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DOE OSTI2024

Innovative recycling of high purity silver from silicon solar cells by acid leaching and ultrasonication

Precious and scarce silver (Ag) is used as a front electrical contact in silicon solar panels. With massive amounts of solar panel waste coming to end-of-life, it is imperative to recover all the Ag from these modules. In this paper, we propose a novel method to easily reclaim Ag from end-of-life silicon solar cells using low concentration sulfuric acid (H 2 SO 4 ) leaching followed by ultrasonication. Our process simplifies the Ag recycling procedure by directly recovering the Ag contacts from solar cells, eliminating the need for secondary precipitation/electrodeposition. First, scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) was used to study the leaching and ultrasonication process on rejected solar wafers. Next, a solar panel from landfill was heated in a furnace to burn off the polymer encapsulant. The silicon wafers were then collected from the burning process and leached in 2 M H 2 SO 4 at two different shaking speeds for 48 hours at room temperature. Finally, the end-of-life silicon wafer pieces were collected, sonicated in water, and then the sonication water was centrifuged to show a proof-of-concept to recover the Ag contacts. Inductively coupled plasma optical emission spectroscopy (ICPOES) is used to monitor dissolved elements in the leachate as a function of time and shaking speed. XPS is used to evaluate the composition of the silicon cell wafer surface before and after H 2 SO 4 leaching. SEM is used to image the recovered Ag contacts morphology and EDX confirms the recovered particles contain high amounts of Ag. Furthermore, a proposed schematic illustrates the authors’ hypothesis for the peeling mechanism.

14 SOLAR ENERGY↗

DOE OSTI2024

Assessment of dissimilar metal corrosion in molten chloride salt

Dissimilar metal corrosion between high nickel alloys and stainless steel was tested in purified molten chloride salt. Preliminary results have shown that corrosion rates are significantly affected for samples both when electrically connected and isolated. Suggesting that galvanic corrosion as well as non-galvanic dissimilar metal corrosion play a role in corrosion processes for multi component systems. Finally, these results suggest that even if efforts to prevent electrical contact are taken, close proximity of structural materials can still change corrosion rates in molten salt environments.

14 SOLAR ENERGY↗

DOE OSTI2019

Surface energies, adhesion energies, and exfoliation energies relevant to copper-graphene and copper-graphite systems

We have generated precise values for several key energies that are relevant to Cu-graphene or Cu-graphite systems. Such systems may find technological applications that range from graphene synthesis, to condensation heat transfer, to electrical contacts to graphene, to composites. Using density functional theory, we have calculated surface energies of the three low-index faces of bulk Cu. We find that these surface energies, calculated with the PBEsol functional, are significantly higher than with the more common PBE functional and agree more closely with experiment. We have also calculated the surface energies of graphene and graphite, the exfoliation energy between graphene and graphite, and the adhesion energies between graphene or graphite and a Cu(111) slab. The adhesion energy between a carbon layer and Cu(111) is close to the exfoliation energy and cleavage energy of graphite, the four sets of values spanning a range of only 0.394–0.456 J/m2. Our results are consistent with the earlier experimental observation of three-dimensional growth of Cu on top of graphite. The energies are also used to perform a continuum Winterbottom analysis and also discrete (atomistic) variants of this analysis to predict the equilibrium shapes of Cu particles supported on graphite.

Han, Yong↗

DOE OSTI2025

High-throughput multimodal exploration of a nanocrystalline Cu-Ag library

Sputter-deposited, nanocrystalline Cu-Ag thin films produced across a broad compositional and deposition-parameter space were evaluated to unravel the process-structure-property relationships important for creating hard, conductive electrical contacts and coatings. Combinatorial deposition involving pulsed direct current magnetron sputtering of elemental targets enabled swift examination of nearly the full range of alloy compositions and a relevant portion of deposition atomistics. Several high-throughput characterization modalities were employed to evaluate the chemistry, structure, and properties of the films. The resultant hardness, modulus, film density, crystal texture, and resistivity were analyzed in terms of key deposition characteristics (incident atom kinetic energy and incidence angle) predicted by binary-collision, kinematic Monte Carlo simulations. The study revealed improved hardness, parabolic resistivity dependence on composition, and compositional and process dependencies of film tarnishing. The results are discussed in the context of variations in microstructure and film density. Transmission electron microscopy and X-ray diffraction demonstrate several forms of compositional variation including solute segregation to grain boundaries as well as periodic, intragranular compositional modulations. Annealing of a Cu-rich alloy film exhibiting grain boundary segregation showed that this as-deposited, compositional variation is not stable above 100 °C. Finally, the Cu-Ag system is shown to have potential for hard, conductive, tarnish-resistant and room temperature-stable nanocrystalline thin films across the composition space.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Thick Electrode Design for Facile Electron and Ion Transport: Architectures, Advanced Characterization, and Modeling

The demand for lithium ion batteries continues to expand for powering applications such as portable electronics, grid-scale energy storage, and electric vehicles. As the application requirements advance, the innovation of lithium ion batteries toward higher energy density and power output is required. Along with the investigation of new materials, an important strategy for increasing battery energy content is to design electrodes with high areal loading to minimize the fraction of nonactive materials such as current collectors, separators, and packaging components, resulting in significant gains in energy content and the reduction of the system-level cost. However, the adoption of thick high areal loading electrodes has been impeded by sluggish charge transport and mechanical instability. With conventional slurry cast electrodes, battery function significantly deteriorates with increases in electrode thickness due to high cell polarization and the incomplete utilization of active materials. Thus, a consideration of approaches that facilitate an understanding and eventual adoption of high-loading electrodes is warranted to enable the deliberate advancement of next-generation batteries. Herein, this Account considers three aspects critical to the science and technology of thick high-loading electrodes. The first discussion covers recent approaches to the design and fabrication of high-loading electrodes. Ensuring electrical contact throughout the electrode is accomplished through the manipulation of conductive additives or using a conductive scaffold within the electrode. Ion transport can be facilitated through electrode design and fabrication approaches that deliberately control the electrode porosity and tortuosity. Second, advanced characterization methodologies are presented as the ability to determine the origins of transport limitations provide the insight needed to deliberately approach future designs. Spectroscopic and diffraction methods have been used to characterize the 2D and 3D pore structure and composition of the electrodes. Furthermore, operando methods that yield spatially and temporally resolved information regarding the progression of the electrochemical reaction are highlighted. The third aspect considered is the utilization of modeling. Physically based continuum models linked with the results of experimental characterization have been demonstrated and then allow the rapid simulation of a variety of deliberate electrode designs and their impacts on functional electrochemistry. Variables relevant to the designs can be tested by the model under a series of use conditions to identify those of most promise for a specific application. Finally, an outlook on future opportunities for high-loading battery electrode research is provided to inform and entice practitioners in the field to pursue these important directions of inquiry.

25 ENERGY STORAGE↗

DOE OSTI2021

Direct Optical Lithography of CsPbX 3 Nanocrystals via Photoinduced Ligand Cleavage with Postpatterning Chemical Modification and Electronic Coupling

Microscale patterning of solution-processed nanomaterials is important for integration in functional devices. Colloidal lead halide perovskite (LHP) nanocrystals (NCs) can be particularly challenging to pattern due to their incompatibility with polar solvents and lability of surface ligands. Here, we introduce a direct photopatterning approach for LHP NCs through the binding and subsequent cleavage of a photosensitive oxime sulfonate ester (-C=N-OSOO-). The photosensitizer binds to the NCs through its sulfonate group and is cleaved at the N-O bond during photoirradiation with 405 nm light. This bond cleavage decreases the solubility of the NCs, which allows patterns to emerge upon development with toluene. Postpatterning ligand exchange results in photoluminescence quantum yields of up to 79%, while anion exchange provides tunability in the emission wavelength. Finally, the patterned NC films show photoconductive behavior, demonstrating that good electrical contact between the NCs can be established.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2019

Poly(4-vinylbenzoic acid): A Re-Engineered Binder for Improved Performance from Water-Free Slurry Processing for Silicon Graphite Composite Electrodes

In silicon-based lithium-ion batteries, polymeric binders play the crucial role of “gluing” the electrode matrix together, providing strong adhesion between the active silicon (Si) and conductive carbon particles and keeping them in electrical contact, despite considerable volumetric changes during cycling. While remarkable progress has been seen in the development of binders, improved cycling performance is still needed to fully enable Si anodes. Achieving that end requires in turn a better understanding of the relationship between binder properties and cell cycling performance. Here, we describe a novel polymer binder, poly(4-vinylbenzoic acid) (P4VBA), developed by re-engineering the widely used poly(acrylic acid) (PAA) binder to explore that relationship. The modified structure produces a binder that is more compatible with 1-methyl-2-pyrrolidinone (NMP) slurries and affords much improved cycling performance of the fabricated cells. Compared with PAA binders, P4VBA provides higher initial and average capacities and better capacity retention. While P4VBA offers an interesting alternative to wet processing of the Si-based electrodes, this re-engineered binder is an initial effort to develop a better binder material by exploring the relationship between binder and cell cycling performance.

25 ENERGY STORAGE↗

DOE OSTI2019

Nanoimaging of Organic Charge Retention Effects: Implications for Nonvolatile Memory, Neuromorphic Computing, and High Dielectric Breakdown Devices

While a large variety of organic and molecular materials have been found to exhibit charge memory effects, the underlying mechanism is not well-understood, which hinders rational device design. Here, we study the charge retention mechanism of a nanoscale memory system, an organic monolayer on a silicon substrate, with Au nanoparticles on top serving as the electrical contact. Combining scanning probe imaging/manipulation and density functional simulations, we observe stable charge retention effects in the system and attributed it to polaron effects at the amine functional groups. Finally, our findings can pave the way for applications in nonvolatile memory, neuromorphic computing, and high dielectric breakdown devices.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Individual Electron and Hole Mobilities in Lead-Halide Perovskites Revealed by Noncontact Methods

Charge carrier mobilities help determine semiconductor performance in optoelectronic applications, but measurement of the individual electron and hole mobilities usually involves indirect methods or probes with electrical contacts that are influenced by the quality of the interface or contact. Here, a noncontact method is introduced to distinguish the mobilities of electrons and holes by combining time-resolved terahertz spectroscopy (TRTS) and optical transient reflection (TR) spectroscopy. The validation of this method is first demonstrated on a semi-insulator GaAs wafer, and then, three lead-halide perovskite polycrystalline films with different cation mixtures are studied. We find that the hole mobility is significantly higher (~10x) than that of the electron mobility in all of the perovskite thin films studied. The highly alloyed triple cation polycrystalline film shows the highest mobility, longest bulk carrier lifetime, and lowest surface recombination velocity.

14 SOLAR ENERGY↗

DOE OSTI2025

Shape Anisotropy-Dependent Leaking in Magnetic Neurons for Bio-Mimetic Neuromorphic Computing

Spiking neural networks seek to emulate biological computation through interconnected artificial neuron and synapse devices. Spintronic neurons can leverage magnetization physics to mimic biological neuron functions, such as integration tied to magnetic domain wall (DW) propagation in a patterned nanotrack and firing tied to the resistance change of a magnetic tunnel junction (MTJ), captured in the domain wall-magnetic tunnel junction (DW-MTJ) device. Leaking, relaxation of a neuron when it is not under stimulation, is also predicted to be implemented based on DW drift as a DW relaxes to a low energy position, but it has not been well explored or demonstrated in device prototypes. Here, in this work, we study DW-MTJ artificial neurons capable of leaky integrate-and-fire (LIF) behavior and demonstrate geometry-dependent leaking dynamics that results in repeatable, tunable LIF operation. Studying the behavior of five different device designs, we show tuning the geometry, stimulating fields and currents, and location of electrical contacts results in a wide range of neuron behavior. Additionally, implementation of an asymmetric notch allows for nonlinear pinning which increased expressivity without sacrificing leaking. The measured behavior is implemented in a simulated spiking neural network that outperforms a 1D model of continuous DW motion and approaches the performance of an ideal LIF activation function. The results show that the analog LIF capability of DW-MTJ neurons combines many desirable neuron functions into a single device, which can result in varied forms of multifunctional neuromorphic computing.

42 ENGINEERING↗

DOE OSTI2022

Magnetotelluric Investigations of the Kilauea Volcano, Hawaii

In 2002 and 2003 a collaborative effort was undertaken between Lawrence Berkeley National Laboratory, Sandia National Laboratories, the U.S. Geological Survey (USGS) Menlo Park, the USGS Hawaiian Volcano Observatory, and Electromagnetic Instruments Inc. to study the Kilauea volcano in Hawaii using the magnetotelluric (MT) technique. The work was motivated by a desire to improve understanding of the magma reservoirs and conduits within Kilauea and the East and Southwest Rift zones, which has implications for understanding Kilauea's plumbing system. An improved understanding of the rift zones has implications in understanding large-scale landslides that are generated in the Hilina Slump, which produce significant impacts on coastal communities. Up to eight stations operated simultaneously, with multiple remote reference sites, and data were processed using multi-station robust processing techniques. Data was acquired at 70 sites over the Southwest and East rift zones. Good to excellent quality data were obtained even in the harshest conditions, such as those encountered on the fresh lava flows of the East Rift Zone, where electrical contact resistances are on the order of 100 kΩ. A three-dimensional (3D) MT model study was done to guide interpretation of the observed MT measurements. Synthetic modeling demonstrates that conductive bodies in the upper 3 km can be spatially resolved where MT station sampling is good. Resistivity anomalies in the 3D inversions have a high degree of spatial correlation with previously published seismic velocity anomalies beneath Kilauea. Melt fractions between 0.096 and 0.117 are calculated for the Kilauea and Pu'u'ō'ō low resistivity anomalies, respectively.

58 GEOSCIENCES↗

DOE OSTI2019

Optically read Coriolis vibratory gyroscope based on a silicon tuning fork

In this work, we describe the design, fabrication, and characterization of purely mechanical miniature resonating structures that exhibit gyroscopic performance comparable to that of more complex microelectromechanical systems. Compared to previous implementations of Coriolis vibratory gyroscopes, the present approach has the key advantage of using excitation and probing that do not require any on-chip electronics or electrical contacts near the resonating structure. More specifically, our design relies on differential optical readout, each channel of which is similar to the 'optical lever' readout used in atomic force microscopy. The piezoelectrically actuated stage provides highly efficient excitation of millimeter-scale tuning fork structures that were fabricated using widely available high-throughput wafer-level silicon processing. In our experiments, reproducible responses to rotational rates as low as 1.8 × 10 3° h –1 were demonstrated using a benchtop prototype without any additional processing of the raw signal. The noise-equivalent rate, ΩNER, derived from the Allan deviation plot, was found to be <0.5° h –1 for a time of 10 3 s. Despite the relatively low Q factors (<10 4 ) of the tuning fork structures operating under ambient pressure and temperature conditions, the measured performance was not limited by thermomechanical noise. In fact, the performance demonstrated in this proof-of-principle study is approximately four orders of magnitude away from the fundamental limit.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Odd- and even-denominator fractional quantum Hall states in monolayer WSe 2

Monolayer semiconducting transition-metal dichalcogenides (TMDs) represent a unique class of two-dimensional (2D) electron systems. Their atomically thin structure facilitates gate tunability just like graphene does, but unlike graphene, TMDs have the advantage of a sizable band gap and strong spin–orbit coupling. Measurements under large magnetic fields have revealed an unusual Landau level (LL) structure, distinct from other 2D electron systems. However, owing to the limited sample quality and poor electrical contact, probing the lowest LLs has been challenging, and observation of electron correlations within the fractionally filled LL regime has not been possible. Here, through bulk electronic compressibility measurements, we investigate the LL structure of monolayer WSe 2 in the extreme quantum limit, and observe fractional quantum Hall states in the lowest three LLs. The odd-denominator fractional quantum Hall sequences demonstrate a systematic evolution with the LL orbital index, consistent with generic theoretical expectations. In addition, we observe an even-denominator state in the second LL that is expected to host non-Abelian statistics. Finally, our results suggest that the 2D semiconductors can provide an experimental platform that closely resembles idealized theoretical models in the quantum Hall regime.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Gas adsorption and light interaction mechanism in phosphorene-based field-effect transistors

Phosphorene-based field effect transistor (FET) structures were fabricated to study the gas- and photo-detection properties of phosphorene. The interplay between device performance and environmental conditions was probed and analyzed using in situ transport measurements. The device structures were exposed to different chemical and light environments to understand how they perform under different external stimuli. For the gas/molecule detection studies, inert (Ar), as well as, oxidizing (N 2 O), and reducing (H 2 and also N 2 H 4 ) agents were selected. The FET structure was exposed to these different gases, and the effect of each gas on the device resistance was measured. The study showed varying response towards different molecules. Specifically, no significant resistance change was observed upon exposure to Ar, while H 2 and N 2 H 4 were found to decrease the resistance and N 2 O had the opposite effect resulting in an increase in resistance. This work is the first demonstration for the detection of N 2 H 2 and N 2 O using a phosphorene-based system. These phosphorene-based FET structures were also found to be sensitive to light exposure. When such structure was irradiated with light, the current modulation was lost. The observed resistance changes can be explained as a result of the modulation of the Schottky barrier at the phosphorene-electrical contact interface due to the adsorbed molecules and charge transfer, and/or photo-induced carrier generation. Furthermore, the results were consistent with the transfer characteristics of V ds v s . V g .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Lithium vanadium oxide (Li 1.1 V 3 O 8 ) thick porous electrodes with high rate capacity: utilization and evolution upon extended cycling elucidated via operando energy dispersive X-ray diffraction and continuum simulation

The phase distribution of lithiated LVO in thick (~500 μm) porous electrodes (TPEs) designed to facilitate both ion and electron transport was determined using synchrotron-based operando energy dispersive X-ray diffraction (EDXRD). Probing 3 positions in the TPE while cycling at a 1C rate revealed a homogeneous phase transition across the thickness of the electrode at the 1st and 95th cycles. Additionally, continuum modelling indicated uniform lithiation across the TPE in agreement with the EDXRD results and ascribed decreasing accessible active material to be the cause of loss in delivered capacity between the 1st and 95th cycles. The model was supported by the observation of significant particle fracture by SEM consistent with loss of electrical contact. Overall, the combination of operando EDXRD, continuum modeling, and ex situ measurements enabled a deeper understanding of lithium vanadium oxide transport properties under high rate extended cycling within a thick highly porous electrode architecture.

25 ENERGY STORAGE↗

DOE OSTI2020

An interface-controlled Mott memristor in α -RuCl 3

Memristor devices have history-dependent charge transport properties that are ideal for neuromorphic computing applications. We reveal a memristor material and mechanism in the layered Mott insulator α-RuCl 3 . The pinched hysteresis loops and S-shaped negative differential resistance in bulk crystals verify memristor behavior and are attributed to a nonlinear coupling between charge injection over a Schottky barrier at the electrical contacts and concurrent Joule heating. Direct simulations of this coupling can reproduce the device characteristics.

Physics↗

DOE OSTI2023

An electron paramagnetic resonance study of the electron transport in heavily Si-doped high Al content AlxGa1−xN

High Al mole fraction AlGaN is an ultrawide bandgap semiconductor with potential applications in power electronics and deep UV detectors. Although n-type material is achievable with Si-doping, the role of Si is controversial, particularly for AlxGa1−xN with x > 0.8. For this paper, AlGaN films were grown by plasma-assisted molecular beam epitaxy onto bulk AlN substrates and doped with 1018–1020 cm−3 Si. We examine electron transport in heavily Si-doped AlxGa1−xN with x ≥ 0.65 using magnetic resonance, which allows us to probe the neutral donors directly rather than the free carriers and avoids complications due to electrical contacts. Transport was studied through the temperature-dependent linewidth of the electron paramagnetic resonance (EPR) signature for the neutral donor. Analysis shows evidence of hopping conductivity in the most lightly doped samples and impurity band formation in the most heavily doped ones. The EPR results, which are consistent with Hall measurements performed on the same samples, are promising for the development of highly conducting high Al content AlGaN.

Materials Science↗

DOE OSTI2024

Optical contrast analysis of α -RuCl 3 nanoflakes on oxidized silicon wafers

α-RuCl 3 , a narrow-band Mott insulator with a large work function, offers intriguing potential as a quantum material or as a charge acceptor for electrical contacts in van der Waals devices. In this work, we perform a systematic study of the optical reflection contrast of α-RuCl 3 nanoflakes on oxidized silicon wafers and estimate the accuracy of this imaging technique to assess the crystal thickness. Via spectroscopic micro-ellipsometry measurements, we characterize the wavelength-dependent complex refractive index of α-RuCl 3 nanoflakes of varying thickness in the visible and near-infrared. Building on these results, we simulate the optical contrast of α-RuCl 3 nanoflakes with thicknesses below 100 nm on SiO 2 /Si substrates under different illumination conditions. We compare the simulated optical contrast with experimental values extracted from optical microscopy images and obtain good agreement. Finally, we show that optical contrast imaging allows us to retrieve the thickness of the RuCl 3 nanoflakes exfoliated on an oxidized silicon substrate with a mean deviation of –0.2 nm for thicknesses below 100 nm with a standard deviation of only 1 nm. Our results demonstrate that optical contrast can be used as a non-invasive, fast, and reliable technique to estimate the α-RuCl 3 thickness.

2D materials↗