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DOE OSTI2025

Investigation of Solid Particle Reactors for Nonoxidative Dehydrogenation of Ethane: Toward Solar Thermal Ethylene Production

Concentrating solar power plants can generate renewable heat at temperatures well above those of most industrial processes. Ceramic particles irradiated with concentrated sunlight can store high-quality sensible heat and transfer this to power generation systems. These concepts and materials hold great potential to also enable thermal processes in the chemical industry, but effective strategies for transferring heat from thermal energy storage media into chemical reactors are still under development. This present work evaluated the thermal and chemical compatibility of various solid particle media (including quartz, bauxite, and alumina particles) integrated directly into tube reactors and the subsequent effects on reactor performance for the nonoxidative dehydrogenation of ethane reaction. Empty tube reactors without loaded particles (representing conventional ethane cracking coils) showed significant heat transfer limitations as the tube diameter was scaled. The incorporation of media into the reactor significantly aided heat transfer to the gaseous ethane reactant and increased its conversion by as much as 10% at similar space velocities. Despite direct contact with hydrocarbon gases, alumina and quartz media showed negligible coke formation. Even during reaction in 100% ethane feed gas at 825 °C, the average selectivity of the coke product was only 0.57% when using the quartz media. These materials further demonstrated excellent thermal stability during subsequent reoxidation in air at 800 °C, which simulated the reheating of particles in a circulating particle solar receiver. Conversely, high rates of coke formation, with a product selectivity of 27.5%, were observed on sintered bauxite particles during the reaction, likely promoted by transition metal constituents. These particles fractured upon reoxidation due to exotherms generated from coke combustion. In conclusion, while the use of cofed steam could mitigate attrition of redox-active particles, the ability of inert metal oxide particles to efficiently transfer heat to concentrated ethane reactant gas while suppressing side reactions or degradation suggests that these media could effectively couple solar thermal plants to reactors for next-generation production of ethylene and other critical chemicals.

Hydrocarbons↗

DOE OSTI2014

Development of ITM Oxygen Technology for Low-cost and Low-emission Gasification and Other Industrial Applications

Air Products is carrying out a scope of work under DOE Award No. DE-FE0012065 “Development of ITM Oxygen Technology for Low-cost and Low-emission Gasification and Other Industrial Applications.” The Statement of Project Objectives (SOPO) includes a Task 4f in which a Decision Point shall be reached, necessitating a review of Tasks 2-5 with an emphasis on Task 4f. This Topical Report constitutes the Decision Point Application pertaining to Task 4f. The SOPO under DOE Award No. DE-FE0012065 is aimed at furthering the development of the Ion Transport Membrane (ITM) Oxygen production process toward a demonstration scale facility known as the Oxygen Development Facility (ODF). It is anticipated that the completion of the current SOPO will advance the technology significantly along a pathway towards enabling the design and construction of the ODF. Development progress on several fronts is critical before an ODF project can commence; this Topical Report serves as an early update on the progress in critical development areas. Progress was made under all tasks, including Materials Development, Ceramic Processing Development, Engineering Development, and Performance Testing. Under Task 4f, Air Products carried out a cost and performance study in which several process design and cost parameters were varied and assessed with a process model and budgetary costing exercise. The results show that the major variables include ceramic module reliability, ITM operating temperature, module production yield, and heat addition strategy. High-temperature compact heat exchangers are shown to contribute significant cost benefits, while directly firing into the feed stream to an ITM are even a mild improvement on the high-temperature recuperation approach. Based on the findings to-date, Air Products recommends no changes to the content or emphasis in the current SOPO and recommends its completion prior to another formal assessment of these factors.

Armstrong, Phillip↗

DOE OSTI2013

High-temperature X-ray analysis of phase evolution in lithium ion conductor Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3}

Series of Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} glass ceramic samples were prepared in this work through the change of heat treatment temperature from 650 to 1050 °C. The structures of glass ceramic samples were characterized by means of high temperature X-ray diffraction and Field Emission Scanning Electron Microscope. And the lithium ionic conductivity was analyzed through AC impedance spectroscopy. Through heat treatment at 850 °C for 4 h for the base glass sample, we obtained a maximum conductivity of 5.8 × 10{sup −4} S/cm at room temperature. - Graphical Abstract: High temperature X-ray diffraction (HT-XRD) and Rietveld refinement of Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} (LAGP) glass-ceramics were recorded to investigate the phase transformation, cell parameters and the mass fraction of each crystal phase, which occur in the glass to glass-ceramics process during different crystallization temperatures. The relationship between the average grain size and conductivity that originate from and relate to the crystallization temperature was analyzed by SEM micrograph and AC impedance spectroscopy. - Highlights: • Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} glass-ceramics were prepared from as-prepared glass. • The phases decomposition and mass fraction of each phase were analyzed by HT-XRD. • Conductivity is relate to grain size that influenced by crystallization temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Preparing Li-garnet electrodes with engineered structures by phase inversion and high shear compaction processes

We report solid-state lithium batteries are promising for safety and energy density com-pared with traditional lithium-ion batteries. However, the large interfacial resistance between the electrode and electrolyte is a bottleneck to achieving high-performance solid-state batteries. Engineered electrode structures with a porous scaffold of the solid electrolyte material are promising to lower the interfacial resistance and provide a mechanical support for a thin solid electrolyte layer. In this work, two ceramic processing techniques are used to fabricate porous/dense bilayer architectures based on a Li 6.25 Al 0.25 La 3 Zr 2 O 12 (LLZO) Li-garnet material. Finger-like vertically aligned pores are created by the phase inversion (PI) process. A water bath presaturated with Li salt prevents Li loss during the PI solvent exchange step. Pore size and porosity can be optimized by adjusting the bath temperature. The high shear compaction process was used to prepare LLZO tapes with 40, 60, and 80 vol% poreformer. The porosity of the tapes after sintering is 39.5%, 58.4%, and 75.4%, respectively. Microtomography exhibits the porosity, pore shape, and pore distribution of the tapes. A typical cathode material LiNi 0.33 Mn 0.33 Co 0.33 O 2 (NMC) is filled into the pores via vacuum infiltration, and a dense cathode layer is formed within the garnet scaffold.

25 ENERGY STORAGE↗

DOE OSTI2013

Dielectric, ferromagnetic and maganetoelectric properties of BaTiO{sub 3}–Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} composite ceramics

Graphical abstract: - Highlights: • The lead-free ME ceramic composites BaTiO{sub 3}–Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} were successfully synthesized. • The composites showed high dielectric constant and low dielectric loss. • The composite with 30% NiZn ferrite presented good soft magnetic properties and ME performance. - Abstract: Lead-free magnetoelectric composite ceramics (1 − x)BaTiO{sub 3}–xNi{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} (x = 0.15, 0.3, 0.45) were successfully prepared by conventional oxide ceramic process. The tetragonal perovskite BaTiO{sub 3} and cubic spinel Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} were confirmed by X-ray diffraction. The dielectric behaviors of all composite samples show a normal response to the increasing measurement frequency and Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} ferrite content. Well defined ferromagnetic hysteresis loops and obvious magnetoelectric coupling effect are observed in the composite ceramics. The influence of applied dc bias magnetic field and Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} ferrite content on the magnetoelectric coupling responding voltage is investigated. The strongest peak magnetoelectric coupling voltage coefficient is 124 μV/cm Oe when x = 0.3, which corresponds to the maximum magnetoelectric coupling responding voltage of 200 μV.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Effects of MnO doping on the electronic properties of zinc oxide: 406 GHz electron paramagnetic resonance spectroscopy and Newman superposition model analysis

MnO-doped ZnO ceramics have been synthesized through the conventional ceramic processing route. Mn{sup 2+} ions have been incorporated into the ZnO lattice within the limits of solid solubility. By using X-band-frequency and high-field electron paramagnetic resonance (EPR), we have resolved some of the main electronic transitions for the S = 5/2, I = 5/2 high-spin system and have determined accurately the EPR spin-Hamiltonian parameters. By combining data from crystallographic X-ray diffraction and EPR with the semi-empirical Newman superposition model, we have found the local configurational position of Mn{sup 2+} and have confirmed the symmetry of the lattice. The results presented in this contribution indicate that Mn ions substitute at Zn sites in ZnO. The effect of Mn{sup 2+} ions on the intrinsic defects becomes remarkable, thus the vacancy related intrinsic defect signals cannot be visible in the EPR spectrum. MnO doping affects the band gap energy of ZnO system which was confirmed via UV-Vis spectroscopy.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2014

Nanostructured gadolinium-doped ceria microsphere synthesis from ion exchange resin: Multi-scale in-situ studies of solid solution formation

In the current nano-sized material revolution, the main limitations to a large-scale deployment of nanomaterials involve health concerns related to nano-dissemination via air. Developing new chemical routes benefiting from nano-size advantages while avoiding their hazards could overcome these limitations. Addressing this need, a chemical route leading to soft nano-particle agglomerates, i.e., macroscopic precursors presenting the ability to be decomposed into nano-sized materials, was developed and applied to Ce{sub 0.8}Gd{sub 0.2}O{sub 2−δ}. Using cerium/gadolinium-loaded ion exchange resin, the Ce{sub 0.8}Gd{sub 0.2}O{sub 2−δ} solid solution formation as a function of temperature was studied in-situ through X-ray diffraction, X-ray absorption spectroscopy and Raman spectroscopy. Temperatures corresponding to the organic skeleton decomposition and to the mixed oxide crystallization were identified. An optimal heat treatment, leading to nanostructured soft agglomerates, was established. Microsphere processing capabilities were evaluated and particle size distribution measurements were recorded. A very low fracture strength was calculated, and a nanometric particle size distribution (170 nm) was determined. - Graphical abstract: The elaboration of micro-spherical precursors leading to the formation of nano-oxide soft agglomerates was studied and approved through the use of ion exchange resin loaded with cerium and gadolinium. The formation of the solid solution was followed through in-situ measurements such as XAS, XRD, Raman, TGA and DSC. Key temperatures were identified for the formation of the mixed-oxide. Following this study, the microstructure and particle size of oxide microspheres formed highlight the formation of soft nano-arrangments. - Highlights: • Soft microspherical agglomerates able to be decomposed into nano-sized materials. • In situ study of cerium/gadolinium-loaded ion exchange resin conversion in oxide. • In situ multi-scale study through Raman spectroscopy, XAS and HT-XRD. • Monodisperse nanometric particle synthesis suitable for ceramic processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

Comparison of structural and magnetic properties of Zn{sub x}Mg{sub 1.5-x}Mn{sub 0.5}FeO{sub 4} and MgAl{sub x}Cr{sub x}Fe{sub 2-2x}O{sub 4} spinel oxides

The spinel oxides Zn{sub x}Mg{sub 1.5-x}Mn{sub 0.5}FeO{sub 4} (x = 0.0 to 0.6) and MgAl{sub x}Cr{sub x}Fe{sub 2-2x}O{sub 4} (x = 0.0 to 0.6) abbreviated as ZMMFO and MACFO respectively, were synthesized by standard ceramic processing. The compositional purity of all the specimens was checked by EDAX technique. The X-ray diffractometry was employed to determine the lattice constants and distribution of cations in the interstitial voids. The initial decrease of cell edge parameter (a) for ZMMFO up to x = 0.2 and thereafter expected rise in the ‘a’ and the initial slower rate of reduction in the lattice constant for MACFO are explained as basic of cation occupancy. The magnetic ordering in both systems is explained by invoking statistical canting models. The compositional variation of magneton number (n{sub B}) for ZMMFO could be very well explained by Localized canting of spin (LCS) model while Random canting of spin (RCS) model was used for MACFO system.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2019

Microstructure and Magnetic Properties of Ba{sub 0.95}Y{sub 0.05}Fe{sub 12−x}Co{sub x}O{sub 19} Hexaferrites

Magnetoplumbite-type (M-type) barium ferrites doped with different Y–Co doping content Ba{sub 0.95}Y{sub 0.05}Fe{sub 12−x}Co{sub x}O{sub 19} (x = 0, 0.1, 0.2, 0.3, 0.4, and 0.5) were successfully prepared by ceramic process and investigated in this paper for the first time. X-ray diffraction were used to analyze the phase of the prepared sample. The scanning electron microscopy (SEM) was used to measure the morphology, and magnetic properties were measured by vibrating sample magnetometer (VSM). The results of XRD show that the single phase of M-type barium ferrites was obtained with the increase of Co content (x), but α-Fe{sub 2}O{sub 3} occurred when x exceeds 0.3. The SEM results exhibit the uniform plane hexagonal structures of M-type ferrites with all range of Co doping content. VSM results display that magnetization (M{sub s}) and coercivity (H{sub c}) show the same tendency that their values first increase and then decrease with the increase of Co content.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Influence of secondary phases on phase and microwave dielectric properties of new Ca{sub 2}Ce{sub 2}Ti{sub 5}O{sub 16} ceramics

Ca{sub 2}Ce{sub 2}Ti{sub 5}O{sub 16} ceramics processed via mix oxide route was investigated. Phase composition and microwave dielectric properties were measured using X-ray diffraction and a cavity method, respectively. CeO{sub 2} and another unidentified phase (that vanishes at ≥1400°C) existed as secondary phases along with the parent Ca{sub 2}Ce{sub 2}Ti{sub 5}O{sub 16} phase. The amount of the parent Ca{sub 2}Ce{sub 2}Ti{sub 5}O{sub 16} phase increased with increasing sintering temperature from 1350°C to 1450 °C accompanied by a decrease in the apparent density. The density decreased but ε{sub r} and Qufo increased with sintering temperature. An ε{sub r} ∼87.2, Qufo ∼5915 GHz and τ{sub f} ∼219 GHz was achieved for the sample sintered at 1450°C.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Continuing the Validation of CCIM Processability for Glass Ceramic HLLW Forms: Plan for Test AFY14CCIM-GC1

This test plan covers test AFY14CCIM-GC1which is the first of two scheduled FY-2014 test runs involving glass ceramic waste forms in the Idaho National Laboratory’s Cold Crucible Induction Melter Pilot Plant. The test plan is based on the successes and challenges of previous tests performed in FY-2012 and FY-2013. The purpose of this test is to continue to collect data for validating the glass ceramic High Level Liquid Waste form processability advantages using Cold Crucible Induction Melter technology. The major objective of AFYCCIM-GC1 is to complete additional proposed crucible pouring and post tapping controlled cooling experiments not completed during previous tests due to crucible drain failure. This is necessary to qualify that no heat treatments in standard waste disposal canisters are necessary for the operational scale production of glass ceramic waste forms. Other objectives include the production and post-test analysis of surrogate waste forms made from separate pours into the same graphite mold canister, testing the robustness of an upgraded crucible bottom drain and drain heater assembly, testing the effectiveness of inductive melt initiation using a resistive starter ring with a square wave configuration, and observing the tapped molten flow behavior in pans with areas identical to standard High Level Waste disposal canisters. Testing conditions, the surrogate waste composition, key testing steps, testing parameters, and sampling and analysis requirements are defined.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2014

In vitro cytotoxicity tests of ZnO‐Bi{sub 2}O{sub 3}‐Mn{sub 2}O{sub 3}-based varistor fabricated from ZnO micro and nanoparticle powders on L929 mouse cells

The present study investigated the cytotoxicity of ZnO‐Bi{sub 2}O{sub 3}‐Mn{sub 2}O{sub 3}-varistors. To this effect, ZnO‐Bi{sub 2}O{sub 3}‐Mn{sub 2}O{sub 3} varistors fabricated from ZnO micro-and nanoparticle powders are prepared via conventional ceramic processing method. The effects of ZnO particle size on the properties of ZnO varistors are also investigated. The strong solid-state reaction during sintering may be attributed to the high surface area of the 20 nm ZnO nanoparticles that promote strong surface reaction. The intensity of XRD peaks reflected the high degree of crystallinity of the ZnO nanoparticles. However, the width of the peaks in case of ZnO nanoparticles has increased due to the quantum size effect. The cytotoxicity evaluation of ZnO varistor was conducted on mouse connective tissue fibroblast cells (L929) using Trypan Blue Exclusion Assay analysis. The results show that the four types of varistor samples lead to cellular mitochondrial dysfunction, morphological modifications and apoptosis at the various concentration range and the toxic effects are obviously displayed in high concentration samples. 20nm-VDR is the most toxic materials followed by 40nm-VDR, P8-VDR, and W4-VDR in a descending order.

36 MATERIALS SCIENCE↗

DOE OSTI2014

The emergence of magnetic properties in (Pb{sub 0.845}Sm{sub 0.08}Fe{sub 0.035})(Ti{sub 0.98}Mn{sub 0.02})O{sub 3} and (Pb{sub 0.88}Nd{sub 0.08})(Ti{sub 0.98}Mn{sub 0.02})O{sub 3} perovskite ceramics

The emergence of magnetic properties and quadratic magnetoelectric coupling in a material with outstanding ferroelectric properties has been pursued. Thus, the multiferroicity driven by the substitution of rare earth R{sup 3+} ions (R = Sm, Nd) on the A-site of PbTiO{sub 3} perovskite ceramics has been investigated. In some samples, a transition element with large ionic radius, like Fe{sup 2+}, has been also added on the A site. Polycrystalline ceramic samples with composition (Pb{sub 1-3x/2-y}R{sub x}Fe{sub y}) (Ti{sub 0.98}Mn{sub 0.02})O{sub 3} (R = Sm; x = 0.08, y = 0.035) and (Pb{sub 1−3x/2}R{sub x})(Ti{sub 0.98}Mn{sub 0.02})O{sub 3} (R = Nd, x = 0.08) have been prepared by conventional solid state ceramic processing, starting from reagent grade oxide powders. X-ray diffraction analysis confirmed the obtaining of a crystalline phase with tetragonal P4 mm symmetry. Transmission electron microscopy and high resolution transmission electron microscopy investigations have been carried out in order to analyze the local structure. Temperature dependence of dielectric permittivity revealed a strong anomaly at the temperature T{sub c} of the paraelectric-ferroelectric phase transition. Transition temperature values depend on the R ion type and are lower than in pure lead titanate by 80–100 K. A broad anomaly of dielectric permittivity is found below 140–180 K, where magnetization also increases due to the quadratic magnetoelectric coupling between ferroelectric and magnetic states. For the (Pb{sub 0.845}Sm{sub 0.08}Fe{sub 0.035})(Ti{sub 0.98}Mn{sub 0.02})O{sub 3} composition, the piezoelectric charge coefficient at room temperature was d{sub 31} ∼−6.5 pC/N and the remanent magnetization M{sub r} at room temperature was about 0.1 emu/g.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Synthesis and characterization of mixed phases in the Ca–Co–O system using the Pechini method

Highlights: ► We have prepared mixed Ca–Co–O phases using the Pechini method. ► Reaction times are reduced relative to conventional solid-state synthesis. ► Products have high surface area suitable for ceramic processing. ► Product composition is dictated by both kinetic and thermodynamic control. ► A revised phase diagram of the Ca–Co–O system is proposed. - Abstract: The synthesis of mixed phases in the Ca–Co–O system using the Pechini method was investigated. The phases CaCo{sub 2}O{sub 4}, Ca{sub 3}Co{sub 4}O{sub 9} and Ca{sub 3}Co{sub 2}O{sub 6}, which can be expressed in terms of the molar ratios of the binary oxides (CaO:Co{sub 2}O{sub 3}) as (1:1), (3:2) and (3:1) respectively, were obtained in pure form. Powder X-ray diffraction data showed they are comparable with materials obtained by conventional solid-state synthesis. The mild synthesis conditions of the Pechini method allowed the evolution of the Ca–Co–O phases to be studied as a function of temperature and heating time. Both variables have a strong influence on the composition of the products, indicating that both kinetic and thermodynamic factors play a role, with the former being of more importance at lower temperatures. The (1:1) phase, previously not identified in the phase diagram of the Ca–Co–O system, was obtained preferentially across the composition range below ca. 650 °C. The (3:2) phase was preferred until ca. 800 °C. At even higher temperatures, the (3:1) phase is obtained. The upper thermal stability limit of mixed phases in the Ca–Co–O system increases with the Ca:Co ratio. An updated phase diagram for the Ca–Co–O system is proposed.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Structural, Bulk Permittivity, and Magnetic Properties of Lead-Free Electronic Material: Ba{sub 1}Bi{sub 1}Cu{sub 1}Fe{sub 1}Ni{sub 1}Ti{sub 3}O{sub 12}

In this report, Ba{sub 1}Bi{sub 1}Cu{sub 1}Fe{sub 1}Ni{sub 1}Ti{sub 3}O{sub 12} (BBCFNTO termed further) ceramics were synthesized using a conventional ceramic processing route. The formation of multiple phases has been confirmed from by the XRD pattern at room temperature. The surface micrograph indicates the uniform distribution of grains with distinct grain boundary. The co-relation between the impedance and dielectric parameters was realized by using a phase sensitive meter over a good temperature and frequency range. The temperature- and frequency-dependent dielectric properties are linked to the conduction mechanism. The dielectric constant (K) and loss (tanδ) are increased sharply at high-temperature region, which is expected to be the onset of dipolar relaxation phenomena. The contribution of grain boundary (GBs) and grain (Gs) effects can be identified using the complex impedance spectroscopy. This synthesized material is investigated to model multifunctional devices.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Solid State Reduction Driven Synthesis of Mn Containing Multi-principal Component Alloys

In recent years, high entropy alloys (HEAs), also known as multi-principal component alloys (MPCAs) have emerged as a new and exciting class of materials. This paper reports on the solid state reduction synthesis of a series of CoFeNiMn-based MPCA compositions, starting from a mixture of the corresponding oxides. One of the aims of the study was to test whether the degree of reduction of MnO, a highly stable oxide, could be enhanced by tailoring the alloy composition. Specifically, the influence of Ni content was studied because Ni exhibits a significant negative enthalpy of mixing with Mn. High purity precursor powders of Co(OH) 2 , Fe 2 O 3 , MnO 2 , and NiO were milled and mixed using standard ceramic processing methods. Here, the nominal sample compositions (assuming complete oxide reduction) were (CoFeMn) x Ni (1-x) , for x = 0, 0.083, 0.166, and 0.25. The oxide samples were subjected to a series of isothermal reduction anneals in flowing 3 pct H 2 –Ar at 1100 °C. The resulting microstructures were characterized using scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The composition of the resulting MPCAs was determined quantitatively using wavelength dispersive spectroscopy (WDS) in the electron microprobe. The study revealed that for each of the initial oxide compositions studied, it was possible to achieve an MPCA with ~ 25 at. pct Mn. These results were found to be consistent with the predictions of a thermodynamic model whereby a negative enthalpy of mixing (ΔH mix ), combined with a contribution from configurational entropy, can offset a positive free energy of reduction (ΔG red ). The incorporation of vibrational entropy into first principles calculations was found to have a significant effect on the predicted crystal structure of the MPCAs.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Thin film growth effects on electrical conductivity in entropy stabilized oxides

Entropy stabilization has garnered significant attention as a new approach to designing novel materials. Much of the work in this area has focused on bulk ceramic processing, leaving entropy-stabilized thin films relatively under-explored. Following an extensive multi-variable investigation of polycrystalline (Mg 0.2 Co 0.2 Ni 0.2 Cu 0.2 Zn 0.2 )O thin films deposited via pulsed laser deposition (PLD), it is shown here that substrate temperature and deposition pressure have strong and repeatable effects on film texture and lattice parameter. Further analysis shows that films deposited at lower temperatures and under lower oxygen chamber pressure are 40x less electrically resistive than otherwise identical films grown at higher temperature and pressure. Annealing these films in an oxygen-rich environment increases their electrical resistivity to match that of the films grown at higher temperatures and pressures. Because of this, the electric conductivity is hypothesized to be the result of polaron hopping mediated by transition metal valence changes which compensate for oxygen off-stoichiometry.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Review of additive manufacturing and densification techniques for the net- and near net-shaping of geometrically complex silicon nitride components

Silicon nitride (Si 3 N 4 ) is an advantageous material due its unique combination of mechanical, thermal, chemical, and electrical properties both at ambient and elevated temperatures. Because of these properties there are a wide range of applications for Si 3 N 4 components. Applications include heat exchangers, environmental barrier coatings, osteointegration scaffolds, radomes, and integrated circuitry. Furthermore, such applications often require geometric complexity for efficient and/or effective operation. However, traditional ceramics processing methods such as hot-pressing or die extrusion are typically limited to simple axis-symmetric shapes. With the advent of additive manufacturing, there has been significant advancement into the forming of geometrically complex Si 3 N 4 components. This review documents additive manufacturing advancements that have demonstrated, or are capable of, fabricating Si 3 N 4 components with complex geometry.

36 MATERIALS SCIENCE↗