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DOE OSTI2023

Pre-ceramic polymer-assisted nucleation and growth of copper sulfide nanoplates

Abstract Polymer-derived ceramics derived from pre-ceramic polymers (PCPs), have access to several form factors and are highly tunable systems. Tunability can be further expanded with the incorporation of functional nanoparticle fillers throughout the matrix for advanced nanocomposite polymer-derived ceramic development. However, capping ligands used in nanoparticle syntheses mix unfavorably with PCPs, giving aggregated filler material and diminished properties. To control dispersion, secondary nanoparticle processing is performed by adhering PCP-miscible caps to the surface after synthesis. This often sacrifices size control established for small nanoparticles (<10 nm). Herein, we successfully eliminate the need for extra nanoparticle processing through the development of a one-pot, copper sulfide synthesis in which a PCP assists the stable formation of nanoparticles and serves as the final graft molecule. We monitor the success of this methodology and the PCP’s role in the reaction through several characterization methods probing both the nanoparticle core and polymer graft.

Loughney, Patricia A. (ORCID:0000000199472267)↗

DOE OSTI2020

Boosted piezoelectricity with excellent thermal stability in tetragonal NaNbO 3 -based ceramics

The realization of high piezoelectric performance and excellent temperature stability simultaneously in Pb-free ceramics is the key for replacing Pb-containing perovskites in the industry. In this study, large piezoelectric performance (d 33 = 354 pC N –1 ) was achieved in a wide temperature sinterable potassium-free NaNbO 3 –BaTiO 3 –BaSnO 3 system, which is twice more than the piezoelectricity found in NaNbO 3 –BaTiO 3 binary ceramics. Structural refinement of high-energy synchrotron powder diffraction data suggests a single tetragonal structure with P4bm symmetry for the studied NaNbO 3 -based Pb-free ceramic. The results indicate that the small axial ratio favoring polarization reorientation benefits strong piezoelectricity, while the large oxygen octahedron tilt enhances the stability of the P4bm structure during the changing temperature according to the in situ high-energy synchrotron X-ray diffraction measurements and provides the foundation for the excellent thermal stability (20–100 °C) of the piezoelectric properties. Furthermore, a single tetragonal phase with a tiny axial ratio and large oxygen octahedron tilt effectively balances the piezoelectricity and thermal stability in Pb-free systems.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Superior plastic flow stability of self-patterned carbide – amorphous ceramic nanostructures

Amorphous ceramics and carbides exhibit superb strength but poor plasticity. Here, we synthesized TiC-SiOC nanostructures with TiC-nanocarbides embedded in amorphous ceramic SiOC by co-sputtering followed by high-temperature annealing and/or irradiation. TiC-SiOC nanostructures exhibit high strength and good plastic flow stability even after heavy irradiation, 7 GPa at room temperature and 3.6 GPa at 700 ℃ with a uniform strain of about 10%∼18%. The uniform deformation is accommodated by the shearing of amorphous ceramic and the rotation of nanocarbides. Nanocarbides inhibit the propagation of shear banding in amorphous SiOC, and amorphous-crystal interfaces act as sinks to manage irradiation-induced defects.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Breakdown in ceramic window

A capacitive type coaxial ceramic window is designed for the SC linac. The coaxial power coupler has inner conductor diameter 34.8 mm and outer conductor diameter 80 mm. An alumina disk of diameter 150 mm and thickness 3.6 mm is used as ceramic. The diameter of the inner conductor of the coupler near the ceramic is increased to 39.2 mm to match the impedance at 1050 MHz. A copper prototype of the window is fabricated and characterized. A performance of the window is often degraded because of the multipacting. A CST particle studio is used to simulate the multipacting trajectories. The particle trajectories are observed at different locations and different power levels up to 1 MW. The results are dependent on the initial position of the primary electron and power level. A few soft multipacting barriers are observed at the operating power level. (author)

43 PARTICLE ACCELERATORS↗

DOE OSTI2015

Evaluation of a Fluorochlorozirconate Glass-Ceramic Storage Phosphor Plate for Gamma-Ray Computed Radiography

In this paper, a fluorochlorozirconate (FCZ) glass-ceramic containing orthorhombic barium chloride crystals doped with divalent europium was evaluated for use as a storage phosphor in gamma-ray imaging. X-ray diffraction and phosphorimetry of the glass-ceramic sample showed the presence of a significant amount of orthorhombic barium chloride crystals in the glass matrix. Transmission electron microscopy and scanning electron microscopy were used to identify crystal size, structure, and morphology. The size of the orthorhombic barium chloride crystals in the FCZ glass matrix was very large, ~0.5–0.7 μm, which can limit image resolution. The FCZ glass-ceramic sample was exposed to 1 MeV gamma rays to determine its photostimulated emission characteristics at high energies, which were found to be suitable for imaging applications. Test images were made at 2 MeV energies using gap and step wedge phantoms. Gaps as small as 101.6 μm in a 440 stainless steel phantom were imaged using the sample imaging plate. Analysis of an image created using a depleted uranium step wedge phantom showed that emission is proportional to incident energy at the sample and the estimated absorbed dose. Finally, the results showed that the sample imaging plate has potential for gamma-ray-computed radiography and dosimetry applications.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Simultaneous three-dimensional elemental mapping of Hollandite and Pyrochlore material phases in ceramic waste form materials

In this study, differential X-ray absorption contrast tomography was performed on model ceramic composite systems to image the 3D spatial distributions of Ga and Nd containing phases. The model material systems were fabricated such that they contained two constituent phases. Ga–doped Ba hollandite (Ba 1.33 Ga 2.66 Ti 5.34 O 16 ), and pyrochlore (Nd 2 Ti 2 O 7 ) which are under consideration as nuclear waste immobilization matrices. Two complementary techniques have been used to characterize the 3D distribution of phases. The analysis suggests that the 3D spatial distributions of hollandite and pyrochlore can be readily identified through the distributions Ga and Nd, respectively. These results represent a critical development towards characterizing the complex microstructure inherent to practical materials such as multiphase ceramic composite waste forms. Furthermore, these methods can be applied to elucidate microstructural features that fundamentally determine the performance and properties of complex systems, which is central to the design of durable waste forms as well as many other real materials such fuel cells, batteries, ultra-high temperature ceramics.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Synthesis and electrical properties of BaBiO 3 and high resistivity BaTiO 3 –BaBiO 3 ceramics

Ceramics of the composition BaBiO3 (BB) were sintered in oxygen to obtain a single phase with monoclinic II2/mm symmetry as suggested by high-resolution X-ray diffraction. X-ray photoelectron spectroscopy confirmed the presence of bismuth in two valence states - 3+ and 5+. Optical spectroscopy showed presence of a direct bandgap at ~ 2.2eV and a possible indirect bandgap at ~ 0.9eV. This combined with determination of the activation energy for conduction of 0.25eV, as obtained from ac impedance spectroscopy, suggested that a polaron-mediated conduction mechanism was prevalent in BB. The BB ceramics were crushed, mixed with BaTiO3 (BT), and sintered to obtain BT–BB solid solutions. All the ceramics had tetragonal symmetry and exhibited a normal ferroelectric-like dielectric response. Using ac impedance and optical spectroscopy, it was shown that resistivity values of BT–BB were orders of magnitude higher than BT or BB alone, indicating a change in the fundamental defect equilibrium conditions. A shift in the site occupancy of Bi to the A-site is proposed to be the mechanism for the increased electrical resistivity.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effects of Plasticizer Content and Ceramic Addition on Electrochemical Properties of Cross-Linked Polymer Electrolyte

The development of a safe electrolyte is the key to improving energy density for next generation lithium batteries. In this work, UV-crosslinked poly(ethylene oxide) (PEO) -based polymer and composite electrolytes are systematically investigated on their ionic conductivity, mechanical and electrochemical properties. The polymer electrolytes are plasticized with non-flammable linear short-chain PEO. In the composite electrolytes, a doped lithium aluminum titanium phosphate (LATP) ceramic, LICGC™, is used as the ceramic filler. It is found that the addition of the plasticizer leads to a tradeoff between ion transport and mechanical properties. In contrast, the addition of ceramic fillers improves both the ionic conductivity and mechanical properties. The sample with 20 wt% of LICGC™ shows a conductivity of ~0.6 mS cm –1 at 50 °C. This sample also demonstrates much longer cycle life than the neat polymer electrolyte in Li platting/stripping test with a capacity of 1 mAh cm –2 . Further, a full cell made with this composite electrolyte against Li metal anode and high voltage LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode shows 94% capacity retention after 30 cycles, compared to 58% capacity retention with the neat polymer electrolyte. These results demonstrate that a hybrid of polymer/ceramic/non-flammable plasticizer is a promising path to high energy density, high voltage lithium batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

High Performance SrFe 0.2 Co 0.4 Mo 0.4 O 3–δ Ceramic Anode Supported Low-Temperature SOFCs

The development of alternative ceramic anodes for low-temperature solid oxide fuel cells (LT-SOFCs) is essential to overcome the inherent challenges such as redox instability and coking associated with Ni-based cermet anodes. Moreover, due to the large electrolyte ohmic loss at low temperature, it is critical to developing an electrode supported cell that allows electrolyte thickness reduction. Here we successfully demonstrated a high performance SrFe 0.2 Co 0.4 Mo 0.4 O 3–δ (SFCM) ceramic anode supported LT-SOFC with a peak power density of 730 mW cm –2 and 300 mW cm –2 at ambitious low temperatures of 550 °C and 450 °C, respectively, in humidified H 2 . The new anode material SFCM exhibits exceptional conductivity of over 30 S cm –1 at 450 °C in humidified H 2 , providing essential current collection capability as an anode backbone appropriate for the infiltration of Ni-gadolinia doped ceria (GDC) electrocatalysts. Compared to conventional Ni-cermet anodes, the nano-sized Ni-GDC particles in our SFCM based electrode significantly improves the cell stability in hydrocarbon gases. We demonstrated a stable long-term operation over a period of 380 h in CH 4 –containing gas mixtures at 450 °C with a voltage degradation rate of 4% per 1000 h at a constant current of 0.2 A*cm –2 . Furthermore, our results demonstrate a high performance ceramic anode with high stability for low temperature operation.

25 ENERGY STORAGE↗

DOE OSTI2023

Understanding Chemo-Mechanical Stability of Protonic Ceramic Cells Through Electronic Conduction in the BaCe 0.7 Zr 0.1 Y 0.1 Yb 0.1 O 3-δ Electrolyte

BaCe 0.7 Zr 0.1 Y 0.1 Yb 0.1 O 3-δ (BCZYYb) is a promising ceramic electrolyte for reversible protonic ceramic cells. It is reported that BCZYYb-based cells show excellent long-term durability, particularly in the electrolysis mode, in contrast to the cells based on the conventional electrolyte yttria-stabilized zirconia. In this study, we investigate the chemo-mechanical stability behavior (a low tendency of delamination) of the BCZYYb-based protonic ceramic cells in terms of local electronic conduction in the electrolyte. The local electronic conductivity of the BCZYYb electrolyte is determined using Pt-probe-embedded cells near each electrode interface. The BCZYYb electrolyte exhibits sufficient p-type conductivity (∼10 −3 S cm −1 ) near the oxygen electrode (corresponding p O 2 : 5.27–21 × 10 −2 atm) and n-type conductivity (∼10 −4 S cm −1 ) near the hydrogen electrode (corresponding p O 2 : 0.99–1.30 × 10 −24 atm) at 600 °C. A standard cell is prepared and tested over long-term in the fuel cell (at positive and negative voltages) and electrolysis modes. The cell exhibits stable performance without delamination or cracks in both operating modes, owing to local electronic conduction.

Electrochemistry↗

DOE OSTI2026

All-ceramic channel waveguides fabricated via 3D printing

All-ceramic channel waveguides (CWGs) in Yb:YAG transparent ceramics have been fabricated for the first time, to the best of our knowledge, via direct ink write (DIW) and their laser performance has been demonstrated. Single filaments of Yb:YAG nanoparticle-loaded ink were extruded into undoped YAG; the Yb:YAG filaments formed the CWGs, surrounded by undoped cladding. Elemental mapping confirmed the Yb doping profile and waveguide integrity. Optical characterization showed low cladding scatter losses (<1.3%/cm at 1.3 µm), and laser testing with a 940 nm Ti:sapphire pump demonstrated efficient lasing at 1030 nm. The best-performing waveguide, with an elliptical cross-section (100 µm × 60 µm and a length of 1.4 cm), achieved a slope efficiency of 61% and a roundtrip loss of 12.4%. These results identify DIW as a promising approach for fabricating high-performance channel waveguides in transparent ceramics.

36 MATERIALS SCIENCE↗

DOE OSTI2015

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↗

DOE OSTI2017

Development of a Repeatable Protocol to Uniformly Coat Internal Complex Geometries of Fine Featured 3D Printed Objects with Ceramic Material, including Determination of Viscosity Limits to Properly Coat Certain Pore Sizes

HEPA filters are commonly used in air filtration systems ranging in application from simple home systems to the more advanced networks used in research and development. Currently, these filters are most often composed of glass fibers with diameter on the order of one micron with polymer binders. These fibers, as well as the polymers used, are known to be fragile and can degrade or become extremely brittle with heat, severely limiting their use in high temperature applications. Ceramics are one promising alternative and can enhance the filtration capabilities compared to the current technology. Because ceramic materials are more thermally resistant and chemically stable, there is great interest in developing a repeatable protocol to uniformly coat fine featured polymer objects with ceramic material for use as a filter. The purpose of this experiment is to determine viscosity limits that are able to properly coat certain pore sizes in 3D printed objects, and additionally to characterize the coatings themselves. Latex paint was used as a surrogate because it is specifically designed to produce uniform coatings.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Development of Agile and Cost Effective Routes for Manufacturing Reliable Ceramic Components for SOFC Systems (Final Report)

Additive manufacturing routes were explored and developed to enable the low to medium volume manufacturing of ceramic components with a short lead time, flexibility for iterative design, and without the high CAPEX and tooling costs associated with green machining or injection molding. Agile manufacturing route of gelcasting and 3D printing were selected and work focused on the production of ceramic manifold components utilized in the balance of plant for Saint-Gobain’s all-ceramic SOFC stack. This work showed that both gelcasting and a specific version of 3D printing were able to create parts with the proper fidelity and at lower cost than traditional powder processing followed by green machining.

03 NATURAL GAS↗

DOE OSTI2019

Development of Agile and Cost Effective Routes for Manufacturing Reliable Ceramic Components for SOFC Systems (Final Scientific Report Updated)

36 MATERIALS SCIENCE↗

DOE OSTI2021

Cold Sintered Ceramics and Cements for Part Encapsulation

In this project, ceramic encapsulation materials were studied for high temperature (>~°500 C) applications where typical polymer encapsulants are unstable. A new low temperature (<~°200 C) method of processing ceramics, the cold sintering process was examined. Additionally, commercially available high temperature ceramic cements were investigated. In both cases, the mechanical strengths of available materials are less than desired (i.e., desired strengths similar to Si 3 N 4 ), limiting applicability. Composite designs to increase mechanical strength are suggested. Additionally, non-uniformities in stresses and densification while embedding alumina sheets in encapsulants via cold sintering using uni-axial pressing led to fracture of sheets, and an alternative iso-static based approach is recommended for future studies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Development of a Kollidon 90F-PEG300-Glycerin Binder for PZT 95/5 Ceramic Processing

This SAND Report documents the development of organic binder system for PZT 95/5 consisting of Kollidon 90F, PEG300, and glycerin. Binders are a critical component in the manufacture of ceramic components. Low performing binders can result in poor yield and lower performance of ceramic components. This study sought to develop a well performing binder system for PZT 95/5 ceramics to support Ferroelectric Neutron Generator manufacturing. The study explored the glass transition temperature, powder compaction properties, green strengths, and thermal decomposition over a wide composition range. An optimal composition was found consisting of 1.3 wt.% Kollidon 90F, 0.5 wt.% PEG300, and 0.2 wt.% glycerin, and incorporating humidity conditioning . The results showed that the optimized binder exhibited improved compaction performance and enhanced green strength compared to a baseline binder and at lower loading. Further, sintered PZT 95/5 parts prepared using the optimized binder exhibited ~5% improved polarization performance without alteration to the microstructure.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Advanced Fuel Cycle Cost Basis Report: Module D1-1: Uranium-based Ceramic LWR Fuel Fabrication (Rev.2)

Cost module on LWR fuel fabrication to accompany the Advanced Fuel Cycle Cost Basis Report. In this update, we are adding detailed life cycle cost data and a calculated, levelized fabrication cost derived from a non-proprietary bottom-up estimate prepared in 1978 by Oak Ridge National Laboratory (ORNL) (Judkins and Olsen 1978a). In 2018, the 1978 ORNL estimate was escalated by SA&I authors to 2017 USD using factors that represent inflation, escalation above inflation typical of nuclear projects, and the effects of more stringent safety and environmental regulations. In this FY-21 document, the $/kgU results in 2017 USD from the unpublished 2018 interim study (Williams and Ganda 2018) can be escalated to 2020 USD using a factor of 1.052. The literature-based unit cost (or price) data from previous (2004–2017) AFC-CBRs are escalated to 2020 USD using factors from Chapter 8 of the main FY-21 AFC-CBR document. This data, in addition to the results of the updated bottom-up estimate, are used to define the “what-it-takes” (WIT) range for the unit fabrication costs for conventional ceramic UOX light-water reactor (LWR) fuel. This FY-23 document also includes calculated unit costs for accident-tolerant LWR fuels (ATFs) of three different types. Some of these fuels constitute a ceramic pelletized form with fuel meat uranium compounds other than UO2 (a.k.a.,. UOX), thus the change in the title of this module in which the word “UO2” is changed to “Uranium-based Ceramic.”

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗