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DOE OSTI2024

Improving 2D Schottky contacts using an intralayer strategy

An additional insulating layer between the electrode and semiconductor is beneficial to reduce the interfacial coupling and build two-dimensional (2D) Schottky contacts. Here, an intralayer strategy was proposed by using metallic 2D Bi 2 Sr 2 CaCu 2 O 8+δ (BSCCO) as contacts on 2D semiconductors. Inside a BSCCO monolayer, a conductive layer is sandwiched between insulating layers. Thus, the BSCCO contact has its own insulating layer, which is ultra-thin, single crystalline, and of high quality. This native layer could reduce the metal-induced gap state and thus weaken the interfacial Fermi level pinning effect. Such 2D Schottky diodes thus have barrier heights of 300 mV and a rectification ratio of 104. Furthermore, 2D metal-semiconductor field-effect transistors with BSCCO Schottky gate have a high on-off ratio, low leakage current, and low subthreshold swing value near the theoretical limit. The intralayer structure offers a new approach to improve the 2D Schottky junctions and has prospects in 2D electronics and optoelectronics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Tree-inspired lignin microrods-based composite heterogeneous nanochannels for ion transport and osmotic energy harvesting

One of the key processes of tree lignification is that lignin penetrates into the cell wall and fills in the cell wall framework, thereby increasing the hardness and hydrophobic of the tree channels, which is beneficial to consolidate and support the tree cell wall and water transport. Inspired by this natural process, we demonstrated a lignin-based nanofluidic heterogeneous membrane that closely mimics the channels in tree, which can realize ion transport function and effectively capture reverse electrodialysis. The membrane was synthesized by heating dealkaline lignin and PVA at 200 °C and this formed fusiform microrods and a closed-packed membrane. Simultaneously, this membrane composited with anodized aluminum (AAO) channels membrane at 200 °C to form asymmetric heterogeneous nanochannels membrane, which can transport counter-ions and harvest osmotic energy. This membrane implements ion current rectification in 0.1 M KCl electrolyte solution at pH 3 due to the confinement of pores and opposite surface charges in lignin-based heterogeneous nanochannel. An output power density of 0.97 W m- 2 is obtained under a 50-fold salinity gradient, which can be further improved to 1.19 W m -2 by increasing the salinity gradient from 50-fold to 500-fold. Accordingly, this nanofluidic membranes were prepared by using lignin, the key component in tree, which not only mimicked a crucial process of the water and ionic transport process of channels in tree, but also had the prospect in the field of osmotic energy harvesting.

09 BIOMASS FUELS↗

DOE OSTI2024

Ionic liquid mediated one-step perpendicular assembly in block copolymer thin films for ultrafiltration membrane applications

The rapid rise of oil and gas, petrochemical, food processing, and pharmaceutical industries has added a complex mixture of contaminants like oil, particulates, metals, and other organic compounds to wastewater. Multipurpose membranes with precise pore structure can offer a solution to this problem and block copolymers (BCP) can be used to achieve such structures. Achieving vertical assembly of BCP domains provides a perfect template for developing uniform through film channels for separation and transport of material, besides being useful for the rectification of defects in photolithography patterns. Producing such morphologies may require extensive film/substrate processing and is not always feasible for scale-up. With this article, we demonstrate a facile solution casting method to induce vertical domain assembly in as-cast diblock copolymer thin films in the presence of an ionic liquid (IL) additive that preferentially segregates to one block and neutralizes interfacial interactions. We also show the tunability of domain sizes by controlling the additive concentration. These vertically aligned morphologies are important for the development of next-generation lithographic techniques and form excellent templates for ultrafiltration membranes with uniform pore sizes. In conclusion, this article demonstrates how IL additives can be used to obtain stable non-equilibrium morphologies in as-cast BCP films and the effect of BCP molecular mass, block volume fractions, and IL content on self-assembly.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Dynamic characterization and performance evaluation of a 10-kW power take-off with mechanical motion rectifier for wave energy conversion

The power take-off (PTO) is a key component for wave energy converters. In this paper, a compact PTO with mechanical motion rectification rated at 10 kW is designed and prototyped, and characterized. A piecewise nonlinear dynamic model is established to describe its unique dynamic property. A linear hydraulic actuator is adopted in lab testing to drive the prototype and the unknown parameters of the dynamic model are identified. Further verification shows that the model can predict the dynamic performance of the PTO well. The test results show that the mechanical motion rectifier-based PTO can achieve overall energy transfer efficiency as high as 65% in regular waves even when the generator is working below the rated electric load and speed. In the irregular wave test, the PTO achieved the overall energy transfer efficiency of 54%, and the peak-to-average ratio acquired during the test is 12.5.

16 TIDAL AND WAVE POWER↗

DOE OSTI2022

Flexible cryogenic air separation unit—An application for low-carbon fossil-fuel plants

In this study, the rapid integration of intermittent renewable sources into the electricity grid is driving the need for a flexible cryogenic air separation unit (ASU) coupled with a low-carbon fossil-fuel plant. However, the state-of-the-art ASU process is highly integrated and nonlinear, which can significantly restrict its ramping rate. In this work, we study the fundamental dynamics of a state-of-the-art double-column ASU, focusing on the dynamic characteristics of the highly integrated and nonlinear heat and mass transfers, and we propose basic control methods for achieving high process ramping rates. We found that the vapor–liquid countercurrent flows in the low-pressure column are critical to the cryogenic rectification of air, which governs the ramp rate of the ASU. This countercurrent flow structure is created through a complex heat integration process in the ASU. Here, this process is simplified as a countercurrent heat transfer to reduce the complexity of studying the ASU dynamics. To preserve this flow structure, the heat integration is maintained so that its heat duty follows the ASU load, using several basic controllers on the critical stream flowrates. A flow-driven dynamic ASU model is built in Aspen Plus Dynamics to capture the basic ramping dynamics. This model revealed a fundamental mismatch in the dynamics in the ASU column that causes a significant loss of O 2 product purity when ramping down the ASU and slightly increases the purity when ramping up. Based on these findings, we propose a basic control method for rapidly ramping down/up the ASU while maintaining O 2 product purity. Simulation results show the ASU basic dynamic process successfully ramps at a rate up to 10 %/min (40–100 % load) while maintaining the O 2 product purity at 95.2–95.6 mol%.

42 ENGINEERING↗

DOE OSTI2020

Single Entity Electrochemistry in Nanopore Electrode Arrays: Ion Transport Meets Electron Transfer in Confined Geometries

Electrochemical measurements conducted in confined volumes provide a powerful and direct means to address scientific questions at the nexus of nanoscience, biotechnology, and chemical analysis. How are electron transfer and ion transport coupled in confined volumes and how does understanding them require moving beyond macroscopic theories? Also, how do these coupled processes impact electrochemical detection and processing? We address these questions by studying a special type of confined-volume architecture, the nanopore electrode array, or NEA, which is designed to be commensurate in size with physical scaling lengths, such as the Debye length, a concordance that offers performance characteristics not available in larger scale structures. The experiments described here depend critically on carefully constructed nanoscale architectures that can usefully control molecular transport and electrochemical reactivity. We begin by considering the experimental constraints that guide the design and fabrication of zero-dimensional nanopore arrays with multiple embedded electrodes. These zero-dimensional structures are nearly ideal for exploring how permselectivity and unscreened ion migration can be combined to amplify signals and improve selectivity by enabling highly efficient redox cycling. Our studies also highlight the benefits of arrays, in that molecules escaping from a single nanopore are efficiently captured by neighboring pores and returned to the population of active redox species being measured, benefits that arise from coupling ion accumulation and migration. These tools for manipulating redox species are well-positioned to explore single molecule and single particle electron transfer events through spectroelectrochemistry, studies which are enabled by the electrochemical zero-mode waveguide (ZMW), a special hybrid nanophotonic/nanoelectronic architecture in which the lower ring electrode of an NEA nanopore functions both as a working electrode to initiate electron transfer reactions and as the optical cladding layer of a ZMW. Furthermore, while the work described here is largely exploratory and fundamental, we believe that the development of NEAs will enable important applications that emerge directly from the unique coupled transport and electron-transfer capabilities of NEAs, including in situ molecular separation and detection with external stimuli, redox-based electrochemical rectification in individually encapsulated nanopores, and coupled sorters and analyzers for nanoparticles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Highly Rectifying Fluidic Diodes Based on Asymmetric Layer-by-Layer Nanofilms on Nanochannel Membranes

Nanochannel-based fluidic diodes display ion selectivity and ion-current rectification (ICR), which may prove important in energy harvesting and biosensors. This paper reports asymmetric functionalization of the outer surface of a flexible nanochannel polymer membrane to create fluidic diodes that give ICR. Layer-by-layer (LbL) adsorption with cross-linking of only the underlying part of the polyelectrolyte nanofilm leads to a porosity step across the film. The combination of a high effective surface-charge density and the porosity step in the film leads to a remarkable maximum ICR factor of ~200 with a pH gradient across the film. Incorporation of pH-sensitive polyelectrolyte components enables the ICR factor to increase an order of magnitude on going from pH 8 to pH 3. Furthermore, the coated membrane shows excellent anion-selectivity. Thus, LbL adsorption with partial cross-linking provides a simple method for creating coated nanochannel membranes that serve as pH-responsive ionic diodes for potential chemical/biosensors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Higher Ion Selectivity with Lower Energy Usage Promoted by Electro-osmotic Flow in the Transport through Conical Nanopores

The tradeoff between selectivity and throughput presents fundamental challenges to improve desalination and charge storage, salinity gradient-based energy harvesting, memory device/circuit development, and so forth. The well-known ion-current rectification and the recently resolved time-dependent transport hysteresis in conical nanopores or asymmetric nanointerfaces offer new opportunities for the selective transport of matter. This report shows that electro-osmotic flow (EOF) is an overlooked factor that increases ion selectivity while maintaining enhanced transport throughput in rectified nanoscale electrokinetic transport. The increased selectivity originates primarily from the suppression of anion flux by the fluid flow in the opposite direction under the applied electrical field. By solving the Poisson and Nernst–Planck (PNP) equations without and with coupled Navier–Stokes (PNP–NS) equations, the EOF effects on cation and anion transport are unequivocally revealed in asymmetric nanopipettes. The flux of cations and anions as well as the transference number and flow velocity are elucidated using the models and boundary conditions validated by previous experiments. A dimensionless parameter, radius over the Debye length, reveals optimal ion selectivity and energy cost at intermediate ion concentrations and nanopore sizes, up to hundreds of millimolars and tens of nanometers under time-dependent potential stimulus. Furthermore, the fundamental insights into EOF at nanointerfaces suggest new routes/strategies for better separation, analysis, and energy applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Tip-Enhanced Raman Nanospectroscopy of Smooth Spherical Gold Nanoparticles

We record nanoscale-resolved chemical images of thiobenzonitrile (TBN)-functionalized smooth gold nanospheres on silicon via tip-enhanced Raman (TER) nano-spectroscopy. The recorded images trace the nascence of the familiar doughnut-shaped scattering profile of nanoparticles on silicon at its origin (the particle surface), which appears as a horseshoe-shaped scattering pattern under our experimental conditions. The local optical field maps are in agreement with their simulated finite-difference time-domain analogues. Analysis of the recorded spectra with the aid of ab initio molecular dynamics-based Raman spectral simulations further suggests that optical rectification and molecular charging take place throughout the course of atomic force microscopy-based TER nanoscale chemical imaging.

Bhattarai, Ashish↗

DOE OSTI2020

A Closer Look at Corrugated Au Tips

A series of optical and electron microscopies are utilized in concert to unravel the structural, optical, and plasmonic properties of corrugated metallic tips. While the overall microscopic shapes of the tips dictate their optical resonances and plasmonic field enhancement factors, nanometric structural details govern their tip-enhanced Raman (TER) spectra and images. Using 4-thiobenzonitrile (TBN) as a molecular reporter, spatially resolved TER spectra reveal that optical rectification and molecular charging are among the prominent observables in the tip-tip TER geometry. The comparisons we provide reinforce the complexity of what otherwise may be regarded as sharp tip probes. We show the spurious appearance of anions is driven by highly localized resonances that appear as a result of surface corrugation and their manifestation throughout the course of TER nano-spectroscopy complicates spectral assignments, particularly in works aimed at understanding plasmon-enhanced/induced chemical transformations through enhanced Raman spectroscopy and imaging. Overall, nanoscale spatial variations in the TERS spectra suggest that the tip-tip geometry sustains junction plasmons that appear very different from what may be expected from the hybridization of the bulk tip resonances.

Bhattarai, Ashish↗

DOE OSTI2020

Gate-Tunable Semiconductor Heterojunctions from 2D/3D van der Waals Interfaces

Van der Waals (vdW) semiconductors are attractive for highly scaled devices and heterogeneous integration since they can be isolated into self-passivated, two-dimensional (2D) layers that enable superior electrostatic control. These attributes have led to numerous demonstrations of field-effect devices ranging from transistors to triodes. By exploiting the controlled, substitutional doping schemes in covalently-bonded, three-dimensional (3D) semiconductors and the passivated surfaces of 2D semiconductors, one can construct devices that can exceed performance metrics of “all-2D” vdW heterojunctions. Here, we demonstrate, 2D/3D semiconductor heterojunctions using MoS2 as the prototypical 2D semiconductor laid upon Si and GaN as the 3D semiconductor layers. By tuning the Fermi levels in MoS2, we demonstrate devices that concurrently exhibit over seven orders of magnitude modulation in rectification ratios and conductance. Our results further suggest that the interface quality does not necessarily affect Fermi-level tuning at the junction opening up possibilities for novel 2D/3D heterojunction device architectures

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2023

Dislocation-Assisted Quasi-Two-Dimensional Semiconducting Nanochannels Embedded in Perovskite Thin Films

Defect engineering in perovskite thin films has attracted extensive attention recently due to the films’ atomic-scale modification, allowing for remarkable flexibility to design novel nanostructures for next generation nanodevices. However, the defect-assisted three-dimensional nanostructures in thin film matrices usually has large misfit strain and thus causes unstable thin film structures. In contrast, defect-assisted one- or two-dimensional nanostructures embedded in thin films can sustain large misfit strains without relaxation, which make them suitable for defect engineering in perovskite thin films. Here, we reported the fabrication and characterization of edge-type misfit dislocation-assisted two-dimensional BiMnO x nanochannels embedded in SrTiO 3 /La 0.7 Sr 0.3 MnO 3 /TbScO 3 perovskite thin films. The nanochannels are epitaxially grown from the surrounding films without noticeable misfit strain. Diode-like current rectification was spatially observed at nanochannels due to the formation of Schottky junctions between BiMnO x nanochannels and conducting La 0.7 Sr 0.3 MnO 3 thin films. Such atomically scaled heterostructures constitute more flexible ultimate functional units for nanoscale electronic devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2025

Deriving Material Properties from Feedback Error Signals in Scanning Tunneling Microscopy

Imperfections in measurements, e.g., deviations and broadening, are not devoid of information; rather, they can reveal valuable physical properties and processes. Scanning tunneling microscopy leverages a negative feedback loop to regulate the tunneling current. Practically, current fluctuates around its set point, and such deviations are considered insignificant and ignored. Here, in this study, we investigate the information embedded in these deviations. In the constant-current mode with an active feedback loop, we observe an unexpected persistent DC current offset from its set point when the tunneling junction is periodically perturbed. We demonstrate both experimentally and theoretically that such error signals encode local tunneling barrier heights and the square of local differential conductance as a consequence of the interplay between rectification and active feedback compensation. We provide evidence on the generalizability of this phenomenology to other negative feedback systems. This new approach has the potential to broadly impact physical sciences by allowing rapid measurements without lock-in amplifiers.

36 MATERIALS SCIENCE↗

DOE OSTI2026

KTaO 3 -Based Supercurrent Diode

The supercurrent diode effect (SDE), characterized by nonreciprocal critical currents, represents a promising building block for future dissipationless electronics and quantum circuits. Realizing SDE requires breaking both time-reversal and inversion symmetry in the device. Here we use conductive atomic force microscope (c-AFM) lithography to pattern reconfigurable superconducting weak links (WLs) at the LaAlO 3 /KTaO 3 (LAO/KTO) interface. By deliberately engineering the WL geometry at the nanoscale, we realize SDE in these devices in the presence of modest out-of-plane magnetic fields. The SDE polarity can be reversed by simply changing the WL position, and the rectification efficiency reaches up to 13% under optimal magnetic field conditions. Time-dependent Ginzburg–Landau simulations reveal that the observed SDE originates from asymmetric vortex motion in the inversion-symmetry-breaking device geometry. This demonstration of SDE in the LAO/KTO system establishes a versatile platform for investigating and engineering vortex dynamics, forming the basis for engineered quantum circuit elements.

C-AFM lithography↗

DOE OSTI2026

Electrostatic Gating of Ionic Conductance through Heterogeneous van der Waals Nanopores

Nanofluidic ionic transistors typically require gate voltages above 1 V and operate only at submillimolar ionic strengths, limiting their biocompatible applications. We demonstrate ionic transistors consisting of single sub-10 nm nanopores drilled in van der Waals (vdW) heterostructures with internal gate electrodes made of few-layer graphene. These devices deliver up to 10-fold current modulation at gate voltages as low as 0.3 V in 10 mM KCl, and ∼2-fold modulation at near-physiological 100 mM KCl. Baseline conductance with no gate shows surface-charge-dominated transport below 100 mM KCl, consistent with negatively charged hBN walls and ∼5 nm opening of the pores. The surface charge and the electrochemical asymmetry introduced by the three-electrode configuration govern the device’s behavior: negative gate voltage (V G ) enriches ionic concentrations and enhances current, whereas positive V G induces a local depletion zone that suppresses transport. The current modulation by V G is dependent on the polarity of the transmembrane potential and leads to ion current rectification. Molecular dynamics simulations of a nanopore in a hBN–graphene–hBN stack reveal confinement and surface charge-dependent suppression of the relative permittivity of interfacial water. Continuum modeling with radially varying interfacial water permittivity reproduces the asymmetric I–V characteristics and explains how the embedded gate sculpts local potential and ion concentrations. By enabling sub-0.5 V control of ionic transport at up to 100 mM salt concentrations, these devices address a key need in nanofluidics to create low-power ionic circuits and biosensing.

Materials science↗

DOE OSTI2025

Anodized Aluminum Oxide Membrane Ionic Memristors

Memory effect in ion transport (IT) at the solid–solution interface is uniquely attractive in that the conductance depends on or “memorizes” the previous states. Hysteretic and rectified transport properties offer exciting potential to developing advanced iontronics and neuromorphic functions, improving the efficiency of energy conversion and electrochemical processes, and overcoming the selectivity-throughput bottleneck in the enrichment of low abundant species for environment- and energy-friendly separations, among others. Herein, memory effects are discovered in the rectified electrokinetic IT through anodized aluminum oxide (AAO) membranes containing densely packed highly ordered nanochannels (10 10 per cm 2 ). Characteristic memristor responses of pinched current–potential loops are resolved in voltammetric experiments and successfully reproduced through finite element simulation. Excitatory and inhibitory conductance states are shown to arise from the enrichment and depletion of mobile charge carriers. Structurewise, the transport symmetry is broken by the barrier oxide layer (BOL) on the one end of the cylindrical nanochannels across the AAO membranes. Charge selectivity is attributed to the gradient(s) of the space charge density across the BOL characterized by depth profiling via X-ray photoelectron spectroscopy analysis. The space charge gradient(s) overcomes the fundamental limitation of widely exploited surface charge effects to enable intense rectification and hysteresis prevailing at very high ionic concentrations up to 1–2 M. A new strategy is developed for controlling the preferential IT direction and selectivity via counterion intercalation and extraction/exchange. Mechanistic understanding is further confirmed through parameter variations such as potential scan rate and ionic strength, which also demonstrates convenient controls of the related functions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Enhancement of THz generation in LiNbO3 waveguides via multi-bounce velocity matching

Abstract To realize the full promise of terahertz polaritonics (waveguide-based terahertz field generation, interaction, and readout) as a viable spectroscopy platform, much stronger terahertz fields are needed to enable nonlinear and even robust linear terahertz measurements. We use a novel geometric approach in which the optical pump is totally internally reflected to increase the distance over which optical rectification occurs. Velocity matching is achieved by tuning the angle of internal reflection. By doing this, we are able to enhance terahertz spectral amplitude by over 10x compared to conventional single-pass terahertz generation. An analysis of the depletion mechanisms reveals that 3-photon absorption and divergence of the pump beam are the primary limiters of further enhancement. This level of enhancement is promising for enabling routine spectroscopic measurements in an integrated fashion and is made more encouraging by the prospect of further enhancement by using longer pump wavelengths.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Spatial defects nanoengineering for bipolar conductivity in MoS 2

Understanding the atomistic origin of defects in two-dimensional transition metal dichalcogenides, their impact on the electronic properties, and how to control them is critical for future electronics and optoelectronics. Here, we demonstrate the integration of thermochemical scanning probe lithography (tc-SPL) with a flow-through reactive gas cell to achieve nanoscale control of defects in monolayer MoS 2 . The tc-SPL produced defects can present either p- or n-type doping on demand, depending on the used gasses, allowing the realization of field effect transistors, and p-n junctions with precise sub-μm spatial control, and a rectification ratio of over 10 4 . Doping and defects formation are elucidated by means of X-Ray photoelectron spectroscopy, scanning transmission electron microscopy, and density functional theory. We find that p-type doping in HCl/H 2 O atmosphere is related to the rearrangement of sulfur atoms, and the formation of protruding covalent S-S bonds on the surface. Alternatively, local heating MoS 2 in N 2 produces n-character.

36 MATERIALS SCIENCE↗