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NASA NTRS1992

The LiAl/FeS2 battery power source for the future

Advanced high power density rechargeable batteries are currently under development. These batteries have the potential of greatly increasing the power and energy densities available for space applications. Depending on whether the system is optimized for high power or high energy, values up to 150 Wh/kg and 2100 W/kg (including hardware) are projected. This is due to the fact that the system uses a high conductivity molten salt electrolyte. The electrolyte also serves as a separator layer with unlimited freeze thaw capabilities. Life of 1000 cycles and ten calendar years is projected. The electrochemistry consists of a lithium aluminum alloy negative electrode, iron disulfide positive electrode, and magnesium oxide powder immobilized molten salt electrolyte. Processed powders are cold compacted into circular discs which are assembled into bipolar cell hardware with peripheral ceramic salts. The culmination of the work will be a high energy battery of 40 kWh and a high power battery of 28 kWh.

Briscoe, J. Douglass↗

DOE OSTI2023

Reference electrode and electrochemical monitoring system

A reference electrode includes a metal body, a lead disposed within the metal body, an insulator disposed between the lead and the metal body, the insulator including a ceramic material, and a porous metal chamber coupled to the metal body, the lead extending into the porous metal chamber. The porous metal chamber is configured to maintain an electrolyte solution within the porous metal chamber to establish a redox couple with the lead.

Burak, Adam↗

DOE OSTI2022

Methods—Kintsugi Imaging of Battery Electrodes: Distinguishing Pores from the Carbon Binder Domain using Pt Deposition

The mesostructure of porous electrodes used in lithium-ion batteries strongly influences cell performance. Accurate imaging of the distribution of phases in these electrodes would allow this relationship to be better understood through simulation. However, imaging the nanoscale features in these components is challenging. While scanning electron microscopy is able to achieve the required resolution, it has well established difficulties imaging porous media. This is because the flat imaging planes prepared using focused ion beam milling will intersect with the pores, which makes the images hard to interpret as the inside walls of the pores are observed. It is common to infiltrate porous media with resin prior to imaging to help resolve this issue, but both the nanoscale porosity and the chemical similarity of the resins to the battery materials undermine the utility of this approach for most electrodes. In this study, a technique is demonstrated which uses in situ infiltration of platinum to fill the pores and thus enhance their contrast during imaging. Reminiscent of the Japanese art of repairing cracked ceramics with precious metals, this technique is referred to as the kintsugi method. The images resulting from applying this technique to a conventional porous cathode are presented and then segmented using a multi-channel convolutional method. We show that while some cracks in active material particles were empty, others appear to be filled (perhaps with the carbon binder phase), which will have implications for the rate performance of the cell. Energy dispersive X-ray spectroscopy was used to validate the distribution of phases resulting from image analysis, which also suggested a graded distribution of the binder relative to the carbon additive. The equipment required to use the kintsugi method is commonly available in major research facilities and so we hope that this method will be rapidly adopted to improve the imaging of electrode materials and porous media in general.

25 ENERGY STORAGE↗

DOE OSTI2021

Methods for tuning plasmonic and photonic optical resonances in high surface area porous electrodes

Abstract Surface plasmons have found a wide range of applications in plasmonic and nanophotonic devices. The combination of plasmonics with three-dimensional photonic crystals has enormous potential for the efficient localization of light in high surface area photoelectrodes. However, the metals traditionally used for plasmonics are difficult to form into three-dimensional periodic structures and have limited optical penetration depth at operational frequencies, which limits their use in nanofabricated photonic crystal devices. The recent decade has seen an expansion of the plasmonic material portfolio into conducting ceramics, driven by their potential for improved stability, and their conformal growth via atomic layer deposition has been established. In this work, we have created three-dimensional photonic crystals with an ultrathin plasmonic titanium nitride coating that preserves photonic activity. Plasmonic titanium nitride enhances optical fields within the photonic electrode while maintaining sufficient light penetration. Additionally, we show that post-growth annealing can tune the plasmonic resonance of titanium nitride to overlap with the photonic resonance, potentially enabling coupled-phenomena applications for these three-dimensional nanophotonic systems. Through characterization of the tuning knobs of bead size, deposition temperature and cycle count, and annealing conditions, we can create an electrically- and plasmonically-active photonic crystal as-desired for a particular application of choice.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Effects of processing conditions on flash sintering of commercial ZrN

Flash sintering (FS) is a potentially rapid and low-cost manufacturing technique for advanced ceramics. There are still many unknowns about ceramic FS, especially for highly conductive high-temperature ceramics (HTC), which often display decreased bulk conductivity with increasing temperature. This study qualitatively characterizes the flash behavior of highly conductive HTC materials using zirconium nitride (ZrN) as an example. The effects of processing parameters (e.g., DC voltage/electrical field strength, voltage ramp rate, post-flash holding time, mechanical pressure, sample milling, and choice of electrode materials) on ZrN flash behavior are also qualitatively studied and linked to samples microstructure and hardness. It is observed that best densification was achieved using 5 min Spex-milled ZrN powder under 25 MPa of applied pressure and constant 8 V DC. The potential mechanism for ZrN FS and the similarity and difference from FS of conventional oxides like YSZ have been proposed based on experimental observations, and the directions for future research are also pointed out.

Flash Sintering↗

DOE OSTI2024

A self-healing plastic ceramic electrolyte by an aprotic dynamic polymer network for lithium metal batteries

Abstract Oxide ceramic electrolytes (OCEs) have great potential for solid-state lithium metal (Li 0 ) battery applications because, in theory, their high elastic modulus provides better resistance to Li 0 dendrite growth. However, in practice, OCEs can hardly survive critical current densities higher than 1 mA/cm 2 . Key issues that contribute to the breakdown of OCEs include Li 0 penetration promoted by grain boundaries (GBs), uncontrolled side reactions at electrode-OCE interfaces, and, equally importantly, defects evolution (e.g., void growth and crack propagation) that leads to local current concentration and mechanical failure inside and on OCEs. Here, taking advantage of a dynamically crosslinked aprotic polymer with non-covalent –CH 3 ⋯CF 3 bonds, we developed a plastic ceramic electrolyte (PCE) by hybridizing the polymer framework with ionically conductive ceramics. Using in-situ synchrotron X-ray technique and Cryogenic transmission electron microscopy (Cryo-TEM), we uncover that the PCE exhibits self-healing/repairing capability through a two-step dynamic defects removal mechanism. This significantly suppresses the generation of hotspots for Li 0 penetration and chemomechanical degradations, resulting in durability beyond 2000 hours in Li 0 -Li 0 cells at 1 mA/cm 2 . Furthermore, by introducing a polyacrylate buffer layer between PCE and Li 0 -anode, long cycle life >3600 cycles was achieved when paired with a 4.2 V zero-strain cathode, all under near-zero stack pressure.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Atomic layer deposition for surface area determination of solid oxide electrodes

Surface area measurements are important for characterizing porous solids, but commonly used methods such as Brunauer–Emmett–Teller (BET) gas adsorption and computed nanotomography are lacking for certain applications such as the development of solid oxide fuel cell electrodes, which often have absolute surface areas <1 m 2 and contain nanoscale features. Presented is a novel method for the surface area determination of samples with total measurable areas of 1–1000 cm 2 with a standard deviation ± 1 cm 2 , utilizing the atomic layer deposition (ALD) of Al 2 O 3 over microstructurally complex internal porosity. The volume of alumina is then quantified using plasma spectroscopy and converted to an area using the known ALD layer thickness. Under the modest ALD reactor soak times used (8.5 s), the precursor penetration depth is found to be ~50 μm, exceeding the requirement for uniformly coating SOFC functional layers. A model system, (La 0.8 Sr 0.2 ) 0.98 MnO 3–δ /Ce 0.9 Gd 0.1 O 1.95 (LSM/GDC) scaffolds of ~2.7 m 2 g –1 , was measured using the technique and compared against the BET method, and comparable results were obtained but with 1000 times less material needed. The technique is demonstrated for measurements in two example areas of active SOFC research: exsolved (Ni, Fe) nanoparticles on an Sr(Ti, Fe, Ni)O 3–δ electrode and PrO x catalyst nanoparticles infiltrated onto LSM/GDC scaffolds. Finally, the technique may be broadly useful wherever the accurate surface area determination of small absolute quantities of porous ceramic structures on the order of 0.1–50 m 2 g –1 is sought.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

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↗

NASA NTRS1995

Improved Piezoelectric Loudspeakers And Transducers

Loudspeakers and related acoustic transducers of improved type feature both light weight and energy efficiency of piezoelectric transducers and mechanical coupling efficiency. Active component of transducer made from wafer of "rainbow" piezoelectric material, ceramic piezoelectric material chemically reduced on one face. Chemical treatment forms wafer into dishlike shallow section of sphere. Both faces then coated with electrically conductive surface layers serving as electrodes. Applications include high-fidelity loudspeakers, and underwater echo ranging devices.

Regan, Curtis Randall↗

DOE OSTI2022

Modeling ammonia-fueled co-flow dual-channel protonic-ceramic fuel cells

This paper reports the model development for a dual-channel protonic-ceramic fuel cell (PCFC) operating on ammonia fuel. The model considers the coupled interactions of several physical and chemical processes, including three-dimensional heat conduction within the bipolar plates and the membrane-electrode assembly (MEA), one-dimensional flow within the fuel and air channels, detailed heterogeneous catalytic reactions within the porous composite anode structure, Butler–Volmer representation of the charge-transfer chemistry, and Nernst–Planck transport of three charged defects (protons, oxygen vacancies, and small polarons) within the dense electrolyte membrane. The membrane-electrode assembly is composed of a Ni-BCZYYb (BaCe 0.7 Zr 0.1 Y 0.1 Yb 0.1 O 3-δ ) anode, a BCZYYb electrolyte membrane, and a BCFZY (BaCo 0.4 Fe 0.4 Zr 0.1 Y 0.1 O 3-δ ) cathode. Chemical and physical parameters for the MEA model are established using previously published button-cell data. One aspect of the study is to investigate the partial ammonia decomposition upstream of the fuel cell. Such fuel cracking increases the H 2 content of the fuel entering the PCFC, which may have benefits. However, endothermic ammonia pyrolysis within the composite anode structure assists with thermal control of the cell. The dual-channel model can be considered as the unit cell of a full fuel-cell stack.

25 ENERGY STORAGE↗

DOE OSTI2022

Electrochemical Aging and Halogen Oxides Formation on Multiwalled Carbon Nanotubes and Fe 3 O 4 @g-C 3 N 4 Coated Conductive Membranes

Electrochemical membrane filtration is widely reported to enhance water contaminants' degradation or rejection via anodic oxidation or cathodic repulsion. Despite their advances, electrochemical membranes or electrocatalysts often suffer from corrosion or passivation, especially under strong electrode potentials or reactions. Moreover, the formation of toxic byproducts, such as chlorinated organic compounds and oxyhalides (e.g., ClO 4 - ) is another major concern. This study investigated the membrane aging processes of two types of conductive membranes, multiwalled carbon nanotubes (MWCNTs) and ferrite/graphitic carbon nitride hybrids (Fe 3 O 4 @g-C 3 N 4 ) coated on ceramic membranes. Under high current densities (~ 20 mA∙cm -2 ) with anodic potentials (~10 V), MWCNTs and Fe 3 O 4 @g-C 3 N 4 catalysts underwent evident oxidation as indicated by an increase of the intensity ratio of the Raman spectral bands (I D /I G ) and charge transfer resistance (R ct ) of two electrochemical membranes. Under variations of electrode potentials, chloride or bromide were shown to be oxidized to bromate (BrO 3 - ) and chlorate (ClO 3 - ) at levels of 1-10 mmol∙L -1 . The formation of BrO 3 - and ClO 3 - was dependent on the solution pH, current densities (1-20 mA∙cm -2 ), and initial concentrations of Br or Cl ions. Finally, to warrant a safe and rational design and operation of electrochemically reactive membrane processes, membrane aging and toxic byproduct's formation deserve careful characterization under relevant water filtration environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Root Cause Analysis of Degradation in Protonic Ceramic Electrochemical Cell with Interfacial Electrical Sensors Using Data‐Driven Machine Learning

Abstract Protonic ceramic electrochemical cells (PCECs) offer promising paths for energy storage and conversion. Despite considerable achievements made, PCECs still face challenges such as physiochemical compatibility between componenets and suboptimal solid–solid contact at the interfaces between the electrolytes and electrodes. In this study, a novel approach is proposed that combines in situ electrochemical characterization of interfacial electrical sensor embedded PCECs and machine learning to quantify the contributions of different cell components to total degradation, as well as to predict the remaining useful life. The experimental results suggest that the overpotential induced by the oxygen electrode is 48% less than that of oxygen electrode/electrolyte interfacial contact for up to 1171 h. The data‐driven machine learning simulation predicts the RUL of up to 2132 h. The root cause of degradation is overpotential increase induced by oxygen electrode, which accounts for 82.9% of total cell degradation. The success of the failure diagnostic model is demonstrated by its consistency with degradation modes that do not manifest in electrolysis fade during early real operations. This synergistic approach provides valuable insights into practical failure diagnosis of PCECs and has the potential to revolutionize their development by enabling improved performance prediction and material selection for enhanced durability and efficiency.

25 ENERGY STORAGE↗

DOE OSTI2022

Direct utilization of gaseous fuels in metal supported solid oxide fuel cells

Direct utilization and internal reforming of gaseous fuels is investigated on symmetric-architecture metal supported solid oxide fuel cells (MS-SOFCs) with thin ceramic electrolyte and scaffold backbone layers, and low cost ferritic stainless steel supports on both sides. Infiltrated Pr-oxide and Ni/samarium-doped ceria catalysts are added to the cathode and anode electrodes, respectively. Initial performance and durability is evaluated for MS-SOFCs operating with natural gas, propane, ammonia, and dimethyl ether at 700 °C. Cells for natural gas and propane utilize a novel high entropy alloy (HEA) catalyst for internal reforming with performance and degradation rates similar to H 2 (0.5W cm -2 and ~12%/100 h). In conclusion, initial testing with sulfur shows reversible degradation for levels found in natural gas and irreversible degradation for higher levels found in commercial propane. Overall, MS-SOFCs show successful fuel flexibility.

08 HYDROGEN↗

DOE OSTI2023

Structural Tolerance of Zirconium Diboride under Electron Irradiation through in-situ Convergent Beam Electron Diffraction and Energy-dispersive X-ray Spectroscopy

Zirconium diboride (ZrB 2 ) is a ultra-high temperature ceramic with high melting temperature (>3000 K), super strength and hardness, good thermal conductivity, and excellent resistance to plasma erosion and chemical erosion, being widely applied in hypersonic flight, arc-electrodes, refractory materials, and plasma-facing materials in fusion reactors. Therefore, the structural stability of the material is essential for the applications. Up to now, the material was investigated under neutron irradiation and high-energy ion irradiations. It was reported that the neutron irradiation caused swelling and catastrophic cracking. High-energy ions (30 keV He + ) changed the surface morphology and caused the bright blue and brown colors on ZrB 2 surfaces between 920 K and 1120 K. The electron irradiation tolerance of the material has not been reported yet. Here we used convergent beam electron diffraction (CBED) and energy-dispersive X-ray spectroscopy (EDS) to investigate structural tolerances of ZrB 2 crystals under high-energy electrons at room temperature under vacuum. Finally, the investigation would benefit the understanding of its structural tolerance at microscales.

42 ENGINEERING↗

NASA NTRS2008

NASA Tech Briefs, July 2008

Topics covered include: Torque Sensor Based on Tunnel-Diode Oscillator; Shaft-Angle Sensor Based on Tunnel-Diode Oscillator; Ground Facility for Vicarious Calibration of Skyborne Sensors; Optical Pressure-Temperature Sensor for a Combustion Chamber; Impact-Locator Sensor Panels; Low-Loss Waveguides for Terahertz Frequencies; MEMS/ECD Method for Making Bi(2-x)Sb(x)Te3 Thermoelectric Devices; Low-Temperature Supercapacitors; Making a Back-Illuminated Imager with Back-Side Contact and Alignment Markers; Compact, Single-Stage MMIC InP HEMT Amplifier; Nb(x)Ti(1-x)N Superconducting-Nanowire Single-Photon Detectors; Improved Sand-Compaction Method for Lost-Foam Metal Casting; Improved Probe for Evaluating Compaction of Mold Sand; Polymer-Based Composite Catholytes for Li Thin-Film Cells; Using ALD To Bond CNTs to Substrates and Matrices; Alternating-Composition Layered Ceramic Barrier Coatings; Variable-Structure Control of a Model Glider Airplane; Axial Halbach Magnetic Bearings; Compact, Non-Pneumatic Rock-Powder Samplers; Biochips Containing Arrays of Carbon-Nanotube Electrodes; Nb(x)Ti(1-x)N Superconducting-Nanowire Single-Photon Detectors; Neon as a Buffer Gas for a Mercury-Ion Clock; Miniature Incandescent Lamps as Fiber-Optic Light Sources; Bidirectional Pressure-Regulator System; and Prism Window for Optical Alignment. Single-Grid-Pair Fourier Telescope for Imaging in Hard-X Rays and gamma Rays Range-Gated Metrology with Compact Optical Head Lossless, Multi-Spectral Data Compressor for Improved Compression for Pushbroom-Typetruments.

Source record↗

DOE OSTI2021

A mechanistic damage model for solid oxide fuel cell ceramic materials - Part I: Constitutive modeling

A multiscale mechanistic damage model for solid oxide fuel cell (SOFC) ceramics that combines micromechanics of stiffness reduction due to material porosity change and microcracking with a continuum damage mechanics (CDM) description for the evolution of microcracks up to fracture is developed in this work. The model also accounts for volumetric swelling of the anode due to redox cycling. Porosity change and swelling during redox combined with normal operating thermomechanical loads could increase the stress, strain and damage distributions in SOFC stacks leading them to failure. The proposed model involves three governing parameters: (i) the porosity in terms of the pore or void volume fraction, (ii) material swelling magnitude prescribed at a given loading step, and (iii) the damage variable that describes microcracking caused by thermomechanical loads and swelling. Pores and microcracks in the ceramics are modeled as randomly distributed ellipsoidal inclusions with negligible stiffness by an Eshelby-Mori-Tanaka formulation combined with an inclusion orientation distribution method. Microcracking damage evolution is described by a CDM formulation. Volumetric swelling is treated in a similar way to thermal expansion in the constitutive relations. After validation and numerical checks, the damage model is used to analyze a simplified SOFC positive-electrode/electrolyte/negative-electrode (PEN) structure subjected a redox cycle in addition to thermomechanical loads experienced during normal operation of a SOFC stack.

30 DIRECT ENERGY CONVERSION↗

NASA NTRS1996

Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

Advanced materials play an important role in the development of electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. The sol-gel process is a versatile solution for use in the fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. This processing technique is particularly useful in producing porous materials with high surface area and low density, two of the most desirable characteristics for electrode materials. In addition,the porous surface of gels can be modified chemically to create tailored surface properties, and inorganic/organic micro-composites can be prepared for improved material performance device fabrication. Applications of several sol-gel derived electrode materials in different energy storage devices are illustrated in this paper. V2O5 gels are shown to be a promising cathode material for solid state lithium batteries. Carbon aerogels, amorphous RuO2 gels and sol-gel derived hafnium compounds have been studied as electrode materials for high energy density and high power density electrochemical capacitors.

Chung-tse Chu↗

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↗