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At least 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

VTO FY20Q4 quarterly report

Project Objective.This project has three objectives: (1) tuning microstructures of 3D-printed SSE separators,(2) determining material and processing compatibilities with cathode printing,and (3)3D printing of sintering-free SSE separators.Project Impact.All-solid-state lithium batteries are difficult to process due to the brittleness of ceramic materials, poor solid-solid contact, and electrolyte-electrode stability issues. As a result, the energy and power density and also cycling stability are far from satisfying. This project will address fabrication difficulties by using state-of-the-art 3D-printing techniques that can introduce 3D interfaces and architectures to enhance solid-solid contact and reduce charge transfer resistance. Success will benefit the DOE by establishing the best manufacturing methods for ASSBsto achieve VTO goals on the performance of beyond Li-ion batteries. Approach.The project employs 3D-printing techniques to manufacture SSEs and related components for ASSBs. The team starts with direct ink writing (DIW) to develop ink recipes with desired rheological properties and explore post-sintering approaches to achieve high densification. In parallel with DIW3D printing, the team also explores other 3D printing options, such as projection microstereolithography (PuSL). Both sintering and sintering-free approaches can gain benefit from 3D printing and therefore will be investigated.Out-Year Goals.The team will determine particle sizes and morphologies as well as post-processing conditions that deliver good ionic conductivity and charge transfer properties of LLZTO separators. They will examine co-sintering of LLZTO/cathode and determine the effects of material, particle size, surface coating, and sintering conditions.Collaborations.Microstructures, ionic conductivities, and mechanical properties will be provided to the LLNL simulation team, led by PI B. Wood, for establishing and validating phase-field modeling methods.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Tape casting and characterizations of MgO ceramics

Herein we report a high density MgO ceramic substrate produced by the tape casting technology. The tape casting formulation and process produced a uniform tape free of cracking. Y 2 O 3 and SiO 2 were used as the sintering aid for the pressureless sintering of the green tape. X-ray diffraction phase identification indicates that MgO is the main phase, while both Y 2 O 3 and SiO 2 sintering aids react with MgO to form MgY 4 Si 3 O 13 as the second phase. Liquid phase sintering occurs in the temperature range from 1030°C to ~1500°C, which is confirmed by the simultaneous Thermal Gravitation Analysis/ Differential Scanning Calorimeter (TGA/DSC) and the percent linear shrinkage and densification. A 96.5% theoretical density was achieved by presureless sintering at 1650°C for 2 hours, which was further increased to a fully dense structure using hotisostatic- pressing(HIP) at 1650°C and 207 MPa in argon. Scanning electron microscopy (SEM) and energy dispersive(EDS) spectroscopic analysis on the HIP’ed sample show that MgY 4 Si 3 O 13 is located at the MgO grain boundary and the sample has a fully dense structure. The refractive indices and extinction coefficient were measured on the HIP’ed sample along with thermal properties and dielectric properties. Thermal diffusivity and heat capacity were measured to calculate the thermal conductivity.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Microstructure evolution during binder jet additive manufacturing of H13 tool steel

H13 is one of the most used tool steels for both hot and cold work tooling applications. Binder jet additive manufacturing offers the potential to deposit complex tools at scale due to larger powder bed sizes and faster deposition rates. However, to date there is no published literature on the sintering of H13 to full densification. Here, we discuss the pressureless sintering of binder jet AM H13 steel to full densification via supersolidus liquid phase sintering (SLPS) while presenting appropriate process windows (1360 °C – 1380 °C) for densification without distortion. The process windows have been rationalized based on thermodynamic calculations of liquid volume fractions with temperature. We show that higher binder saturation results in higher carbon retention and subsequently early liquid formation that can initiate the sintering process at lower temperatures. We report abnormal grain growth during sintering and found that the solidification phase transformations play a critical role on microstructural evolution and must be considered to accurately model the kinetics of SLPS.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Tuning transition metal nanoparticles on a non-traditional support via experimental design

The ability to control metal nanoparticle size and morphology on supported catalysts is crucial for optimizing catalytic performance in targeted applications. Here, this work presents a systematic approach for tuning Ni particle and crystallite size on an unconventional, low-porosity silica fume support through select thermal treatments. The catalyst was synthesized via the deposition of nickelocene onto silica fume, resulting in well-dispersed Ni nanoparticles. A face-centered central composite design was employed to systematically assess the effects of time, temperature, and sintering gas environment on metal particle growth. The results demonstrate that the sintering gas environment is the primary factor governing particle and crystallite evolution, with temperature as the next most significant influence. Nickel nanoparticles sintered at temperatures of 650 °C and above under inert conditions exhibited substantial growth and polycrystalline structures, whereas samples treated in oxidative environments formed NiO, restricting particle mobility. Minimally oxidative (500 ppm O₂) environments facilitated rapid sintering while effectively removing residual ligands from the one-step nickelocene deposition process. Extensive structural characterization via a combination of scanning transmission electron microscopy, X-ray diffraction, hydrogen temperature programmed reduction, and small-angle X-ray scattering revealed that oxidative treatments enhanced metal-support interactions, as evidenced by increased reduction temperatures and narrower particle size distributions. These findings establish quantitative relationships between sintering parameters and Ni nanoparticle characteristics, providing a framework for rational catalyst design through controlled thermal treatments. This methodology is broadly applicable to other catalytic systems and provides a quantitative foundation for catalyst design.

CVD↗
DOE OSTI2025

Densification, microstructure, and mechanical properties of Mo–30W alloys fabricated from conditioned powders

Refractory alloys, such as molybdenum-based systems, are attracting growing interest for applications in extreme environments, such as in the nuclear and aerospace industries. Recent advances in sintering technologies, coupled with mechanical alloying, have enabled the tailored design of these alloys by leveraging powder characteristics to control final microstructures and mechanical properties. In this study, Mo-30W alloys were fabricated using electric field-assisted sintering (EFAS) from ball-milled powders with and without hydrogen treatment to investigate the influence of surface oxides on material properties and sintering behavior. The results revealed that samples processed from as-ball-milled powder contained a high density of oxides within the microstructure, whereas oxide presence was significantly reduced in samples fabricated from hydrogen-treated powders. Interestingly, the two powder types led to opposite trends in grain size distribution: samples from untreated powders exhibited grain refinement from sample periphery to the center, while samples from hydrogen-treated powders showed grain coarsening toward the center. This behavior is attributed to temperature gradients present during sintering due to electrical percolation pathway differences during Joule heating. The powder surface oxides may have influenced the temperature distribution and grain evolution. Microhardness profiles measured along both axial and thickness directions were consistent with the grain size distribution. Furthermore, oxide films on powder surfaces have delayed densification by hindering particle necking and atomic diffusion during sintering.

36 - MATERIALS SCIENCE↗
DOE OSTI2022

Fabrication and accelerated long-term stability test of asymmetrical hollow fiber-supported thin film oxygen separation membrane

Asymmetrical hollow fiber-supported thin film membrane may provide microstructural advantages for air separation and oxygen production. The fabrication of such a membrane is usually very difficult, particularly the sintering behaviors and thermal expansion coefficient (TEC) mismatch among multiple layers. This directly affects the reliability and long-term stability of the membrane. Here, in this research, the sintering behaviors of a set of simple oxides are systematically studied and ZnO is identified as a material component for composite substrate La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ (LSCF)-ZnO. The LSCF-ZnO ratios are further optimized by trading off several factors, e.g., matching the sintering behaviors and TECs of the LSCF-ZnO composite with those of LSCF thin film separation layer while enhancing the substrate strength. With the identified LSCF-ZnO ratio, the LSCF-ZnO composite hollow fiber substrate precursor is formed through slurry spinning process with porous microstructure being formed via phase inversion process. The thin film LSCF dense separation layer is then dip-coated on the substrate followed by co-sintering process. A thin, porous PrBaCo(Fe 0.6 Zr 0.2 Y 0.2 )O 5+δ (PBCFZY) catalyst layer is fabricated on the dense LSCF separation layer with dip-coating and sintering process, forming an asymmetrical membrane device LSCF-ZnO/LSCF/PBCFZY. Oxygen permeation test of the device is systematically conducted, and the fundamental mechanisms are analyzed. An accelerated long-term stability test of the membrane is also conducted (~550h, 46 thermal cycling loads), demonstrating excellent robustness and durability. The device is characterized and analyzed before and after the test. By replacing a considerable amount of high cost LSCF with low cost ZnO in the substrate, it not only enhances the stability but also reduces the capital cost of the membrane for practical applications.

42 ENGINEERING↗
DOE OSTI2023

Integrating fiber optic sensors into metallic components for sensing in harsh environments

The integration of fiber optic sensors into high-temperature materials is critical for real-time monitoring and autonomous operation of engineering systems. This study demonstrated a spark plasma sintering (SPS)-assisted embedding process for integrating sapphire fiber optic sensors into stainless steel components during part fabrication. Optical fibers were encapsulated in stainless steel 316L powders which were sintered at different fabrication conditions using SPS to investigate the effects of sintering parameters on the embedment. Measurements of optical transmittance, combined with microstructural analysis (X-ray computed tomography and scanning electron microscopy) and mechanical testing (tensile and microhardness), were conducted to examine the fiber functionality, fiber–matrix bonding quality, and properties of the sintered materials. Here, the results show that under suitable fabrication conditions, intact optical fibers can be encapsulated in highly-densified (>98 % relative density) stainless steel components. These conditions also led to a good bond at the fiber–matrix interface with micron-sized material interdiffusion across the interface. The sintering parameters were observed to affect fiber optical attenuation, where high temperature, pressure, and hold time during SPS enhanced fiber–matrix bonding and adversely affected optical transmission. Tensile testing confirmed the superior tensile strength and ductility of the matrix fabricated by SPS. Furthermore, the materials exhibited limited strength reduction (~70 MPa) upon the integration of fibers. This study demonstrates the effectiveness of SPS for fiber-material integration for high-temperature applications.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Dry Printing Pure Copper with High Conductivity and Adhesion for Flexible Electronics

Additive manufacturing of functional devices on various rigid and flexible substrates is rising rapidly due to their design flexibility, rapid manufacturing, and lower cost. Current printing technologies are ink-based and focused on printing silver (Ag) as conductive lines due to its matured ink formulation process, low sintering temperature, ease of printing, and low oxidation rate. However, Ag is the 68th most abundant element on Earth, while copper (Cu) is the 25th, making it much cheaper (>100×) while having a comparable conductivity to Ag. Therefore, printing Cu has become technologically and economically more attractive than Ag. Nevertheless, Cu printing is still a significant challenge in ink-based printing methods due to the higher sintering temperature relative to the glass-transition temperature of most flexible substrates, the higher oxidation rate, the challenging ink formulation process, and ink stability concerns. Here, we demonstrate printing highly conductive Cu on flexible polyimide substrates using a dry printing technique. Cu nanoparticles (~3–30 nm) are generated by on-demand laser ablation of a solid Cu target inside the printer head and under argon background gas. These Cu nanoparticles are then transported through a nozzle and onto the substrate, where they are laser-sintered in real time. The argon gas plays three critical roles in laser plume condensation for nanoparticle generation, transport, and sheath gas to avoid oxidation during sintering. The sintered nanoparticles thus show high electrical conductivity and mechanical stability under static and cyclic tests. Our dry printing technique can potentially revolutionize how electronic devices and sensors are additively manufactured for earth and space applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Smaller feature size impairs densification in digital light processing 3D printed ceramic samples

In this study, we investigate how geometric miniaturization affects the sintering densification behavior of alumina cylinders with various wall thicknesses (down to ∼500 µm in green body) fabricated via digital light processing (DLP). As the wall thickness decreased, the density of the sintered samples consistently declined. Microstructural characterization revealed the presence of a crack-rich surface skin that is ∼500 µm thick. As the wall thickness decreases, the skin's volume fraction rises, and its poor local densification increasingly dominates the part average, leading to an overall decrease in the density of the sintered samples. For the thinnest wall (500 µm) cylinder, macroscopic warping occurred during sintering. We suggest that warping further disrupts particle packing and induces through-thickness nonuniformity, further impairing densification in addition to the skin-fraction effect. These results highlight how geometric miniaturization may adversely influence the sintering behavior and final density of DLP-printed ceramics through distinct densification-limiting mechanisms.

Materials science↗
DOE OSTI2021

Ultra-Fast Laser Fabrication of Alumina Micro-Sample Array and High-Throughput Characterization of Microstructure and Hardness

In the light of recent advances in material informatics, there is a great demand for high-throughput approaches of sample fabrication and property characterization. Currently, no high-throughput approach has been demonstrated for the fast sampling of the microstructure and the correlated properties. In this paper, we demonstrate the ultra-fast fabrication of an alumina sample array and the high-throughput hardness characterization of these sample units. The alumina sample array was fabricated using picosecond (PS) laser micromachining and CO2 laser sintering within a short time (i.e., less than a few minutes). After laser sintering, the hardness of these sample units was characterized using micro-indentation, and the microstructure was observed using scanning electron microscopy (SEM). In each sample unit, the microstructure was uniform for the entire top surface and within about 20 µm depth from the top surface. The relative density (RD) and corresponding micro-hardness of the sample units was found to continuously vary over a wide range from 89% RD with 600 kgf/mm2 hardness to 99% RD with 1609 kgf/mm2 hardness. For these laser-sintered samples, the correlation of hardness and relative density of the alumina matched well with the literature reports on sintered alumina obtained using conventional low-throughput furnace sintering experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Power Electronics Materials and Bonded Interfaces - Reliability and Lifetime

The need for reliable bonded interface materials is critical to realize the performance benefits of wide-bandgap devices in power electronic modules, especially in operating temperatures greater than 150 degrees Celsius. In this paper, we investigate the thermomechanical performance of sintered copper (Cu) as a large-area attachment, bonded between Cu baseplates and active-metal-bonded substrates, under accelerated thermal shock (-40 degrees Celsius to 200 degrees Celsius) conditions. In the fabrication phase of the samples, we used different stencil patterns and found out that the grid and stripe patterns resulted in a better outgassing of the residual organics during the sintering process, thereby ensuring a substantially improved bond quality than a full-area print. The paste consisted of Cu microflakes and we performed sintering using a Budatec SP300 sintering press at 275 degrees Celsius with 15 MPa of bonding pressure for 5 minutes in a nitrogen atmosphere. Under accelerated experiments, we monitored the degradation of the sintered Cu bond in the samples through C-mode scanning acoustic microscope (C-SAM) images. To quantify the defect percentage in C-SAM images, we investigated image denoising techniques to exclude the pattern prints. Finally, we cross-sectioned a sample and obtained digital microscope images, which revealed adhesive fracture as the dominant failure mechanism.

ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2024

Ink Casting and 3D‐Extrusion Printing of Yb 14 MnSb 11 for High‐Temperature Thermoelectric Material

Abstract Complex shapes are created from Yb 14 MnSb 11 , a high‐temperature thermoelectric Zintl phase, via a two‐step process: i) layer‐by‐layer 3D‐extrusion of ink containing partially‐reacted powders which are ball‐milled from a blend of Yb, MnSb, and Sb powders; ii) heat treatment to synthesize the ternary compound Yb 14 MnSb 11 and densify the extruded powders. A high phase purity for Yb 14 MnSb 11 (83–94%) is achieved in both cast and 3D‐extruded ink specimens via a solid‐state reaction between Yb, MnSb, and Yb 4 Sb 3 during reactive sintering. Pressure‐free sintering at temperatures of 1200–1400 °C densifies the powders to 82% relative density but can also induce the decomposition of the Yb 14 MnSb 11 phase due to Yb sublimation. A process window with optimized sintering temperature and time is identified, achieving both low porosity and high phase purity and reaching a maximum zT = 0.61 at 1000 °C, about half of the maximum zT value for bulk Yb 14 MnSb 11 made via conventional processes (pressure sintering of precursor powders). The present approach – direct ink writing of ball‐milled powders, combined with reactive sintering – is a scalable and affordable method to fabricate thermoelectric legs with intricate 3D shapes, for enhanced performances in high‐temperature thermoelectric applications.

Chen, Ming [Department of Materials Science &amp, ↗
DOE OSTI2024

Optimization of Structurally Enhanced Solder Transient Liquid Phase Bonding

High temperature packaging technologies are a necessity for high temperature capable devices. SAC305 solder has an operational limit of 174°C imposed by creep effects which aligns well with current junction temperature limits of 175°C. Wide band gap semiconductor materials have the potential to reach junction temperatures of up to 800°C that are not currently attainable with significant reliability. Capitalizing on this potential will requires substrates and attachments that can operate well beyond the current 175°C standard. Silver sintering pastes have received widespread interest as a high temperature attachment alternative. However, the process requires high pressure bonding in an inert environment to achieve acceptable bond quality. Transient liquid phase (TLP) sintering is capable of good bond quality without pressure requirements but suffers from low thermal conductivity and only slightly reduced cost compared to silver sintering. SAC305 solder contains the same constituent materials for TLP as available copper-tin TLP sintering paste. By introducing engineered surface structures into the bond, intermetallic formation can be accelerated producing a bond similar to TLP sintering but in an ambient environment and for reduced cost. While this process has been demonstrated, it has not yet been optimized. Currently bonds are formed using a 75 μm stencil on substrate surface structures 24 μm tall, covering 19% of the bonding area. The process takes about 4 hours not including the formation of surface structures. Here, this study will center on the effects of stencil thickness and coating methods. Samples will be analyzed by scanning acoustic microscopy, die shear testing and cross sectional scanning acoustic microscopy.

42 ENGINEERING↗
DOE OSTI2021

Laser-based Adhesion Strength Measurements for Advanced Manufactured Sensor Adhesion Characterization

As part of the advanced manufacturing (AM) focus of the Nuclear Energy Enabling Technologies (NEET) Advanced Sensors and Instrumentation (ASI) Program, new in-house capabilities to fabricate and test novel active and passive in-pile sensors are being developed at the Idaho National Laboratory (INL). These advanced-manufactured sensors, such as peak temperature monitors and strain gauges, must be miniaturized and be able to provide real-time feedback, all while withstanding the coupled extremes of temperature and radiation typically observed in the environment of a nuclear test reactor. Fabricating durable and robust in-pile sensors with high fidelity requires a fundamental understanding of the optimal process parameters required in the AM technique, as well as the effect of deviations from optimal process parameters on the sensor-substrate adhesion and the ultimate robustness of the sensor. This report presents the use of a laser-based, non-contact approach for characterizing the adhesion of sensors manufactured using aerosol jet printing (AJP) that comprise of silver nanoparticle inks deposited and sintered on austenitic stainless steel (SS) 316L substrates. The effect of substrate surface roughness, surface energy, ink sintering time and sintering temperature on the printed sensor topography and the sensor-substrate adhesion has been systematically investigated. The sensor-substrate interfacial adhesion strength was determined from the critical laser pulse energy required to ablate/ detach the printed sensor from the substrate. Measurements of the sensor topography using optical profilometry revealed that post-deposition sintering at 400°C for 60 minutes resulted in a reduced sensor thickness, while plasma treating the substrate prior to printing yielded sensors with uniform thickness profiles transverse to the print direction. Sintering temperature and time were found to be the dominant parameters that affected sensor-substrate adhesion, followed by substrate surface roughness. The laser-based and locally-destructive approach for adhesion strength measurements shows promise in overcoming the challenges and limitations of current standardized peel tests and can be developed into a post-fabrication process control protocol for evaluating the durability of AM printed sensors in a high throughput fashion. Future studies will investigate the use of laser-induced spallation techniques as well as non-destructive laser ultrasonic methods for sensor-substrate adhesion characterization on sensors manufactured using AJP and other AM techniques such as plasma jet printing (PJP).

42 ENGINEERING↗
DOE OSTI2024

Development of Stable Solid Oxide Electrolysis Cells for Low-Cost Hydrogen Production

The project objective was to demonstrate a solid oxide cell-based steam electrolysis stack that exhibits robustness, reliability, endurance, hydrogen purity, and produces hydrogen at elevated pressure of 2 to 3 bar. Innovative materials and processing methods were evaluated to improve degradation characteristics. Performance improvement focused on nearly all layers involved in the cell and stack assembly. Primary attention was paid to zirconia-ceria interface resistance control via sintering optimization and decrease in degradation from the oxygen electrode by evaluating low strontium (Sr) or Sr-free composition for both the oxygen electrode and current collection layer. Stack robustness was addressed by validating redox tolerance of fuel electrode, confirming capability of cells to survive repeated thermal cycles, studying the effect of pressure on performance and degradation, evaluating the effect of contamination on fuel and oxygen electrode performance and degradation, and identifying mitigation strategies to improve performance. The characterization included evaluation of electrochemical performance and stability followed by microstructural analysis. At the cell level, performance and stability improvements were achieved by incorporating a Sr-free oxygen electrode and a denser oxygen electrode barrier layer. At the stack level, pressurized operation reduces demand on first stage compression, the redox tolerant fuel electrode mitigates risk from service interruptions, and improvements to interconnect coating alleviate chromium (Cr) contamination effects. The denser barrier layer was achieved by adding a sintering aid to the samaria-doped ceria (SDC) composition that reduced sintering temperature by 150 °C. The resulting density was on par with the baseline SDC barrier layer density and the lower sintering temperature resulted in less resistive phase formation during sintering. Button cell tests did not demonstrate a change in performance when exposed to silicon (Si) or manganese (Mn) impurities to the fuel electrode and Cr impurity to the oxygen electrode. More detailed study however is warranted. The project addressed SOEC performance and stability at the cell and stack levels through a systematic approach to known sources of degradation that were combined and tested in three stack tests using an electrolyte supported cell design to allow for evaluation of a variety of fuel and oxygen electrode compositions. STK-82 and STK-83 had identical compositions. STK-100 incorporated the best materials and processing variables developed under this and concurrent projects, and was tested at elevated pressure in steam electrolysis. • STK-82 recovered performance after redox and thermal cycling, demonstrating the robustness of the stack and seals. It exhibited stable performance in testing for 500 hours in SOEC mode, followed by 300 hours of cycling between SOEC and SOFC tests. Degradation during SOEC operation was 1.8 %/ 1,000 hours. • STK-83 generated hydrogen at >80% steam conversion, and oxygen above 98.5 % purity during pressurized operation. Both hydrogen and oxygen were generated at 3 barg pressure without the use of a pressure vessel. In addition to balanced pressure, electrolysis operation at 1 bar differential pressure across anode and cathode was also demonstrated to substantial the robustness of the cell and seal. • STK-100 measured at initial ambient pressure conditions showed an area specific resistance of 1.1 ohm-cm 2 , and STK-83 had 1.3 ohm-cm 2 .

08 HYDROGEN↗
DOE OSTI2026

Novel additive manufacturing for plasma facing materials ‐ creating a research pathway for minority students

This project addresses two critical and intertwined challenges in fusion energy, namely the shortage of a broadly trained scientific workforce and the lack of scalable manufacturing solutions for plasma-facing components (PFCs). Through a collaboration among Florida International University (FIU), Miami Dade College (MDC), and Purdue University, the project established structured, reproducible educational and research pathways that recruit and advance students from institutions historically outside the fusion energy enterprise, building the human capital that this field urgently needs. The project integrates the complementary research strengths of FIU and Purdue to investigate flash sintering as a transformative processing route for tungsten-based PFCs. Unlike conventional sintering approaches, flash sintering offers rapid densification at significantly reduced thermal budgets, making it a compelling candidate for fabricating complex tungsten geometries that must withstand extreme plasma-facing environments. Systematic experimental and modeling efforts will elucidate the fundamental mechanisms governing microstructure evolution, grain boundary chemistry, and thermomechanical response during flash sintering — knowledge that is presently lacking but essential for translating this technology into reliable manufacturing practice. The convergence of workforce development and cutting-edge manufacturing research positions this project to deliver measurable, durable impact: a pipeline of fusion-ready researchers cultivated through expanded institutional partnerships, and a validated materials processing framework that accelerates domestic readiness for next-generation fusion reactor construction.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

CEFAS Poster for Advanced Manufacturing Workshop 3/26/24

Electric-field assisted sintering (EFAS) is an advanced manufacturing method for the consolidation and processing of ceramic and metal materials. It is a particularly excellent candidate for efficient materials processing as it has greater than 90% energy cost savings and improved CO2 emissions compared to traditional sintering in a furnace. This is due to direct rapid heating of the materials and molds leveraging an electrification phenomenon called Joule heating where electrical current is passed through the sample/mold assemblies causing direct heating. The technique does have limitations though as it is traditionally a batch-process and suffers from scale up difficulties. To overcome this, researchers at Idaho National Laboratory changed the form factor of traditional EFAS instruments to develop and construct a continuous rolling electric-field assisted sintering (CEFAS) device.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Avoiding CO 2 Improves Thermal Stability at the Interface of Li 7 La 3 Zr 2 O 12 Electrolyte with Layered Oxide Cathodes

Abstract Solid‐state batteries promise higher energy densities and better safety than Li‐ion batteries with liquid electrolytes. However, the interface between solid electrolyte and cathode is unstable at the elevated temperatures that are needed while sintering to achieve good bonding between ceramic components. Here, the hypothesis is that, the gas environment, especially the presence of CO 2, is critical in determining the stability of the solid electrolyte–cathode interface. The effect of gas species on the interface is systematically probed, by a using Li 7 La 3 Zr 2 O 12 (LLZO) solid electrolyte with a thin film LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode as a model system to enable interface sensitivity. Detrimental phases formed at the interface and their onset conditions are identified by X‐ray absorption spectroscopy, X‐ray diffraction, and Gibbs free energy analysis. As a result, removing CO 2 and minimizing H 2 O(g) during sintering is necessary to obtain good contact at the LLZO|cathode interface without forming secondary phases. Sintering in O 2 is ideal, yielding excellent chemical stability and low interfacial resistance. Secondary phases also do not form in N 2, but oxygen loss occurs at elevated temperatures. The interfacial resistance obtained upon sintering in pure O 2 is comparable to the lowest values at LLZO interfaces with protective coatings, but here without the need for interface coatings.

25 ENERGY STORAGE↗