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At least 55 records · Page 3

INL CRMO XRF Special Report No. 3: INL CRMO XRF Calibration Methods for the Analysis of Ceramics and Brick

This report details the analytical methods used by the Idaho National Laboratory Cultural Resource Management Office to characterize ceramic and brick artifacts using X-ray fluorescence spectrometry. More specifically, this report provides details on instrumentation, analysis times, and matrix-specific calibration protocols for ceramic materials. Calibration curves were developed to adjust raw instrumental output for 13 elements using a suite of reference standards made from historic brick borrowed from the Yale Peabody Museum. Calibration curves were validated by plotting predicted values against published reference values for the calibration set as well as a certified soil reference standard (SRM 2711a).

36 MATERIALS SCIENCE↗

Protecting People and Planet

To produce energy, civilian nuclear power plants require fuel. The majority of existing plants rely on solid ceramic fuels that contain concentrations of about 3 to 5% of the element uranium-235. This specific isotope is well suited to sustaining the type of chain reaction required for a nuclear reactor to harness the heat produced by nuclear fission. Title I of the United States Atomic Energy Act of 1954 defines “special nuclear material” as plutonium, uranium-233, or uranium enriched in the isotopes uranium-233 or uranium-235. This label identifies materials that at high concentrations can be used to produce nuclear weapons. The United States and broader international community are fully committed to ensuring the peaceful use of nuclear energy by committing to practices known as safeguards.

99 GENERAL AND MISCELLANEOUS↗

Method for making metal-carbon composites and compositions

A method for making covetic metal-carbon composites or compositions by electron beam melt heating under vacuum (pressure <10−3 Torr) is described herein. This fabrication method is advantageous, in that it provides oxygen-free covetic materials in a process that allows precise control of the composition of the covetic material to be produced. The method described herein also can be applied to produce multi-element-carbon composites within a metal or alloy matrix, including high melting temperature materials such as ceramic particles or prefabricated nano- or micro-structures, such as carbon nanotubes or graphene compounds. The covetic reaction between metal and carbon takes place under the influence of flowing electrons through the melted metal-carbon precursor. This process creates strong bonding between nanocarbon structure and the metal elements in the melt.

36 MATERIALS SCIENCE↗

Crystal Growth and Elemental Homogeneity of the Multicomponent Rare-Earth Garnet (Lu 1/6 Y 1/6 Ho 1/6 Dy 1/6 Tb 1/6 Gd 1/6 ) 3 Al 5 O 12

We report high-entropy aluminum garnets were grown as bulk single crystals using the micro-pulling-down method, taking the synthesis of complex ceramics a step further from the conventional preparation of polycrystalline materials. We studied the effects of growth parameters on the elemental distribution in high optical quality crystals of (Lu 1/6 Y 1/6 Ho 1/6 Dy 1/6 Tb 1/6 Gd 1/6 ) 3 Al 5 O 12 containing six cations (yttrium and rare-earths) taken in equimolar amounts. A single garnet structure was confirmed by powder X-ray diffraction. Electron microprobe measurements were obtained to correlate the radial distribution of rare-earth elements with pulling rates and molten zone height. The nature of the elemental distribution in the radial direction was associated with ionic radius: smaller rare-earths concentrated in the center of the crystal, while larger rare-earths segregated toward the outer edge of the cylindrical crystal. Faster pulling rates led to a flattening of the concentration profiles toward the nominal concentration, promoting a more homogeneous radial elemental distribution, while varying the molten zone height did not have a significant effect. The demonstrated success with crystal growth enables the practical availability of single crystals of multicomponent aluminum garnets for further discovery of new phenomena and applications.

36 MATERIALS SCIENCE↗

Additively manufactured transparent ceramic thin disk gain medium

A novel type of Yb:YAG transparent ceramic thin disk laser amplifier is demonstrated, based on fabricating a composite gain element with a paraboloidal interface between gain and no-gain regions and employing side-pumping of the thin disk. The pump-induced gain and the impact of amplified spontaneous emission on the achievable inversion are reported.

36 MATERIALS SCIENCE↗

Ball-on-ring test validation for equibiaxial flexural strength testing of engineered ceramics

The validation of a ball-on-ring, equibiaxial flexural strength method to obtain the transverse rupture strength (TRS) of right cylindrical ceramic specimens was performed in this study. Validation of the test method was achieved using commercially available engineered high purity alumina disks and finite element (FE) model analysis. The validated fixture was then used to obtain the TRS and Weibull statistical analysis of MgO-partially stabilized zirconia (MSZ) and Y 2 O 3 -partially stabilized zirconia (YSZ) ceramic disks. TRS data for alumina, MSZ, and YSZ agreed with the TRS values reported in the literature. A statistically relevant number of samples (N > 30) for each material were tested to allow for a Weibull statistical analysis. Weibull parameters for these materials were within the expected values for engineered ceramics. The characteristic strength for alumina, MSZ, and YSZ were determined to be 289, 786, and 814 MPa, respectively. The Weibull modulus was determined between 10 and 25 for each material, which is typical of engineered ceramics. In addition, FE model results were in close agreement with experimental fracture values for the three ceramic materials tested in this study.

36 MATERIALS SCIENCE↗

Precipitation Hardening in Ferroelectric Ceramics

Domain wall motion in ferroics, similar to dislocation motion in metals, can be tuned by well-concepted microstructural elements. In demanding high-power applications of piezoelectric materials, the domain wall motion is considered as a lossy hysteretic mechanism that should be restricted. Current applications for so-called hard piezoelectrics are abundant and hinge on the use of an acceptor-doping scheme. However, this mechanism features severe limitations due to enhanced mobility of oxygen vacancies at moderate temperatures. By analogy with metal technology, the authors present here a new solution for electroceramics, where precipitates are utilized to pin domain walls and improve piezoelectric properties. Through a sequence of sintering, nucleation, and precipitate growth, intragranular precipitates leading to a fine domain structure are developed as shown by transmission electron microscopy, piezoresponse force microscopy, and phase-field simulation. This structure impedes the domain wall motion as elucidated by electromechanical characterization. As a result, the mechanical quality factor is increased by ≈50% and the hysteresis in electrostrain is suppressed considerably. This is even achieved with slightly increased piezoelectric coefficient and electromechanical coupling factor. This novel process can be smoothly implemented in industrial production processes and is accessible to simple laboratory experimentation for microstructure optimization and implementation in various ferroelectric systems.

36 MATERIALS SCIENCE↗

Near-net shaping of high-density, complex, spatially-tailored ceramics for extreme environments

The purpose of this subcontract is for LLNL to collaborate with the Subcontractor (UCSB) in the areas of binder jet additive manufacturing (BJAM), hot pressing (HP), finite element modeling (FEM), and multi-material sintering studies. LLNL wants to further develop its hot pressing, AM, and modeling capabilities through LLNL’s Early Career Faculty Program. This work will focus on developing a method to hot press complex-shaped ceramic parts through the co-deposition of a structural/functional ceramic and sacrificial mold material in one assembly via multi-material binder jet printing. The method aims to produce dense, near-net shaped parts with applications relevant to a wide variety of fields including aerospace, defense, and energy.

36 MATERIALS SCIENCE↗

All-Ceramic Passive Wireless Temperature Sensor Realized by Tin-Doped Indium Oxide (ITO) Electrodes for Harsh Environment Applications

In this work, an all-ceramic passive wireless inductor–capacitor (LC) resonator was presented for stable temperature sensing up to 1200 °C in air. Instead of using conventional metallic electrodes, the LC resonators are modeled and fabricated with thermally stable and highly electroconductive ceramic oxide. The LC resonator was modeled in ANSYS HFSS to operate in a low-frequency region (50 MHz) within 50 × 50 mm geometry using the actual material properties of the circuit elements. The LC resonator was composed of a parallel plate capacitor coupled with a planar inductor deposited on an Al2O3 substrate using screen-printing, and the ceramic pattern was sintered at 1250 °C for 4 h in an ambient atmosphere. The sensitivity (average change in resonant frequency with respect to temperature) from 200–1200 °C was ~170 kHz/°C. The temperature-dependent electrical conductivity of the tin-doped indium oxide (ITO, 10% SnO2 doping) on the quality factor showed an increase of Qf from 36 to 43 between 200 °C and 1200 °C. The proposed ITO electrodes displayed improved sensitivity and quality factor at elevated temperatures, proving them to be an excellent candidate for temperature sensing in harsh environments. The microstructural analysis of the co-sintered LC resonator was performed using a scanning electron microscope (SEM) which showed that there are no cross-sectional and topographical defects after several thermal treatments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Technical and economic feasibility of molten chloride salt thermal energy storage systems

A techno-economic study is performed to assess the feasibility of molten chloride salt thermal energy storage (TES) systems for next generation concentrating solar power. Refractory liners internally insulate tanks to allow tank shells to be constructed from carbon steel. The liner must not be wetted by salt to maintain predictable thermal properties and manageable heat loss out of the tank. The commercial scale tank liner is an anchored brick and mortar design with expansion joints to accommodate thermal expansion. Furthermore, finite element analysis is performed to optimize the thermal and mechanical profile of the tank. Equalizing the shell temperature between the water-cooled foundation and the shell wall is necessary to minimize differential thermomechanical stress and lower overall stress values below industrial allowable limits. The cost of the TES system is estimated to be $60/kWhth, which is four times greater than Department of Energy targets. Solutions to reduce system cost and overall risk are proposed.

14 SOLAR ENERGY↗

Neutron Total Scattering Analysis of Materials for the Nuclear Fuel Cycle

Here, this paper reviews recent experimental efforts at the University of Tennessee and Oak Ridge National Laboratory to comprehensively characterize the structural details of materials relevant for the nuclear fuel cycle by employing advanced neutron scattering techniques. For the study of nuclear ceramics, neutron scattering offers distinct advantages over traditional laboratory or synchrotron X-ray diffraction, including enhanced sensitivity to elements with a low atomic mass, such as oxygen, nitrogen, and carbon. The key to these efforts is the recent advancement in the neutron scattering infrastructure at the high-flux diffractometers at the Spallation Neutron Source. The high neutron flux at these instruments enables neutron total scattering, a nondestructive bulk technique that simultaneously captures both short-range structural effects through pair distribution function analysis and long-range order through diffraction pattern analysis. This approach is particularly important for a comprehensive description of defective, disordered, or amorphous nuclear materials. The case studies presented here include analyses of the local defect structure in hyperstoichiometric uranium oxides and short-range order of ion-irradiated ceramics. This advanced analytical methodology will improve our understanding of the behavior of materials in extreme environments and contribute to the development of more resilient nuclear materials.

Neutron scattering↗

Calibration of a mesoscale tritium transport model for ceramic breeder materials in TMAP8 using experimental data

Due to the scarcity of the long-term external tritium supply, lithium-containing breeder materials are used in the blanket of fusion reactors to produce tritium faster than the deuterium-tritium fusion reaction consumes it. A cellular breeder is a promising material with higher lithium density and thermal conductivity than conventional ceramic pebbles and enhanced tritium extraction with interconnected pores. Although several experimental and modeling efforts have improved our understanding of tritium transport, the exact mechanisms governing tritium release from breeder materials are still unknown. As a result, current models cannot reliably assess the tritium breeding capabilities of cellular breeder materials. This work presents a tritium transport multiphysics model and calibrates it using experimental data of deuterium absorption and desorption from cellular breeder materials at different temperatures and pressures. This model accounts for ceramic and pore diffusion, trapping and detrapping, and several surface reactions at the pore surface. After calibrating the model and performing sensitivity analysis, we discuss pre-dominant mechanisms governing tritium release from cellular breeder materials. The model is part of the Tritium Migration Analysis Program [TMAP8], a multiscale, multiphysics framework for tritium transport based on the finite element multiphysics framework MOOSE. This study demonstrates some of TMAP8’s capabilities and provides insight into the mechanisms governing tritium transport in cellular ceramic breeder materials.

08 HYDROGEN↗

An IIPG-based finite element framework in MOOSE for modeling fiber reinforced composite failure governed by extrinsic cohesive laws

Fiber reinforced composites (FRC) are widely applied to many important engineering structures such as silicon carbide ceramic matrix composite (SiC CMC) of nuclear fuel claddings. Many material and structure failures are initiated at the interface between two distinctive materials, such as the debonding of interfaces of matrix/fiber of composites or bulk matrix/inclusion in metals at micro-scales. Accurate and robust modeling of these interface failures is critical to the development of novel material and structure with improved functionality. This paper presents a discontinuous Galerkin (DG) finite element method based on the Incomplete Interior Penalty scheme and its implementation in MOOSE for modeling material interface behaviors. The proposed method naturally accommodates important extrinsic cohesive zone material models and is capable of modeling the failures of material interfaces across which material properties are highly distinctive. We demonstrate a good performance of the proposed method using single fiber and multiple fiber debonding problems.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Toughening materials: enhancing resistance to fracture

It has been said that ‘God invented plasticity, but the Devil invented fracture!’ Both mechanisms represent the two prime modes of structural failure, respectively, plastic collapse and the rupture/breaking of a component, but the concept of developing materials with enhanced resistance to fracture can be difficult. This is because fracture resistance invariably involves a compromise—between strength and ductility, between strength and toughness—fundamentally leading to a ‘conflict’ between nano-/micro-structural damage and the mechanisms of toughening. Here, we examine the two major classes of such toughening: (i) intrinsic toughening, which occurs ahead of a crack tip and is motivated by plasticity—this is the principal mode of fracture resistance in ductile materials, and (ii) extrinsic toughening, which occurs at, or in the wake of, a crack tip and is associated with crack-tip shielding—this is generally the sole mode of fracture resistance in brittle materials. We briefly examine how these distinct mechanistic processes have been used to toughen synthetic materials—intrinsically in gradient materials and in multiple principal-element metallic alloys with the example of metallic glasses and high-entropy alloys, and extrinsically in ceramics with the example of ceramic-matrix composites—in comparison to Nature which has been especially adept in creating biological/natural materials which are toughened by one or both mechanistic classes, despite often consisting of constituents with meagre mechanical properties. The success of Nature has been driven by its ability to cultivate the development of materials with multiple length-scale hierarchical structures that display ingenious gradients and structural adaptability, a philosophy which we need to emulate and more importantly learn to synthesize to make structural materials of the future with unprecedented combinations of mechanical properties.

36 MATERIALS SCIENCE↗

System and method for optical fiber preform preparation via high-surface-area coating

The present disclosure relates to a method for forming a glass, ceramic or composite material. The method may involve initially forming a plurality of tubes and then performing a coating operation to coat the plurality of tubes with materials containing metal or metalloid elements, including inorganic compounds, organometallic compounds, or coordination complexes to form coated tubes. The method may further include performing at least one of a thermal operation or a thermochemical operation on the coated tubes to form a solid glass, ceramic, or composite structure with dimensions representing at least one of a rod or fiber.

Lange, Andrew↗

Single-component-at-a-time variation study for glass-ceramic waste forms

Here, a 51-sample composition variation study was performed on glass-ceramic waste forms for a raffinate waste stream from aqueous reprocessing of used nuclear fuel containing high fractions of Mo, alkalis, alkaline earths (AEs), and rare earths (REs). The study was designed with a single-component-at-a-time variation approach off a centroid composition. The components that were varied included Al, B, Ca, Li, Mo, Na, REs, Si, Zr, and Others (containing minor components). Data analysis included crystallization curves, microstructure, and phase compositions. A number of components (i.e., Li 2 O, B 2 O 3 , REO x , MoO 3 , Na 2 O, and ZrO 2 ) significantly impacted the concentration and chemistry of phases, especially the primary phases of oxyapatite [i.e., Ca 2 RE 8 (SiO 4 ) 6 O 2 ] and powellite (i.e., AEMoO 4 ), precipitated in the slow-cool heat-treated waste forms; minor phases included cerianite [i.e., Ce x Zr (1-x) O 2 ], Ba-molybdate [i.e., Ba(Gd 0.67 Mo 0.33 O 3 ], noble metals, pollucite (i.e., CsAlSiO 4 ), and RE-borosilicate (i.e., RE 3 BSi 2 O 10 ).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗