how stable defects are formed by displacement cascades, as well as the nature and morphology of the defects themselves. The impact of the primary variables cascade energy and irradiation temperature are discussed, along with a range of secondary factors that can influence damage formation.

Zarkadoula, Eva↗

DOE OSTI2016

Combined Pressure, Temperature Contrast and Surface-Enhanced Separation of Carbon Dioxide for Post-Combustion Carbon Capture

The Rice University research team developed a hybrid carbon dioxide (CO 2 ) absorption process combining absorber and stripper columns using a high surface area ceramic foam gas-liquid contactor for enhanced mass transfer and utilizing waste heat for regeneration. This integrated absorber/desorber arrangement will reduce space requirements, an important factor for retrofitting existing coal-fired power plants with CO 2 capture technology. Described in this report, we performed an initial analysis to estimate the technical and economic feasibility of the process. A one-dimensional (1D) CO 2 absorption column was fabricated to measure the hydrodynamic and mass transfer characteristics of the ceramic foam. A bench-scale prototype was constructed to implement the complete CO 2 separation process and tested to study various aspects of fluid flow in the process. A model was developed to simulate the two-dimensional (2D) fluid flow and optimize the CO 2 capture process. Test results were used to develop a final technoeconomic analysis and identify the most appropriate absorbent as well as optimum operating conditions to minimize capital and operating costs. Finally, a technoeconomic study was performed to assess the feasibility of integrating the process into a 600 megawatt electric (MWe) coal-fired power plant. With process optimization, $82/MWh of COE can be achieved using our integrated absorber/desorber CO 2 capture technology, which is very close to DOE's target that no more than a 35% increase in COE with CCS. An environmental, health, and safety (EH&S) assessment of the capture process indicated no significant concern in terms of EH&S effects or legislative compliance.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2005

Glass and Glass-Ceramic Materials from Simulated Composition of Lunar and Martian Soils: Selected Properties and Potential Applications

In-situ resource processing and utilization on planetary bodies is an important and integral part of NASA's space exploration program. Within this scope and context, our general effort is primarily aimed at developing glass and glass-ceramic type materials using lunar and martian soils, and exploring various applications of these materials for planetary surface operations. Our preliminary work to date have demonstrated that glasses can be successfully prepared from melts of the simulated composition of both lunar and martian soils, and the melts have a viscosity-temperature window appropriate for drawing continuous glass fibers. The glasses are shown to have the potential for immobilizing certain types of nuclear wastes without deteriorating their chemical durability and thermal stability. This has a direct impact on successfully and economically disposing nuclear waste generated from a nuclear power plant on a planetary surface. In addition, these materials display characteristics that can be manipulated using appropriate processing protocols to develop glassy or glass-ceramic magnets. Also discussed in this presentation are other potential applications along with a few selected thermal, chemical, and structural properties as evaluated up to this time for these materials.

Ray, C. S.↗

NASA NTRS2010

Methods for producing silicon carbide architectural preforms

Methods are disclosed for producing architectural preforms and high-temperature composite structures containing high-strength ceramic fibers with reduced preforming stresses within each fiber, with an in-situ grown coating on each fiber surface, with reduced boron within the bulk of each fiber, and with improved tensile creep and rupture resistance properties for each fiber. The methods include the steps of preparing an original sample of a preform formed from a pre-selected high-strength silicon carbide ceramic fiber type, placing the original sample in a processing furnace under a pre-selected preforming stress state and thermally treating the sample in the processing furnace at a pre-selected processing temperature and hold time in a processing gas having a pre-selected composition, pressure, and flow rate. For the high-temperature composite structures, the method includes additional steps of depositing a thin interphase coating on the surface of each fiber and forming a ceramic or carbon-based matrix within the sample.

DiCarlo, James A.↗

NASA NTRS2014

Methods for Producing High-Performance Silicon Carbide Fibers, Architectural Preforms, and High-Temperature Composite Structures

Methods are disclosed for producing architectural preforms and high-temperature composite structures containing high-strength ceramic fibers with reduced preforming stresses within each fiber, with an in-situ grown coating on each fiber surface, with reduced boron within the bulk of each fiber, and with improved tensile creep and rupture resistance properties tier each fiber. The methods include the steps of preparing an original sample of a preform formed from a pre-selected high-strength silicon carbide ceramic fiber type, placing the original sample in a processing furnace under a pre-selected preforming stress state and thermally treating the sample in the processing furnace at a pre-selected processing temperature and hold time in a processing gas having a pre-selected composition, pressure, and flow rate. For the high-temperature composite structures, the method includes additional steps of depositing a thin interphase coating on the surface of each fiber and forming a ceramic or carbon-based matrix within the sample.

DiCarlo, James A.↗

NASA NTRS1985

Ceramics for advanced O2/H2 application

Ceramics are prime candidate materials for advanced rocket engines because they possess high-temperature capability, a tolerance for aggressive environments, and low density. A program was conducted to assess the applicability of structural ceramics to advanced versions of the Space Shuttle main engine (SSME). Operating conditions of ceramic turbine components were defined and each component in the hot-gas path was assessed in regard to materials selection, manufacturing process and feasibility, and relative structural reliability. The conclusion is that ceramic components would be viable in advanced SSME turbopumps.

Carpenter, H. W.↗

NASA NTRS2010

High Temperature Damping Behavior of Plasma-Sprayed Thermal Barrier and Protective Coatings

A high temperature damping test apparatus has been developed using a high heat flux CO 2 laser rig in conjunction with a TIRA S540 25 kHz Shaker and Polytec OFV 5000 Vibrometer system. The test rig has been successfully used to determine the damping performance of metallic and ceramic protective coating systems at high temperature for turbine engine applications. The initial work has been primarily focused on the microstructure and processing effects on the coating temperature-dependence damping behavior. Advanced ceramic coatings, including multicomponent tetragonal and cubic phase thermal barrier coatings, along with composite bond coats, have also been investigated. The coating high temperature damping mechanisms will also be discussed.

Zhu, Dongming↗

DOE OSTI2013

Development of scintillation materials for medical imaging and other applications

Scintillation materials that produce pulses of visible light in response to the absorption of energetic photons, neutrons, and charged particles, are widely used in various applications that require the detection of radiation. The discovery and development of new scintillators has accelerated in recent years, due in large part to their importance in medical imaging as well as in security and high energy physics applications. Better understanding of fundamental scintillation mechanisms as well as the roles played by defects and impurities have aided the development of new high performance scintillators for both gamma-ray and neutron detection. Although single crystals continue to dominate gamma-ray based imaging techniques, composite materials and transparent optical ceramics potentially offer advantages in terms of both synthesis processes and scintillation performance. A number of promising scintillator candidates have been identified during the last few years, and several are currently being actively developed for commercial production. Purification and control of raw materials and cost effective crystal growth processes can present significant challenges to the development of practical new scintillation materials.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Additive manufacturing of silicon carbide for nuclear applications

Additive manufacturing (AM) is a rapidly evolving technology being considered for nuclear applications. A special focus on AM to fabricate nuclear-grade silicon carbide (SiC) is explored in this paper. First, we present currently available AM processing options for SiC. AM methods commonly used for other ceramics, in which the feedstocks are forms of polymers, powders, and/or reactive chemical vapors, are also applicable to SiC. SiC phases are formed by pyrolysis of pre-ceramic polymer, direct reaction of powder precursors, sintering of SiC powders, or chemical vapor deposition/infiltration. Second, we discuss how the different microstructures of SiC materials fabricated by various processing methods affect their behavior in nuclear environments. Third, we discuss state-of-the-art AM technologies for the fabrication of relatively pure SiC, which show great potential to retain its strength under neutron irradiation: (1) binder jet printing followed by chemical vapor infiltration, (2) laser chemical vapor deposition, and (3) selective laser sintering of SiC powders.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Characterization by X-ray tomography of granulated alumina powder during in situ die compaction

Compaction process, the aim of which being to obtain green bodies with low porosity and small size, is often used before sintering treatment. Prior to die filling, the ceramic powder is generally granulated to improve flowability. However during compaction, density heterogeneity and critical size defects may appear due to intergranule and granule-die wall frictions. In this work, the influence of granule formulation on the compact morphology has been studied. To do so, a compaction setup was installed inside an X-ray tomography equipment so that the evolution of the compact morphology could be analysed during the whole compaction process. We have demonstrated that high humidity rate and the addition of binder in the granule formulation increase density heterogeneity and generate larger defects. - Highlights: • An original compaction set up was installed inside an X-Ray tomography equipment. • The compaction process of granulated ceramic powder is imaged. • The compact green microstructure is quantified and related to the compaction stages. • The most detrimental defects of dry-pressed parts are caused by hollow granules. • Formulations without binder allow a reduction of the number of large defects.

36 MATERIALS SCIENCE↗

NASA NTRS2006

Covering a Crucible with Metal Containing Channels

In a procedure that partly resembles the lost-wax casting process, a crucible made of a brittle material (ceramic, quartz, or glass) is covered with a layer of metal containing channels. The metal cover and the channels can serve any or all of several purposes, depending upon the application: Typically, the metal would serve at least partly to reinforce the crucible. The channels could be used as passages for narrow objects that could include thermocouples and heat-transfer strips. Alternatively or in addition, channels could be used as flow paths for liquid or gaseous coolants and could be positioned and oriented for position- or direction-selective cooling. In some cases, the channels could be filled with known gases and sealed so that failure of the crucibles could be indicated by instruments that detect the gases. The process consists of three main steps. In the first step, a pattern defining the channels is formed by wrapping or depositing a material in the desired channel pattern on the outer surface of the crucible. The pattern material can be a plastic, wax, low-ash fibrous material, a soluble material, or other suitable material that can subsequently be removed easily. In a proof-of-concept demonstration (see figure), the crucible was an alumina cylinder and the mold material was plastic tie-down tape. In the second step, the patterned crucible is coated with metal. In one variation of the second step, a very thin layer containing or consisting of an electrically conductive material (e.g., gold, silver, or carbon) is painted or otherwise deposited on the mold-covered crucible, then the covering metal required for the specific application is electrodeposited on the very thin conducting layer. In another variation of the second step, the metal coat is formed by chemical vapor deposition. In the proof-of-concept demonstration, a layer of nickel 0.003 in. ( 0.08 mm) thick was electrodeposited. In the third step, the patterned material is removed. This is generally done by heating the crucible assembly until the patterned material melts and runs out, vaporizes, and/or decomposes to an ash, leaving the channels. Alternatively, if the patterned material is soluble, it can be removed by use of a suitable solvent. In the proof-of-concept demonstration, the tape was burned away by heating the assembly to a temperature of 600 C.

Grugel, Richard N.↗

NASA NTRS2001

Evaluation of Data Retention Characteristics for Ferroelectric Random Access Memories (FRAMs)

Data retention and fatigue characteristics of 64 Kb lead zirconate titanate (PZT)-based Ferroelectric Random Access Memories (FRAMs) microcircuits manufactured by Ramtron were examined over temperature range from -85 C to +310 C for ceramic packaged parts and from -85 C to +175 C for plastic parts, during retention periods up to several thousand hours. Intrinsic failures, which were caused by a thermal degradation of the ferroelectric cells, occurred in ceramic parts after tens or hundreds hours of aging at temperatures above 200 C. The activation energy of the retention test failures was 1.05 eV and the extrapolated mean-time-to-failure (MTTF) at room temperature was estimated to be more than 280 years. Multiple write-read cycling (up to 3x10(exp 7)) during the fatigue testing of plastic and ceramic parts did not result in any parametric or functional failures. However, operational currents linearly decreased with the logarithm of number of cycles thus indicating fatigue process in PZT films. Plastic parts, that had more recent date code as compared to ceramic parts, appeared to be using die with improved process technology and showed significantly smaller changes in operational currents and data access times.

Sharma, Ashok K.↗

DOE OSTI2017

Influence of sintering conditions on the microstructure and optical properties of Eu: CaF{sub 2} transparent ceramic

Highlights: • Eu: CaF2 ceramics sintering at different conditions were fabricated by HP method. • The results show that the temperatures have great effect on the microstructure. • The ceramic sintered at 600 °C/30 MPa has high transmittance and pore-free structure. • The diffusion and densification process mainly occurs between 350 °C and 500 °C. • The optical losses in ceramic were caused by structure defects and polishing damage. - Abstract: Nanopowders of the 5 at.% Eu doped CaF{sub 2} have been synthesized by co-precipitated method. X-ray diffraction (XRD) indicated that the samples corresponds to the cubic CaF{sub 2} phase and scanning electron microscopy (SEM) showed that the morphology of nanopowders were approximately spherical. The Eu: CaF{sub 2} transparent ceramics were fabricated by hot-pressing (HP) method at different P-T conditions in a vacuum environment. The fracture surface, the relative density, average grain size and shrinkage displacements were also studied to analysis the influence of sintering conditions on Eu: CaF{sub 2} ceramic. In comparison with other samples, the proper sintering temperature and pressure was 600 °C/30 MPa. The transmittance of ceramic was up to 79.7% and 88.85% at the wavelength of 760 nm and 2400 nm. Furthermore, the emission spectra of Eu: CaF{sub 2} transparent ceramics under 393.5 nm excitation was also discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Discrete Element Model for Simulations of Early-Life Thermal Fracturing Behaviors in Ceramic Nuclear Fuel Pellets

A discrete element Model (DEM) representation of coupled solid mechanics/fracturing and heat conduction processes has been developed and applied to explicitly simulate the random initiations and subsequent propagations of interacting thermal cracks in a ceramic nuclear fuel pellet during initial rise to power and during power cycles. The DEM model clearly predicts realistic early-life crack patterns including both radial cracks and circumferential cracks. Simulation results clearly demonstrate the formation of radial cracks during the initial power rise, and formation of circumferential cracks as the power is ramped down. In these simulations, additional early-life power cycles do not lead to the formation of new thermal cracks. They do, however clearly indicate changes in the apertures of thermal cracks during later power cycles due to thermal expansion and shrinkage. The number of radial cracks increases with increasing power, which is consistent with the experimental observations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

Effect of (Sr{sub 0.7}Ca{sub 0.3})TiO{sub 3}-substitution on structure, dielectric, ferroelectric, and magnetic properties of BiFeO{sub 3} ceramics

Bi{sub 1−x}(Sr{sub 0.7}Ca{sub 0.3}){sub x}Fe{sub 1−x}Ti{sub x}O{sub 3} ceramics were prepared by a standard solid state reaction process, and the influence of Sr/Ca ratio on structure and properties for Bi{sub 1−x}(Sr,Ca){sub x}Fe{sub 1−x}Ti{sub x}O{sub 3} system was discussed by comparing with Sr{sub 0.5}Ca{sub 0.5}TiO{sub 3}-modified BiFeO{sub 3} ceramics. Rietveld analysis of X-ray diffraction data revealed that the crystal structure changed from rhombohedral R3c (x ≤ 0.4) to orthorhombic Pnma (x = 0.6) with Sr{sub 0.7}Ca{sub 0.3}TiO{sub 3} substitution, and biphasic structure (R3c + Pnma) was determined at x = 0.5, while that for Bi{sub 1−x}(Sr{sub 0.5}Ca{sub 0.5}){sub x}Fe{sub 1−x}Ti{sub x}O{sub 3} system was at x = 0.4. This indicated that the morphotropic phase boundary in Bi{sub 1−x}(Sr,Ca){sub x}Fe{sub 1−x}Ti{sub x}O{sub 3} system shifted toward (Sr,Ca)TiO{sub 3} side with increasing Sr/Ca ratio. The Raman spectrometric analysis and selected area electron diffraction analysis also confirmed this transition. The dielectric relaxation could be well fitted by Arrhenius law, and the different activation energies were attributed to the different origins of the dielectric relaxations with increasing temperature. The current density-field (J-E) curves indicated that the leakage current was reduced to about five orders of magnitude with Sr{sub 0.7}Ca{sub 0.3}TiO{sub 3} substitution. The P-E hysteresis loops obtained by three different methods indicated the enhanced ferroelectricity at x = 0.4, and it could be attributed to the decrement of leakage current. Meanwhile, the magnetization was enhanced with Sr{sub 0.7}Ca{sub 0.3}TiO{sub 3} substitution, and the maximum remanent magnetization was determined at x = 0.2. The enhanced magnetization originated from the partial substitution of Fe{sup 3+} by Ti{sup 4+}.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2018

Fourier amplitude sensitivity test applied to dynamic combined finite-discrete element methods-based simulations

Fracture propagation plays a key role for a number of applications of interest to the scientific community, from dynamic fracture processes like spallation and fragmentation in metals to failure of ceramics, airplane wings, etc. Simulations of material deformation and fracture propagation rely on accurate knowledge of material characteristics such as material strength and the amount of energy being dissipated during the fracture process. Within the combined finite-discrete element method (FDEM) framework material fracture behavior is typically described through a parametrized softening curve, which defines a stress-strain relationship unique to each material. We apply the Fourier amplitude sensitivity test to explore how each of these parameters influences the simulated damage processes and to determine the key input parameters that have the most impact on the model response. We present several sensitivity numerical experiments for the simulation of a split Hopkinson pressure bar (SHPB) test for weathered granite samples using different combinations of model parameters. We validate the obtained results against SHPB experimental data. The experiments show that the model is mostly sensitive to parameters related to tensile and shear strengths, even in the presence of other parameter perturbations. Lastly, the results suggest that the specification of tensile and shear strengths at the interfaces dominate the stress-time history of the FDEM simulation of SHPB test.

36 MATERIALS SCIENCE↗

NASA NTRS2004

Advanced SiC/SiC Ceramic Composites For Gas-Turbine Engine Components

NASA Glenn Research Center (GRC) is developing a variety of advanced SiC/SiC ceramic composite (ASC) systems that allow these materials to operate for hundreds of hours under stress in air at temperatures approaching 2700 F. These SiC/SiC composite systems are lightweight (approximately 30% metal density) and, in comparison to monolithic ceramics and carbon fiber-reinforced ceramic composites, are able to reliably retain their structural properties for long times under aggressive gas-turbine engine environments. The key for the ASC systems is related first to the NASA development of the Sylramic-iBN Sic fiber, which displays higher thermal stability than any other SiC- based ceramic fibers and possesses an in-situ grown BN surface layer for higher environmental durability. This fiber is simply derived from Sylramic Sic fiber type that is currently produced at ATK COI Ceramics (COIC). Further capability is then derived by using chemical vapor infiltration (CVI) and/or polymer infiltration and pyrolysis (PIP) to form a Sic-based matrix with high creep and rupture resistance as well as high thermal conductivity. The objectives of this study were (1) to optimize the constituents and processing parameters for a Sylramic-iBN fiber reinforced ceramic composite system in which the Sic-based matrix is formed at COIC almost entirely by PIP (full PIP approach), (2) to evaluate the properties of this system in comparison to other 2700 F Sylramic-iBN systems in which the matrix is formed by full CVI and CVI + PIP, and (3) to examine the pros and cons of the full PIP approach for fabricating hot-section engine components. A key goal is the development of a composite system with low porosity, thereby providing high modulus, high matrix cracking strength, high interlaminar strength, and high thermal conductivity, a major property requirement for engine components that will experience high thermal gradients during service. Other key composite property goals are demonstration at high temperatures of high environmental resistance and high creep resistance, which in turn will result in long component life. Data are presented from a variety of laboratory tests on simple two-dimensional panels that examine these properties and compare the performance of the optimized full PIP system with those of the full CVI and CVI + PIP hybrid systems. Underlying mechanisms for performance differences in the various systems are discussed. Remaining issues for further property enhancement and for application of the full PIP approach for engine components are also discussed, as well as on-going approaches at NASA to solve these issues.

H. M. Yun↗

DOE OSTI2018

High thermal stability and excellent dielectric properties of a novel X8R-type CdCu3Ti4O12 ceramics through a sol-gel technique

Highlights: • CdCu{sub 3}Ti{sub 4}O{sub 12} (CdCTO) ceramics were successfully synthesized via the sol-gel method, and the optimized processing parameters were obtained. • The outstanding dielectric properties: ε{sub r} ≈ 1.63 × 10{sup 4} and tan δ = 0.035 (at 10 kHz) could be obtained in CdCTO ceramics sintered at 1000 °C. • The CdCTO-SG ceramics obtained an excellent thermal stability. - Abstract: CdCu{sub 3}Ti{sub 4}O{sub 12} (CdCTO) ceramics were systematically synthesized via the sol-gel technique. The optimal CH{sub 3}COOH and Ti(OC{sub 4}H{sub 9}){sub 4} concentrations in the synthesis solution and processing temperature were found to be 5.0 vol%, 0.50 mol/L and 60 °C, respectively. These materials exhibited high densities and fine-grained microstructures along with outstanding dielectric properties, including an ε{sub r} of approximately 1.63 × 10{sup 4} and a tan δ of 0.035 at 10 kHz. Over the temperature range from −55 to 150 °C, the temperature coefficients of the dielectric constant at 1 and 10 kHz were −13.9% to 1.20% and −9.10% to 3.92%, respectively, indicating that these ceramics possess excellent thermal stability. These properties also meet the requirements for X8R applications. Data acquired from complex impedance spectroscopy and electrical modulus assessments demonstrates that the superior dielectric properties of these CdCTO ceramics can be attributed to the internal barrier layer capacitor theory (IBLC).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗