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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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Lead leaching and electrowinning in acetic acid for solar module recycling
It is imperative to recover lead (Pb) contained in end-of-life solar modules. In this paper, a two-step leaching and electrowinning process using acetic acid is investigated for Pb recovery. Acetic acid with hydrogen peroxide can dissolve Pb quickly and, under some conditions, in a matter of minutes. Pb electrowinning has been successfully demonstrated from aqueous solutions of 0.009 M lead(II) acetate with 0–10% v/v acetic acid. Pb-containing deposits are found on both the copper cathode and graphite anode. X-ray diffraction, energy-dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy confirm the presence of metallic Pb and Pb(II) oxide (PbO) co-deposits on the cathode. Further, there is also the formation of lead subacetate on the cathode under certain conditions. On the anode, the deposit consists of lead(IV) oxide and superoxide (PbO 2 and Pb 1–x O 2 ). A Pb recovery rate of 99% is achieved in 0.009 M lead(II) acetate solutions with 10% v/v acetic acid by applying a reduction potential of either –0.8 V or –1.0 V versus the silver/silver chloride reference electrode for 24h. Pb leaching with acetic acid is also demonstrated from milled silicon solar modules.
Method of fabricating an imaging X-ray spectrometer
A process for fabricating an X-ray spectrometer having imaging and energy resolution of X-ray sources is discussed. The spectrometer has an array of adjoinging rectangularly shaped detector cells formed in a silicon body. The walls of the cells are created by laser drilling holes completely through the silicon body and diffusing n(+) phosphorous doping material therethrough. A thermally migrated aluminum electrode is formed centrally through each of the cells.
Using the Principals of Electrochemistry to Understand and Overcome the Complicated Degradation Mechanisms of Silicon Anodes in Lithium-Ion Batteries [Slides]
Battery technology is the most significant problem facing widespread market adoption of battery electric vehicles (BEVs). The low energy density of state-of-the-art lithium-ion electrode materials leaves BEV owners and prospective buyers with lower ranges than a comparable internal combustion engine (ICE) vehicle, and vulnerable to a nascent fast charging network. Silicon has the potential to increase the anode energy density by nearly ten times compared to the incumbent material (graphite) and make BEVs a more competitive transportation option. However, lithiated silicon is extremely reactive towards components of the electrolyte and forms a heterogeneous, complicated, and dynamic solid at its surface known as the solid electrolyte interphase (SEI). Ideally, the SEI would passivate the silicon surface, but continuous chemical degradation persists even when the battery is not operating. This reactivity reduces silicon anode lifetimes well below the necessary standards for BEVs. The NREL-led Silicon Consortium Project is dedicated to understanding and solving these mechanisms of degradation. Here, I will discuss an electrochemical method that provides deep insights into the silicon interface during battery operation. I will link these observations to fundamental electrochemical principals and how they translate into actionable strategies that extend the lifetime of silicon anodes.
Mechanistic Understanding of Interphase-driven Aging in Silicon Anodes
Conventional solid electrolyte interphases (SEIs) strongly adhere to micro-silicon (µ-Si) and crack under volume changes, causing poor cycling performance. Nano-silicon improves cycling performance but remains costly with limited calendar life. Here potentiostatic ageing tests demonstrate that both calendar and cycle ageing are governed by SEI cracking and dissolution with different relative contributions. When the system is not dominated by SEI dissolution, the relative calendar life of Si anodes could correlates positively with their cycle life. LiF-rich SEI that enables long cycle life in µ-Si is therefore expected to enhance calendar life as well. Using this framework, we screened electrolytes, SEIs and electrodes and validated them with full-cell storage. LiF-rich SEI minimizes cracking and dissolution, enabling μ-Si to achieve excellent calendar life, whereas nano-silicon suffers from SEI dissolution and needs reduced electrolyte–electrode contact for better calendar life. This work clarifies calendar-ageing behaviour and accelerates electrolytes and SEI development for long-life Si anodes.
Stamping Nanoparticles onto the Electrode for Rapid Electrochemical Analysis in Microfluidics
Electrochemical analysis is an efficient way to study various materials. However, nanoparticles are challenging due to the difficulty in fabricating a uniform electrode containing nanoparticles. We developed novel approaches to incorporate nanoparticles as a working electrode (WE) in a three-electrode microfluidic electrochemical cell. Specifically, conductive epoxy was used as a medium for direct application of nanoparticles onto the electrode surface. Three approaches in this work were illustrated, including sequence stamping, mix stamping, and droplet stamping. Shadow masking was used to form the conductive structure in the WE surface on a thin silicon nitride (SiN) membrane. Two types of nanomaterials, namely cerium oxide (CeO2) and graphite, were chosen as representative nanoparticles. The as-fabricated electrodes with attached particles were characterized using atomic force microscopy (AFM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). Electrochemical analysis was performed to verify the feasibility of these nanoparticles as electrodes. Nanomaterials can be quickly assessed for their electrochemical properties using these new electrode fabrication methods in a microfluidic cell, offering a passport for rapid nanomaterial electrochemical analysis in the future.
High Throughput Source-less Plasma Deposition of Structured Silicon Anodes for Lithium-Ion Batteries
Amprius developed a manufacturing solution for silicon nanowire anode that relies on an inexpensive, high throughput, and high gas precursor utilization plasma deposition method that uses the anode foils as electrodes for plasma generation. The capacitively couple plasma (CCP) method is used in semiconductor and photovoltaic industry and Amprius modified existing high throughput equipment to use anode foils and to deposit amorphous silicon. The equipment was installed ahead of the program at Amprius site. The rest of the tasks included foil handling and process development. The equipment passed site acceptance tests (SAT) and the process parameter mapping was completed, indicating that the target process window limits produce output materials at the rate and with yield and specifications that meet the manufacturing target criteria. Amprius has hired supporting personnel to optimize processes and run the equipment. A parallel task verified the baseline performance of the silicon anode material, to be used as reference for the new manufacturing method.
Measurements of time and spatial resolution of AC-LGADs with different designs
AC-LGAD sensors are prime candidates for fast and precise measurement of charged particles in a variety of applications. In a fine-pitched pixel or strip AC-LGAD sensor, the signal generated by the passage of a particle is not localized in a limited volume in the sensor, but is shared among multiple electrodes. This signal sharing characteristic allows us to improve the spatial resolution of AC-LGAD sensors beyond the capabilities of common silicon trackers. Since the magnitude of the shared signal depends on the distance between the pixels or strips and the point of passage of the particle, signal sharing is strongly influenced by the geometry of the sensor. The electrode pitch and gap size as well as the shape can be fine tuned to maximize the space resolution, while keeping the detector granularity and the number of channels to be read out under control. Prototypes of AC-LGAD sensors produced at the Brookhaven National Laboratory covering a variety of possible geometries have been studied via Transient Current Technique using an infrared laser, and the signal sharing, spatial resolution, and time resolution of the different topologies have been measured. These results have been compared with measurements performed in test-beams with 120 GeV protons at the Fermilab Test Beam Facility. A time resolution of ~30 ps can be achieved using AC-LGAD sensors with a thickness of 50 μm, compatible to that of standard DC-coupled LGADs, while presenting a far superior spatial resolution. Finally, this combination of high precision, fast timing capabilities, and low material budget makes AC-LGADs an ideal choice for a truly 4D detector.
Synthesis and Surface Attachment of Molecular Re(I) Complexes Supported by Functionalized Bipyridyl Ligands
Eleven 2,2'-bipyridine (bpy) ligands functionalized with attachment groups for covalent immobilization on silicon surfaces were prepared. Five of the ligands feature silatrane functional groups for attachment to metal oxide coatings on the silicon surfaces, while six contain either alkene or alkyne functional groups for attachment to hydrogen-terminated silicon surfaces. The bpy ligands were coordinated to Re(CO) 5 Cl to form complexes of the type Re(bpy)(CO) 3 Cl, which are related to known catalysts for CO 2 reduction. Six of the new complexes were characterized using X-ray crystallography. As proof of principle, four molecular Re complexes were immobilized on either a thin layer of TiO 2 on silicon or hydrogen-terminated silicon. The surface-immobilized complexes were characterized using X-ray photoelectron spectroscopy, IR spectroscopy, and cyclic voltammetry (CV) in the dark and for one representative example in the light. The CO stretching frequencies of the attached complexes were similar to those of the pure molecular complexes, but the CVs were less analogous. For two of the complexes, comparison of the electrocatalytic CO 2 reduction performance showed lower CO Faradaic efficiencies for the immobilized complexes than the same complex in solution under similar conditions. In particular, a complex containing a silatrane linked to bpy with an amide linker showed poor catalytic performance and control experiments suggest that amide linkers in conjugation with a redox-active ligand are not stable under highly reducing conditions and alkyl linkers are more stable. So a conclusion of this work is that understanding the behavior of molecular Re catalysts attached to semiconducting silicon is more complicated than related complexes, which have previously been immobilized on metallic electrodes.
Postoperational examination of an externally configured thermionic converter
An externally configured thermionic converter was operated for 200 h. The converter was disassembled and examined to determine internal changes as a result of operation. The metal/ceramic seals and all joints were unaffected by operation. Converter output voltage and operational time were sufficient to produce electrolysis of stabilized zirconia spacers used in the converter. Surface analysis of the electrode surfaces indicated the presence on the tungsten emitter of only oxygen, carbon, and silicon. The niobium collector was, however, 25 to 40% covered with other elements. This coverage represented all elements present within the converter as construction materials other than silicon and tungsten, which were not detected on the collector, and carbon, which was detected only in small amounts.
Micromachined Tunneling Accelerometer
Separation of tunneling electrodes adjusted by varying electrostatic force. Major components of tunneling transducer formed on two silicon chips by microfabrication techniques. Use of electrostatic deflection reduces sensitivity of transducer to thermal drift and simplifies design. Sensitivity suitable for applications in which larger acceleration-sensing instruments required.
From Oxygen Generation to Metals Production: In Situ Resource Utilization by Molten Oxide Electrolysis
For the exploration of other bodies in the solar system, electrochemical processing is arguably the most versatile technology for conversion of local resources into usable commodities: by electrolysis one can, in principle, produce (1) breathable oxygen, (2) silicon for the fabrication of solar cells, (3) various reactive metals for use as electrodes in advanced storage batteries, and (4) structural metals such as steel and aluminum. Even so, to date there has been no sustained effort to develop such processes, in part due to the inadequacy of the database. The objective here is to identify chemistries capable of sustaining molten oxide electrolysis in the cited applications and to examine the behavior of laboratory-scale cells designed to generate oxygen and to produce metal. The basic research includes the study of the underlying high-temperature physical chemistry of oxide melts representative of lunar regolith and of Martian soil. To move beyond empirical approaches to process development, the thermodynamic and transport properties of oxide melts are being studied to help set the limits of composition and temperature for the processing trials conducted in laboratory-scale electrolysis cells. The goal of this investigation is to deliver a working prototype cell that can use lunar regolith and Martian soil to produce breathable oxygen along with metal by-product. Additionally, the process can be generalized to permit adaptation to accommodate different feedstock chemistries, such as those that will be encountered on other bodies in the solar system. The expected results of this research include: (1) the identification of appropriate electrolyte chemistries; (2) the selection of candidate anode and cathode materials compatible with electrolytes named above; and (3) performance data from a laboratory-scale cell producing oxygen and metal. On the strength of these results it should be possible to assess the technical viability of molten oxide electrolysis for in situ resource utilization on the Moon and Mars. In parallel, there may be commercial applications here on earth, such as new green technologies for metals extraction and for treatment of hazardous waste, e.g., fixing heavy metals.
Method of fabricating a PbS-PbSe IR detector array
A silicon wafer is provided which does not employ individually bonded leads between the IR sensitive elements and the input stages of multiplexers. The wafer is first coated with lead selenide in a first detector array area and is thereafter coated with lead sulfide within a second detector array area. The described steps result in the direct chemical deposition of lead selenide and lead sulfide upon the silicon wafer to eliminate individual wire bonding, bumping, flip chiping, planar interconnecting methods of connecting detector array elements to silicon chip circuitry, e.g., multiplexers, to enable easy fabrication of very long arrays. The electrode structure employed, produces an increase in the electrical field gradient between the electrodes for a given volume of detector material, relative to conventional electrode configurations.
PbS-PbSe IR detector arrays
A silicon wafer is provided which does not employ individually bonded leads between the IR sensitive elements and the input stages of multiplexers. The wafer is first coated with lead selenide in a first detector array area and is thereafter coated with lead sulfide within a second detector array area. The described steps result in the direct chemical deposition of lead selenide and lead sulfide upon the silicon wafer to eliminate individual wire bonding, bumping, flip chipping, planar interconnecting methods of connecting detector array elements to silicon chip circuitry, e.g., multiplexers, to enable easy fabrication of very long arrays. The electrode structure employed, produces an increase in the electrical field gradient between the electrodes for a given volume of detector material, relative to conventional electrode configurations.
High energy, long cycle life electrode for lithium-ion batteries
Anodes for electrochemical cells and batteries are described herein. In particular, and anode comprises silicon oxide particles on a transition metal current collector (e.g., copper, nickel, copper alloy, and the like), wherein the particles comprise nanocrystalline domains of silicon dispersed within a silicon oxide matrix. The particles do not include a metal oxide coating, and are produced by heating a silicon monoxide powder at a temperature in the range of about 400 to about 1100° C. under an inert atmosphere for about 2 to about 20 hours. In some embodiments, the particles are free from a metal oxide coating and have an average diameter of about 20 to 10000 nm; the nanocrystalline domains of silicon comprise about 10 to about 90 mole percent of the particles; and the nanocrystalline domains have dimensions of about 0.2 to about 50 nm in average diameter.
A Study on Advanced Lithium-Based Battery Cell Chemistries to Enhance Lunar Exploration Missions
NASA's Exploration Technology Development Program (ETDP) Energy Storage Project conducted an advanced lithium-based battery chemistry feasibility study to determine the best advanced chemistry to develop for the Altair lunar lander and the Extravehicular Activities (EVA) advanced lunar surface spacesuit. These customers require safe, reliable energy storage systems with extremely high specific energy as compared to today's state-of-the-art batteries. Based on customer requirements, the specific energy goals for the development project are 220 watt-hours per kilogram (Wh/kg) delivered at the battery level at 0 degrees Celsius (degrees Celcius) at a C/10 discharge rate. Continuous discharge rates between C/5 and C/2, operation over 0 to 30 degrees C, and 200 cycles are targeted. The team, consisting of members from NASA Glenn Research Center, Johnson Space Center, and Jet Propulsion laboratory, surveyed the literature, compiled information on recent materials developments, and consulted with other battery experts in the community to identify advanced battery materials that might be capable of achieving the desired results with further development. A variety of electrode materials were considered, including layered metal oxides, spinel oxides, and olivine-type cathode materials, and lithium metal, lithium alloy, and silicon-based composite anode materials. lithium-sulfur systems were also considered. Hypothetical cell constructs that combined compatible anode and cathode materials with suitable electrolytes, separators, current collectors, headers, and cell enclosures were modeled. While some of these advanced materials are projected to obtain the desired electrical performance, there are risks that also factored into the decision making process. The risks include uncertainties due to issues such as safety of a system containing some of these materials, ease of scaling-up of large batches of raw materials, adaptability of the materials to processing using established or reasonable cost manufacturing techniques, manufacturability of the materials in dimensions required for integration into battery cells of practical capacities, low Technology Readiness levels (TRl), and the ability to achieve the desired performance by the customer need dates. The advanced cell chemistry options were evaluated with respect to multiple quantitative and qualitative attributes while considering their projected performance at the end of the available development timeframe. Following a rigorous ranking process, a chemistry that combines a lithiated nickel manganese cobalt oxide (lithium NMC) cathode with a silicon-based composite anode was selected as the technology that can offer the best combination of safety, specific energy, energy density, and likelihood of success. Tasks over the next three years will focus on development of electrode materials, compatible electrolytes, and separator materials, and integration of promising components to assess their combined performance in working cells. Cells of the chosen chemistry will be developed to TRl 6 by 2014 and will then be transferred to the customers for infusion into their mission paths.
Pitch Carbon-coated Ultrasmall Si Nanoparticle Lithium-ion Battery Anodes Exhibiting Reduced Reactivity with Carbonate-based Electrolyte
Silicon anodes for lithium-ion batteries (LIBs) have the potential for higher energy density compared to conventionally used graphite-based LIB anodes. However, silicon anodes exhibit poor cycle and calendar lifetimes due to mechanical instabilities and high chemical and electrochemical reactivity with the carbonate-based electrolytes that are typically used in LIBs. In this work, we synthesize a pitch carbon-coated silicon nanoparticle composite active material for LIB anodes that exhibits reduced chemical reactivity with carbonate-based electrolytes compared to an uncoated silicon anode. Silicon primary particle sizes less than 10 nm diameter minimize micro-scale mechanical degradation of the anode composite, while conformal coatings of pitch carbon minimize the parasitic reactions between the silicon and the electrolyte. When matched with a high voltage NMC622 (LiNi 0.6 Mn 0.2 Co 0.2 O 2 ) cathode, the pitch carbon-coated silicon anode retains approximately 75% of its initial capacity at the end of 1000 cycles. Increasing the areal loading of the pitch carbon-coated silicon anodes to realize energy density improvements over graphite anodes results in severe mechanical degradation on the electrode level, highlighting a remaining challenge to be addressed in future work.
Carbon Nanotube-Based Structural Health Monitoring Sensors
Carbon nanotube (CNT)-based sensors for structural health monitoring (SHM) can be embedded in structures of all geometries to monitor conditions both inside and at the surface of the structure to continuously sense changes. These CNTs can be manipulated into specific orientations to create small, powerful, and flexible sensors. One of the sensors is a highly flexible sensor for crack growth detection and strain field mapping that features a very dense and highly ordered array of single-walled CNTs. CNT structural health sensors can be mass-produced, are inexpensive, can be packaged in small sizes (0.5 micron(sup 2)), require less power than electronic or piezoelectric transducers, and produce less waste heat per square centimeter than electronic or piezoelectric transducers. Chemically functionalized lithographic patterns are used to deposit and align the CNTs onto metallic electrodes. This method consistently produces aligned CNTs in the defined locations. Using photo- and electron-beam lithography, simple Cr/Au thin-film circuits are patterned onto oxidized silicon substrates. The samples are then re-patterned with a CNT-attracting, self-assembled monolayer of 3-aminopropyltriethoxysilane (APTES) to delineate the desired CNT locations between electrodes. During the deposition of the solution-suspended single- wall CNTs, the application of an electric field to the metallic contacts causes alignment of the CNTs along the field direction. This innovation is a prime candidate for smart skin technologies with applications ranging from military, to aerospace, to private industry.