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DOE OSTI2018

Microwave sintering of complex shapes: From multiphysics simulation to improvements of process scalability

The microwave sintering homogeneity of large and complex shape specimens is analyzed. A new approach enabling the fabrication of complex shapes ceramics via 3D printing and microwave sintering is presented. The use of a dental microwave cavity is shown to enable a substantial level of densification of complex shape components while restricting the grain growth. The homogeneity of the processed samples during microwave sintering is studied by an electromagnetic-thermal-mechanical simulation. The realistic densification behavior, that phenomenologically takes into account the microwave effect, is included in the modeling framework. We observe that the simulation indicates the sharp correlation between the microwave field distribution in the cavity, the temperature profile, and the specimen's shape distortion.

36 MATERIALS SCIENCE↗

DOE OSTI2019

A three-dimensional interconnected polymer/ceramic composite as a thin film solid electrolyte

In this work we introduce an approach to fabricate a solid composite electrolyte film that is thin, ionically conductive, and mechanically robust with good potential for manufacturability, in the application of lithium metal batteries. First a doped-lithium aluminum titanium phosphate ceramic thin film with thickness of ~25 μm is formed by aqueous spray coating, a scalable process. The film is partially sintered to form a three-dimensionally interconnected structure with a dense backbone. It is then backfilled with a crosslinkable poly(ethylene oxide) (PEO)-based polymer electrolyte. We report the composite has very high ceramic loading of 77 wt% (61 vol%) and an ionic conductivity of 3.5 × 10 -5 S/cm at 20 °C with an activation energy of 0.43 eV. The main ion transport pathway is through the ceramic network, predicted by modelling and verified by experiments. Owing to the interconnected structure of the ceramic, the composite electrolyte exhibits much improved mechanical strength.

25 ENERGY STORAGE↗

DOE OSTI2018

Numerical Modeling of Fiber-Reinforced Metal Matrix Composite Processing by the Liquid Route: Literature Contribution

One of the technologies used to produce metal matrix composites (MMCs) is liquid route processing. One solution is to inject a liquid metal under pressure or at constant rate through a fibrous preform. This foundry technique overcomes the problem of the wettability of ceramic fibers by liquid metal. The liquid route can also be used to produce semiproducts by coating a filament with a molten metal. These processes involve physical phenomena combined with mass and heat transfer and phase change. The phase change phenomena related to solidification and also to the melting of the metal during the process notably result in modifications to the permeability of porous media, in gaps in impregnation, in the appearance of defects (porosities), and in segregation in the final product. In this article, we provide a state-of-the-art review of numerical models and simulation developed to study these physical phenomena involved in MMC processing by the liquid route.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Mechanism of photochromic effect in Pb(Zr,Ti)O{sub 3} and (Pb,La)(Zr,Ti)O{sub 3} ceramics under violet/infrared light illumination

Obvious photochromic effects were observed in Pb(Zr,Ti)O{sub 3} and (Pb,La)(Zr,Ti)O{sub 3} (PLZT) ceramics, along with exponential responses to illumination power in both darkening and bleaching processes. An interesting anomalous dispersion in the transparent PLZT was observed and discussed. A tentative physical picture based on photoinduced electron stimulated processes and on structural change was proposed to explain all the interesting observations. Rate equations were established and solved in verifying the validity of the proposed model. This work may serve as guidance in designing tunable achromatic lenses, UV and IR light detectors and sensors.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Development of New Magnetron Sputter Deposition Processes for Laser Target Fabrication

Magnetron sputter deposition is an enabling technology for laser target fabrication. Solutions are readily available for the deposition of most sub-micron-thick elemental films on planar substrates. However, major challenges still remain for the development of robust deposition processes in regimes of ultrathick (over ~10 μm) coatings and nonplanar substrates. These challenging deposition regimes are directly relevant to laser target applications, including both sphero-cylindrical hohlraums and spherical ablators for inertial confinement fusion (ICF) targets. Understanding underlying physical mechanisms for a specific material system is crucial for process development, given the overall complexity of the deposition process, its nonlinear dependence on deposition parameters, and a very large process space, often precluding conventional process optimization approaches. Here, we describe our approach to developing new deposition processes and give practical advice with examples of new results from our ongoing studies of glassy boron carbide ceramics for next-generation ICF ablators and nonequilibrium gold-tantalum alloys for hohlraums for magnetized ICF schemes. Emphasis is given to two major challenges of ultrathick coatings related to achieving process stability and reducing residual stress.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Research on the interfacial structure and property improvement of the Cfiber/2Si-B-3C-N ceramic matrix composite

Highlights: • The C{sub fiber}/2Si-B-3C-N composite with nice properties was successfully prepared. • ZrO{sub 2} promotes the densification process, homogeneous nucleation and grain growth. • The interface reaction in the composite was well controlled by the addition of ZrO{sub 2}. • The damage to carbon fiber was largely avoided by the addition of ZrO{sub 2}. - Abstract: A mixture of the mechanically alloyed 2Si-B-3C-N powder and short carbon fiber was hot pressed at 1800 °C for 30 mins in nitrogen. Careful investigation to the prepared C{sub fiber}/2Si-B-3C-N ceramic matrix composite revealed that the composite was very difficult to be densified. Heterogeneous nucleation, abnormal grain growth and severe interface reaction occurred on the fiber surface or between the fiber and the ceramic matrix, leading to a small density and weak mechanical properties of the composite. For the prepared composite without any additive, the relative density, flexural strength, elastic modulus and fracture toughness is 71.7%, 64.6 MPa, 14.7 GPa and 1.47 MPa·m{sup 1/2}, respectively. The average size of the SiC grains close to and far away from the carbon fiber is 249.10 nm and 50.45 nm, respectively. However, with the addition of ZrO{sub 2} (7.5 mol%), the above mentioned phenomenons are changed noticeably, and those properties are significantly increased to 88.5%, 112.4 MPa, 111.1 GPa and 2.94 MPa·m{sup 1/2}, respectively. At the same time, the SiC grains close to or far away from the carbon fiber almost have the same average size of about 448.21 nm, and almost no interface reaction occurs. It shows that the addition of ZrO{sub 2} not only facilitates the sintering and densification process, but also depresses the interface reaction, promotes the homogeneous nucleation and grain growth, and hence significantly improves the mechanical properties of the C{sub fiber}/2Si-B-3C-N composite. This interesting finding is favorable for the preparation of carbon fiber reinforced ceramic matrix composite, which requires both a large relative density and well controlled interface reaction.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Sealing glass-ceramics with near-linear thermal strain, part III: Stress modeling of strain and strain rate matched glass-ceramic to metal seals

Thermal mechanical stresses of glass-ceramic to stainless steel (GCtSS) seals are analyzed using finite element modeling over a temperature cycle from a set temperature (T set ) 500°C to -55°C, and then back to 600°C. There are two glass-ceramics that have an identical coefficient of thermal expansion (CTE) at ~16 ppm/°C but have very different linearity of thermal strains, designated as near-linear NL16 and step-like SL16, and were formed from the same parent glass using different crystallization processes. Stress modeling reveals much higher plastic strain in the stainless steel using SL16 glass-ceramic when the GCtSS seal cools from T set . Upon heating tensile stresses start to develop at the GC-SS interface before the temperature reaches T set . On the other hand, the much lower plastic deformation in stainless steel accumulated during cooling using NL16 glass-ceramic allows for radially compressive stress at the GC-SS interface to remain present when the seal is heated back to T set . Finally, the qualitative stress comparison suggests that with a better match of thermal strain rate to that of stainless steel, the NL16 glass-ceramic not only improves the hermeticity of the GCtSS seals, but would also improve the reliability of the seals exposed to high-temperature and/or high-pressure abnormal environments.

36 MATERIALS SCIENCE↗

DOE OSTI2022

In Situ Nanoscale Dynamics Imaging in a Proton‐Conducting Solid Oxide for Protonic Ceramic Fuel Cells

Abstract Hydrogen fuel cells and electrolyzers operating below 600 °C, ideally below 400 °C, are essential components in the clean energy transition. Yttrium‐doped barium zirconate BaZr 0.8 Y 0.2 O 3‐d (BZY) has attracted a lot of attention as a proton‐conducting solid oxide for electrochemical devices due to its high chemical stability and proton conductivity in the desired temperature range. Grain interfaces and topological defects modulate bulk proton conductivity and hydration, especially at low temperatures. Therefore, understanding the nanoscale crystal structure dynamics in situ is crucial to achieving high proton transport, material stability, and extending the operating range of proton‐conducting solid oxides. Here, Bragg coherent X‐ray diffractive imaging is applied to investigate in situ and in 3D nanoscale dynamics in BZY during hydration over 40 h at 200 °C, in the low‐temperature range. An unexpected activity of topological defects and subsequent cracking is found on a nanoscale covered by the macroscale stability. The rearrangements in structure correlate with emergent regions of different lattice constants, suggesting heterogeneous hydration. The results highlight the extent and impact of nanoscale processes in proton‐conducting solid oxides, informing future development of low‐temperature protonic ceramic electrochemical cells.

25 ENERGY STORAGE↗

DOE OSTI2016

The Consolidation of Glass-Ceramic Waste forms by Hot Isostatic Pressing: Sample Optimisation - 16581

Zirconolite based glass-ceramics were developed for the disposition of plutonium residues at the UK's Sellafield site. Glass-ceramics act as double barrier systems, separating Pu into a durable ceramic phase and retaining miscellaneous material in the amorphous phase. Here we discuss the optimisation of processing parameters and formulations of these alternative waste-forms. All samples were HIPed at 1250 deg. C, 100 MPa for 4 hrs. By investigating the effects of different pre-HIP heat treatments on sample quality and throughput, and glass phase compositions on the crystalline phase assemblage, an optimised method and wasteform composition were achieved. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2013

Effects of lanthanum dopants on the Curie–Weiss and the local order behaviors for Pb{sub 1−x}La{sub x}(Fe{sub 2/3}W{sub 1/3}){sub 0.7}Ti{sub 0.3}O{sub 3} relaxor ferroelectrics

Graphical abstract: The local order as a function of temperature by using (a) the spin-glass model and (b) the modified-Landau theory for Pb{sub 1−x}La{sub x}(Fe{sub 2/3}W{sub 1/3}){sub 0.7}Ti{sub 0.3}O{sub 3} ceramics with different amounts of lanthanum dopants. Display Omitted Highlights: ► The effects of La are investigated for Pb{sub 1−x}La{sub x}(Fe{sub 2/3}W{sub 1/3}){sub 0.7}Ti{sub 0.3}O{sub 3} ceramics. ► La can change their dielectric properties and ordering state. ► The spin glassy behaviors and the freezing process are also affected by La. ► The response mechanisms of La are proposed for the local polarization behavior. -- Abstract: The effects of lanthanum dopants are investigated on the dielectric responses for Pb{sub 1−x}La{sub x}(Fe{sub 2/3}W{sub 1/3}){sub 0.7}Ti{sub 0.3}O{sub 3} ceramics. According to the experimental data and fitting results, it is concluded that the dielectric characteristics are changed from a long-range-ordered (LRO) ferroelectric state to a short-range-ordered (SRO) relaxor by increasing the amounts of lanthanum dopants. Furthermore, the spin glassy behaviors and the freezing process of local polarizations are not only affected by the ordering degree of B-site cations but also affected by the defect polar pairs. Their response mechanisms are proposed that the growth of the 1:1 ordered domain Pb{sub 1−x}La{sub x}(Fe{sub 1/2}W{sub 1/2})O{sub 3} is impeded since its charge imbalance is enhanced by increasing the amounts of lanthanum dopants, and the defect polar pairs of lead, tungsten and oxygen vacancy are induced by the pyrochlore phase, PbWO{sub 4} or Pb{sub 0.99}La{sub 0.01}WO{sub 4}, when the amount of lanthanum dopants exceed 5 mol.%.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Al 2 O 3 /TiO 2 coated separators: Roll-to-roll processing and implications for improved battery safety and performance

Heat generation is one of the major concerns with lithium-ion batteries (LIB) while charging them at higher currents, which could inadvertently impact the rate performance and reduce the safety of the cell. Polymer separator is one of the least thermal conductive components of a LIB. In addition, commercial separators for LIB are made from polyolefin membranes that tend to shrink and curl at higher temperatures due to their lower melting temperature (~130 °C). Developing separators with improved thermal stability and higher electrolyte uptake is essential for enhancing the safety as well as the performance of the LIB. In this work, a thin layer of ceramic coatings (Al 2 O 3 and TiO 2 ) is applied on propylene (PP) membrane to improve the thermal stability and electrolyte affinity without compromising the rate performance. A slurry with 100% Al 2 O 3 coated on the polypropylene separator exhibited the best improvement in thermal stability ( shrinkage of 0.6% vs 6.0% for uncoated membrane) and excellent rate performance with 92% capacity retention at 2C. The Al 2 O 3 coated separator demonstrated excellent electrolyte wettability compared to the uncoated membrane. The cross-plane thermal conductivity of the ceramic coated separators is analyzed to understand their heat transfer behavior. The thermal conductivity of the separator is improved by ~3.2 times with the Al 2 O 3 coating.

25 ENERGY STORAGE↗

DOE OSTI2018

Quantitative In Situ Studies of Dynamic Fracture in Brittle Solids Using Dynamic X-ray Phase Contrast Imaging

Here, we demonstrate the use of X-ray phase contrast imaging with sub-microsecond temporal resolution to obtain quantitative visualization of dynamic fracture processes in brittle solids. We examine an amorphous solid (fused silica), a ceramic single crystal (single-crystal quartz), and a polycrystalline ceramic (boron carbide), in the form of single-edge notched specimens loaded using a three-point apparatus at nominal strain rates up to ~800 s -1 . We observe that the crack tip speed for boron carbide is relatively independent of mode I stress intensity factor rate ($\dot{K}$ I ) for these rates of loading, while that of fused silica and single-crystal quartz increases with $\dot{K}$ I . Further, for the amorphous and single crystal cases, we observe the development of a crack tip instability in the form of crack branching as the crack tip speed approaches 45% of the Rayleigh wave speed. This suggests that strain-rate-dependent mechanisms contribute to crack branching. Such mechanisms may, in turn, affect the macroscopic fracture properties of these materials.

36 MATERIALS SCIENCE↗

DOE OSTI2019

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↗

DOE OSTI2018

Laser Induced Breakdown Spectroscopy analysis of europium and samarium in aluminum oxide

The use of Laser Induced Breakdown Spectroscopy as a technique for analysis of europium and samarium concentrations in ceramic aluminum oxide samples was investigated for application to studying lanthanide separation processes. Metal oxide powders of europium and/or samarium were mixed with aluminum oxide at varying concentrations and pressed into pellets. A comparison of different approaches to building a univariate simple linear regression analysis curve is presented. A linear behavior was seen over the total lanthanide concentration range from 0.086 to 12.358 weight percent (wt%). In conclusion, the calculated limits of detection for the univariate calibration curves were determined to range from 0.001 to 0.108 wt% and 0.001 and 0.183 wt% for europium and samarium, respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Experimental and Theoretical Thermokinetic Analysis of the Na 3 VO 4 –CO 2 Reaction System under Different Physicochemical Conditions

Sodium vanadate (Na 3 VO 4 ) was synthesized, structural and microstructurally characterized as well as tested as possible carbon dioxide (CO 2 ) captor through thermodynamic calculations in addition to thermogravimetric dynamic and isothermal analyses. Ceramic structural characterization evidenced the formation of the Na 3 VO 4 crystal phase, while microstructural features evidenced dense agglomerates with a poor specific surface area, although synthesis temperature (600 °C) was not as high as that for other sodium ceramics. Na 3 VO 4 was investigated for the CO 2 capture process through dynamic and isothermal experiments, in the presence or absence of oxygen. All these experiments showed that Na 3 VO 4 possesses interesting CO 2 capture properties in a specific temperature range (520 and 600 °C). Isothermal products characterization allowed to elucidate the reaction pathway, implying the Na 4 V 2 O 7 formation, as possible reactive intermediate. In fact, reaction path evolution was supported with theoretical thermodynamic data. Moreover, the kinetic analysis, performed using the Avrami-Erofeev mathematical model and subsequent thermodynamic data obtention, probed the positive influence of the temperature, in both CO 2 superficial and bulk chemical sorption processes, while oxygen addition did not enhance the superficial process. Additionally, as it would be expected, kinetics were enhanced as a function of the CO 2 concentration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Magnetic and dielectric properties of Aurivillius phase Bi{sub 6}Fe{sub 2}Ti{sub 3−2x}Nb{sub x}Co{sub x}O{sub 18} (0 ≤ x ≤ 0.4)

We investigate the structural, magnetic, and dielectric properties of Bi{sub 6}Fe{sub 2}Ti{sub 3−2x}Nb{sub x}Co{sub x}O{sub 18} (0 ≤ x ≤ 0.4). The room-temperature ferromagnetism is observed in the Nb and Co co-doped samples compared with the paramagnetic behavior in Bi{sub 6}Fe{sub 2}Ti{sub 3}O{sub 18}. The ferromagnetism in Bi{sub 6}Fe{sub 2}Ti{sub 3−2x}Nb{sub x}Co{sub x}O{sub 18} can be understood in terms of spin canting of the antiferromagnetic coupling of the Fe-based and Co-based sublattices via Dzyaloshinsky-Moriya interaction. Moreover, doping Co at Ti sites can significantly enhance the ferromagnetic Curie temperature compared with the substitution of Co for Fe in the Aurivillius compounds. The dielectric loss of Bi{sub 6}Fe{sub 2}Ti{sub 3−2x}Nb{sub x}Co{sub x}O{sub 18} (0.1 ≤ x ≤ 0.4) exhibits a relaxation process. The rather large activation energy in the 0.1 ≤ x ≤ 0.3 samples implies that the relaxation process is not due to the thermal motion of oxygen vacancies inside ceramics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Metal–ceramic composite structures for fabrication of high power density plasmonic devices

The recent decade brought many advances to plasmonics, but high power density plasmonic antennas designed to behave as heaters or operate in high temperature environments are still facing material stability challenges preventing their ultimate use. Gold has been the optimal choice among plasmonic materials but experiences morphology changes at temperature that result in device efficiency reduction and failure. Bulk titanium nitride has been explored as a solution but has deal-breaking tradeoffs in device quality factor. In this paper, we explore via proof-of-concept the use of a metal–ceramic composite structure to determine whether a bulk Au nanorod can provide strong plasmonic resonances while coated with an ultrathin conformal layer of titanium nitride or silica to provide morphological stability and sufficient plasmonic activity without excessive resonance quality degradation. We show SEM-level morphological stability for temperatures up to 500 °C with coatings below 4 nm. Computer modeling suggests the ultrathin titanium nitride has detrimental effects on the strong plasmonic resonances of a Au nanorod. Here, we then looked into other possible coatings for solutions to stabilize high power density plasmonic antennas including plasmonic oxides, metal adhesion layers, and silica, the latter appearing to be the best option while lowering the overall peak electric field intensity, the silica increases the electric field intensity at its boundary.

36 MATERIALS SCIENCE↗

DOE OSTI2021

The Impact of Sintering Atmosphere and Temperature on the Phase Evolution of High Surface Area LSCF Prepared by In Situ Carbon Templating

The thermochemical stability of lanthanum strontium cobalt ferrite (LSCF) processed between 1000 °C–1200 °C via the in situ carbon templating method was studied. This method generates high surface area ceramics at traditional solid oxide fuel cell (SOFC) sintering temperatures by generating a carbon template in situ and subsequently removing the template by oxidation at 700 °C. Argon processed samples produced an amorphous carbon template, whereas nitrogen tended to form graphitic carbon. Prior to the oxidation step, nitrogen samples comprised larger La 2 O 3 crystallites (22–40 nm) compared to argon (9–17 nm). Upon oxidation, argon samples resulted in a pure LSCF phase with surface areas in the 21–29 m 2 ·g −1 range, whereas nitrogen samples contained significant impurities. This demonstrates that the size of La 2 O 3 crystallites formed during inert processing limited the ability to produce a pure LSCF phase. Symmetrical cells comprising nano-LSCF electrodes generated by the templating method were compared to cells sintered directly in air. Impedance results suggest that nano-LSCF cells and cells processed in air were dominated by interfacial charge transfer resistance and gas diffusion, respectively. The results map out conditions for preparing and integrating high surface area, nanostructured LSCF into SOFC electrodes at traditional sintering temperatures. Strategies for improving the interfacial resistance of nano-LSCF electrodes are discussed.

Muhoza, Sixbert P. (ORCID:0000000299864241)↗