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DOE OSTI2019

Characterization of surface layers formed on DU10Mo ingots after processing steps and high humidity exposure

The design of monolithic U-Mo fuel elements fabricated from low-enriched uranium for use in high-power research reactors requires bonding of the fuel foil to either Al cladding or a Zr barrier layer. Processing of the U-Mo ingot to final foil form has the potential to generate surface layers on the foil that differ from the bulk, metallic U-Mo. The interfacial properties between the U-Mo and Zr or Al cladding layers will then be determined by these surface layers. We use x-ray photoelectron spectroscopy, cross-sectional scanning electron microscopy, and atomic force microscopy to characterize the composition, oxidation state, and morphology of the surface layers that form after hot rolling and cold rolling depleted U–10 wt% Mo alloy (DU10Mo). A thick uranium nitride layer is observed after hot rolling, although its origin is likely from a previous processing step. The surface composition of cold-rolled DU10Mo varied significantly between two foils, with a strongly Mo-depleted surface oxide layer observed on one foil but nominal Mo composition observed on the other. The efficacy of acid etching in HNO 3 is compared to that of electropolishing in H 2 SO 4 to remove the surface layers, and both methods are found to be similarly effective. Both laboratory (low humidity) air exposure and longer rinse times in water are shown to promote the formation of surface oxide layers. Exposure of both acid-etched and electropolished DU10Mo foils to humid air (97% relative humidity) for six weeks results in formation of a thick oxide layer due to corrosion. The oxide layer on the acid-etched foil is thicker and more highly oxidized than the oxide layer that forms on the electropolished foil, and these differences in oxidation behavior are attributed to higher surface roughness on the acid-etched foil. In general, Mo is found to play a role as a sacrificial element, typically exhibiting a larger ratio of Mo 6+ / Mo 4+ than U 6+ / U 4+ . This is unexpected, given the greater thermodynamic driving force to form U oxides than Mo oxides.

Kaspar, Tiffany C. (ORCID:0000000328167569)↗

DOE OSTI2019

Scanning Probe Lithography Patterning of Monolayer Semiconductors and Application in Quantifying Edge Recombination

Scanning probe lithography is used to directly pattern monolayer transition metal dichalcogenides (TMDs) without the use of a sacrificial resist. Here, using an atomic-force microscope, a negatively biased tip is brought close to the TMD surface. By inducing a water bridge between the tip and the TMD surface, controllable oxidation is achieved at the sub-100 nm resolution. The oxidized flake is then submerged into water for selective oxide removal which leads to controllable patterning. In addition, by changing the oxidation time, thickness tunable patterning of multilayer TMDs is demonstrated. This resist-less process results in exposed edges, overcoming a barrier in traditional resist-based lithography and dry etch where polymeric byproduct layers are often formed at the edges. By patterning monolayers into geometric patterns of different dimensions and measuring the effective carrier lifetime, the non-radiative recombination velocity due to edge defects is extracted. Using this patterning technique, it is shown that selenide TMDs exhibit lower edge recombination velocity as compared to sulfide TMDs. The utility of scanning probe lithography towards understanding material-dependent edge recombination losses without significantly normalizing edge behaviors due to heavy defect generation, while allowing for eventual exploration of edge passivation schemes is highlighted, which is of profound interest for nanoscale electronics and optoelectronics.

2D materials↗

DOE OSTI2019

Energetic effects of hybrid organic/inorganic interfacial architecture on nanoporous black silicon photoelectrodes

Photoelectrochemical cells have been the subject of great interest in the research community as a route for fuel formation directly from sunlight. Interfacial layers are frequently employed on the surface of light-absorbing semiconductor photoelectrodes to enhance the activity and stability of the semiconductor. Here we consider the energetic effects of such layers on a nanoporous ‘black’ silicon photocathode. We construct hybrid organic/inorganic films by growing an oxide-nucleating molecular monolayer on the nanostructured Si surface and burying this molecular monolayer under TiO2 deposited by atomic layer deposition. We examine the energetic effects of this hybrid interfacial architecture via our recently developed intensity-modulated high-frequency resistivity (IMHFR) impedance spectroscopy technique and quantify the change in thermodynamic flatband potential as the oxide thickness is increased from 0–15 nm. By comparing the IMHFR data with traditional voltammetry, we are able to deconvolute the thermodynamic and kinetic contributions that determine the observed proton reduction onset potential. We also study these photoelectrodes with Pt nanoparticles either (i) deposited on top of the molecular/TiO 2 interfacial layer or (ii) etched into the Si surface. In the first architecture, a beneficial positive shift in the thermodynamic flatband potential is achieved from the Si|molecular|TiO 2 p-n junction, but the lack of a direct Si|Pt contact results in large kinetic charge transfer losses. In contrast, the second architecture allows for facile charge transfer due to the direct Si|Pt contact but negates any benficial thermodynamic effect of the molecular/TiO 2 bilayer. Despite the lack of thermodynamic effect of the hybrid molecular/TiO 2 interfacial layer, we find that there is still a significant kinetic benefit from this layer. This work demonstrates the sensitive nature of the thermodynamics and kinetics on the interfacial architecture and yields critical insights into the design of photoelectrochemical interfaces.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Mitigation of Pitting on Nitrogen-Doped Niobium Surfaces through Two-Step Electropolishing

Surface processing of niobium superconducting RF cavities used in particle accelerators is crucial for determining their performance. The nitrogen (N)-doping method, developed at Fermilab, enhances the cavities’ quality factor by doping the cavity’s interior surface with N atoms at 800 °C. After N-doping, electropolishing (EP) is employed to remove the niobium nitride phases and attain the desired concentration of interstitial N atoms. This study explores the effects of EP conditions on N-doped niobium samples. The samples were electropolished at 5 to 40 °C and voltages between 3 and 22 V. Different EP voltage ranges produced two types of pits, classified based on their sizes. Larger pits, linked to higher voltages, are also affected by the reaction rate. Pitting could be reduced at a lower temperature and adequate EP voltage. However, to effectively minimize gas evolution forming large-sized pitting, peeling off the top nitride layer before EP might be beneficial. This was achieved through precise low-voltage etching, forming a two-step EP process. The process involves removing the top 100–200 nm layer at a low voltage, followed by standard EP to remove the required material. This two-step EP process effectively mitigated the pitting risk associated with gas evolution on N-doped surfaces.

43 PARTICLE ACCELERATORS↗

DOE OSTI2024

The evolution of model Rh/Fe 3 O 4 (001) catalysts in hydrogen environments

Single metal atoms dispersed on oxides are a new emerging class of catalysts owing to their unique electronic and chemical properties. Here, in this study, we have prepared a series of model single-atom catalysts possessing well-characterized Rh sites that include Rh adatoms (Rh ad ), mixed surface layers with octahedrally-coordinated Rh (Rh oct ), as well as metallic Rh clusters and nanoparticles (Rh met ) on Fe 3 O 4 (001). Using X-ray photoelectron spectroscopy (XPS) and scanning tunneling microscopy (STM), we investigated the activity of such model systems towards H2 and their stability in reducing environments. Our results show that the atomically dispersed Rhad and Rhoct species do not activate H 2 , which would result in the formation of surface hydroxyls on Fe 3 O 4 (001). In contrast, the presence of Rh met in H 2 results in the formation of hydroxyls and subsequent etching of the Fe 3 O 4 (001) at higher temperatures (≥ 500 K) due to water formation via the Mars-van Krevelen mechanism. Additionally, such surface etching leads to the release of the Rh oct from the surface lattice and their sintering to Rh met . To bridge the material gap between the surface science models and high surface area catalysts, we perform parallel studies on powder Rh/Fe 3 O 4 catalysts. The XPS characterization shows remarkable similarities between these systems. Further, our surface science studies provide an atomistic picture of the behavior of high surface area catalysts in the H 2 atmosphere.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2007

Decontamination of Genesis Array Materials by UV Ozone Cleaning

Shortly after the NASA Genesis Mission sample return capsule returned to earth on September 8, 2004, the science team discovered that all nine ultra-pure semiconductor materials were contaminated with a thin molecular organic film approximately 0 to 100 angstroms thick. The organic contaminate layer, possibly a silicone, situated on the surface of the materials is speculated to have formed by condensation of organic matter from spacecraft off-gassing at the Lagrange 1 halo orbit during times of solar exposure. While the valuable solar wind atoms are safely secured directly below this organic contamination and/or native oxide layer in approximately the first 1000 angstroms of the ultra-pure material substrate, some analytical techniques that precisely measure solar wind elemental abundances require the removal of this organic contaminate. In 2005, Genesis science team laboratories began to develop various methods for removing the organic thin film without removing the precious material substrate that contained the solar wind atoms. Stephen Sestak and colleagues at Open University first experimented with ultraviolet radiation ozone (UV/O3) cleaning of several non-flight and flown Genesis silicon wafer fragments under a pure flowing oxygen environment. The UV/O3 technique was able to successfully remove organic contamination without etching into the bulk material substrate. At NASA Johnson Space Center Genesis Curation Laboratory, we have installed an UV/O3 cleaning devise in an ambient air environment to further experimentally test the removal of the organic contamination on Genesis wafer materials. Preliminary results from XPS analysis show that the UV/O3 cleaning instrument is a good non-destructive method for removing carbon contamination from flown Genesis array samples. However, spectroscopic ellipsometry results show little change in the thickness of the surface film. All experiments to date have shown UV/O3 cleaning method to be the best non-destructive method for removing organic contamination from the surface of the Genesis materials. The UV/O3 cleaning process can also clean carbon contamination to levels below non-flight standards. This can be seen by comparing sample 60260's carbon 10667 cps with non-flight Si carbon 21675 cps. Therefore, surface carbon contamination should not hinder the analysis of solar wind.

Calaway, Michael J.↗

DOE OSTI2023

Continuous wave room temperature operation of the 2 $μ$m GaSb-based photonic crystal surface emitting diode lasers

Continuous wave room temperature operation of 2 μm GaSb-based photonic-crystal surface-emitting diode lasers has been realized. The deep etched square mesa devices showed threshold current densities of 500 A/cm 2 at 20 °C. The epi-side down mounted lasers generated above 10 mW of output power in the continuous wave regime and tens of milliwatts in pulses from the 200 × 200 μm 2 aperture. Here, the breakthrough in the device performance parameters was achieved thanks to a highly homogeneous air-pocket retaining epitaxial regrowth process optimized for a specifically designed antimonide diode laser heterostructure. The nanofabrication method utilizing low temperature atomic hydrogen surface cleaning yielded low disorder square lattice of droplet-shaped voids covered by uniform p-cladding layer. The laser emission spectrum as well as near/far field patterns demonstrated peculiar features presumably linked to deformation of the void shape during regrowth and formation of the array of filaments.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

NASA NTRS1993

Visible photoluminescence of porous Si(1-x)Ge(x) obtained by stain etching

We have investigated visible photoluminescence (PL) from thin porous Si(1-x)Ge(x) alloy layers prepared by stain etching of molecular-beam-epitaxy-grown material. Seven samples with nominal Ge fraction x varying from 0.04 to 0.41 were studied at room temperature and 80 K. Samples of bulk stain etched Si and Ge were also investigated. The composition of the porous material was determined using X-ray photoemission spectroscopy and Rutherford backscattering techniques to be considerably more Ge-rich than the starting epitaxial layers. While the luminescence intensity drops significantly with the increasing Ge fraction, we observe no significant variation in the PL wavelength at room temperature. This is clearly in contradiction to the popular model based on quantum confinement in crystalline silicon which predicts that the PL energy should follow the bandgap variation of the starting material. However, our data are consistent with small active units containing only a few Si atoms that are responsible for the light emission. Such units are present in many compounds proposed in the literature as the cause of the visible PL in porous Si.

Ksendzov, A.↗

DOE OSTI2021

Self-assembled multifunctional nanostructures for surface passivation and photon management in silicon photovoltaics

This work reports the fabrication and characterization of multifunctional, nanostructured passivation layers formed using a self-assembly process that provide both surface passivation and improved light trapping in crystalline silicon photovoltaic (PV) cells. Scalable block copolymer self-assembly and vapor phase infiltration processes are used to form arrays of aluminum oxide nanostructures (Al 2 O 3 ) on crystalline silicon without substrate etching. The Al 2 O 3 nanostructures are characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and spectroscopic ellipsometry. Injection-level dependent photoconductance measurements are used to determine the effective carrier lifetime of the samples to confirm the nanostructures successfully passivate the Si surface. Finite element method simulations and reflectance measurement show that the nanostructures increase the internal rear reflectance of the PV cell by suppressing the parasitic optical losses in the metal contact. An optimized morphology of the structures is identified for their potential use in PV cells as multifunctional materials providing surface passivation, photon management, and carrier transport pathways.

14 SOLAR ENERGY↗

DOE OSTI2020

A native oxide high-κ gate dielectric for two-dimensional electronics

Silicon-based transistors are approaching their physical limits and thus new high-mobility semiconductors are sought to replace silicon in the microelectronics industry. Both bulk materials (such as silicon-germanium and III–V semiconductors) and low-dimensional nanomaterials (such as one-dimensional carbon nanotubes and two-dimensional transition metal dichalcogenides) have been explored, but, unlike silicon, which uses silicon dioxide (SiO 2 ) as its gate dielectric, these materials suffer from the absence of a high-quality native oxide as a dielectric counterpart. This can lead to compatibility problems in practical devices. Here, we show that an atomically thin gate dielectric of bismuth selenite (Bi 2 SeO 5 ) can be conformally formed via layer-by-layer oxidization of an underlying high-mobility two-dimensional semiconductor, Bi 2 O 2 Se. Using this native oxide dielectric, high-performance Bi 2 O 2 Se field-effect transistors can be created, as well as inverter circuits that exhibit a large voltage gain (as high as 150). The high dielectric constant (~21) of Bi 2 SeO 5 allows its equivalent oxide thickness to be reduced to 0.9 nm while maintaining a gate leakage lower than thermal SiO 2 . The Bi 2 SeO 5 can also be selectively etched away by a wet chemical method that leaves the mobility of the underlying Bi 2 O 2 Se semiconductor almost unchanged.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Ingeniously enhanced ferromagnetism in chemically-reduced 2D Ti 3 C 2 T X MXene

Chemical reduction is a facile and cost-effective technique for the modulation of the physical and chemical properties of nanomaterials. In this work, we demonstrate an enhancement of the magnetic behavior of Ti 3 C 2 T x MXene after its chemical reduction via l-ascorbic acid treatment. Small ferromagnetic loops have been observed below 50 K for Ti 3 C 2 T x prepared by hydrofluoric acid (HF) etching of Al layers from Ti 3 AlC 2 . Such a ferromagnetic ordering of spins was significantly enhanced via a chemical reduction of Ti 3 C 2 T x with l-ascorbic acid. Ferromagnetic hysteresis loops were observed for reduced Ti 3 C 2 T x (r-Ti 3 C 2 T x ) up to 150 K indicating a significant upshift of the paramagnetic to the ferromagnetic transition temperature, pushing towards room temperature. The enhancement of ferromagnetism and upshift of the ferromagnetic transition temperature could be attributed to the localized unpaired electron in Ti-3d orbital of the r-Ti 3 C 2 T x crystal and increase in the number of unsaturated Ti atoms upon l-ascorbic acid treatment. Chemical reduction via l-ascorbic acid treatment shows a promising pathway towards the modulation and enhancement of magnetism in various MXene materials for the development of 2D metallic soft ferromagnets and spintronic devices.

36 MATERIALS SCIENCE↗

NASA NTRS2004

Web Growth Used to Confine Screw Dislocations to Predetermined Lateral Positions in 4H-SiC Epilayers

Silicon-carbide- (SiC-) based power devices could enable substantial aerospace electronics benefits over today's silicon-based electronics. However, present-day SiC wafers contain electrically harmful dislocations (including micropipes) that are unpredictably distributed in high densities across all commercial 4H- and 6H-SiC wafers. The NASA Glenn Research Center recently demonstrated a crystal growth process that moves SiC wafer dislocations to predetermined lateral positions in epitaxial layers so that they can be reproducibly avoided during subsequent SiC electronic device fabrication. The process starts by reactive ion etching mesa patterns with enclosed trench regions into commercial on-axis (0001) 4H- or 6H-SiC substrates. An example of a pregrowth mesa geometry with six enclosed triangular-shaped trench regions is shown. After the etch mask is stripped, homoepitaxial growth is carried out in pure stepflow conditions that enable thin cantilevers to grow laterally from the tops of mesas whose pregrowth top surfaces are not threaded by substrate screw dislocations. The image in the bottom figure shows the postgrowth structure that forms after the lateral cantilevers expand to coalesce and completely roof over each of the six triangular trench regions. Atomic force microscope (AFM) measurements of the roof revealed that three elementary screw dislocation growth spirals, each shown in the AFM insets of the bottom image on the previous page, formed in the film roof at three respective points of cantilever film coalescence. The image above shows the structure following an etch in molten potassium hydroxide (KOH) that produced surface etch pits at the dislocation defects. The larger KOH etch pits--S1, S2, and S3--shown in this image correspond to screw dislocations relocated to the final points of cantilever coalescence. The smaller KOH etch pits are consistent with epilayer threading edge dislocations from the pregrowth substrate mesa (P1, P3, and P4) and a final cantilever coalescence point (P2). No defects (i.e., no etch pits) are observed in other cantilevered portions of the film surface. On the basis of the principle of dislocation Burgers vector conservation, we hypothesize that all vertically propagating substrate dislocations in an enclosed trench region become combined into a single dislocation in the webbed film roof at the point of final roof coalescence. The point of final roof coalescence, and therefore the lateral location of a webbed roof dislocation, can be designed into the pregrowth mesa pattern. Screw dislocations with predetermined lateral positions can then be used to provide the new growth steps necessary for growing a 4H/6H-SiC epilayer with a lower dislocation density than the substrate. Devices fabricated on top of such films can be positioned to avoid the preplaced dislocations.

Powell, J. Anthony↗

DOE OSTI2019

The Underlying Chemical Mechanism of Selective Chemical Etching in CsPbBr 3 Nanocrystals for Reliably Accessing Near-Unity Emitters

Reliably accessing nanocrystal luminophores with near-unity efficiencies aids in the ability to understand the upper performance limits in optoelectronic applications that require minimal nonradiative losses. Constructing structure-function relationships at the atomic level, while accounting for inevitable defects, allows for the development of robust strategies to achieve near-unity quantum yield luminophores. For CsPbBr 3 perovskite nanocrystals, bromine vacancies leave behind undercoordinated lead atoms that act as traps, limiting the achievable optical performance of the material. Here, we show that selective etching represents a promising path for mitigating the consequences of optical defects in CsPbBr 3 nanocrystals. A mechanistic understanding of the etching reaction is essential for developing strategies to finely control the reaction. We report a study of the selective etching mechanism of CsPbBr3 nanocrystal cubes by controlling the etchant chemical potential. We observe optical absorption and luminescence trajectories while varying the extent and rate of lead removal, removing in some cases up to 75% of the lead from the original nanocrystal ensemble. At modest etchant chemical potentials, the size and shape uniformity of the nanocrystal ensemble improves in addition to the quantum yield, proceeding through a layer-by-layer etching mechanism. Operating with excessively high etchant chemical potentials is detrimental to the overall optical performance as the etching transitions to nonselective, while too low of a chemical potential results in incomplete etching. Through this general approach, we show how to finely control selective etching to consistently access a steady state or chemical stability zone of near-unity quantum yield CsPbBr 3 nanocrystals postsynthetically, suggesting a practical framework to extend this treatment to other perovskite compositions and sizes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Inspection of next-generation EUV resists with nano-projectile secondary ion mass spectrometry

There is a rapidly growing need for new materials for extreme ultraviolet (EUV) lithography, which incorporate high EUV absorbing elements. Hybrid resists, which are a combination of inorganic and organic moieties, are promising as they offer both high EUV sensitivity and high etch resistance. However, there is a glaring lack of methods to examine the uniformity of these important materials at the nanoscale. We examine the capabilities of nano-projectile secondary ion mass spectrometry (NP-SIMS) to investigate hybrid resists. NP-SIMS is a mass spectrometry-based technique with high lateral resolution. Using NP-SIMS, a surface is probed stochastically with a suite of individual projectiles, 10 6 to 10 7 in total, separated in time and space. Examining these individual mass spectra allows for nanoscale investigation of the uniformity of the surface. We evaluated the performance of NP-SIMS using samples of poly(methyl methacrylate) (PMMA) infiltrated with varying amounts of InO x via vapor-phase infiltration (VPI), an organic–inorganic hybridization method derived from atomic layer deposition. Here, we found that NP-SIMS measurements contained abundant characteristic ions related to both the PMMA and infiltrated In. The intensity of In atomic ions increased linearly with the number of infiltration cycles; however, the uniformity of In and PMMA varied with the number of infiltration cycles. After one cycle, we found that both the PMMA and In were relatively inhomogeneous. The homogeneity improved with subsequent infiltration cycles. In addition, NP-SIMS measurements contained characteristic ions related to the infiltration reaction and provided insights into the VPI mechanism. Overall, the results show that NP-SIMS is capable of examining both the inorganic and organic moieties in a hybrid resist and will be an important method for understanding the performance of these materials for use in EUV lithography.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Multiscale and Multimodal Characterization of 2D Titanium Carbonitride MXene

Here, a comprehensive study on the prototype solid solution phase carbonitride MXene Ti 3 CN is conducted using nuclear magnetic resonance, electron spin resonance, total and quasi-elastic neutron scattering, combined with density functional theory-based electronic structure and molecular dynamic calculations. The combination of experiment and theory lead toward rational atomic structural models of Ti 3 CN. The remnant Al ions from the etching process significantly tune the interlayer spacing, distinct from the more typical MXene, Ti 3 C 2 , prepared similarly. Neutron scattering indicates the surface terminations of Ti 3 CN display high oxygen and fluorine concentrations and rather low hydroxyl and hydrogen concentrations. Calculations show that the structure including both the residual Al ions and mixed surface terminations give the best agreement with the measurements. The water molecules in Ti 3 CN are highly immobile, in strong contrast to those in Ti 3 C 2 . The analysis of the electronic structure suggests that the nitride MXene displays higher conductivity than the carbides. Finally, the absence of hydroxyl groups in terminations, the solid-solution in the anion sites, the remnants within layers, and immobile water altogether make the carbonitrides a unique series in the MXene family, implying a further exploration of their exotic properties and applications in energy storage.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Tuning the extent of porosity and composition of N-doped carbon materials by NaNO3 and its effect on electrochemical activity

Highlights: • One-pot method using cheap NaNO{sub 3} as etching agent was developed to tune the porous structure. • NaNO{sub 3} was added into NaCl/ZnCl{sub 2} (NaCl 80 mol%) to form ionothermal salts. • The resultant carbon possesses a 3D hierarchical structure, with more mesopores ratio than micropores. • When NaNO{sub 3} amount is 5% in the salt mixture, the optimal ORR activity was obtained. - Abstract: A facile one-pot method using NaNO{sub 3} as etching agent in a molten salt medium is developed to tune the porous structure and composition of N-doped carbon materials derived from biomass at high temperatures. SEM and TEM analyses reveal that by increasing the amount of NaNO{sub 3}, the structures of the obtained carbons become more open and graphene-like layers are formed. N{sub 2} adsorption/desorption isotherms show that the hierarchical porous structure could be efficiently tuned by adjusting the amount of NaNO{sub 3} in the salt mixture. It is observed that the specific surface area of the as-prepared N-doped carbon using NaNO{sub 3} can reach 1430.1 m{sup 2} g{sup −1}, a much higher value than that of the sample prepared in the absence of NaNO{sub 3}. The micropore ratio decreases with increased amount of NaNO{sub 3}, from 49.42% to 9.98%. Whilst the surface composition of the obtained carbon materials is affected by NaNO{sub 3}. The N content increases and O decreases respectively, by increasing the amount of NaNO{sub 3}. Analysis on the N 1s high resolution reveals that the sum of pyridinic-N and graphitic-N increased, whereas the sum of pyridinic-N oxide and NO{sub x} decreases from NC-0 to NC-0.75. It is also found that the changes of the porous structure and the oxygen-containing groups from NC-0 to NC-0.75 led to changes in hydrophilicity. When the as-prepared carbon materials are used as catalysts for the oxygen reduction reaction, high catalytic activity values are obtained, sample NC-0.5 shows the best performance due to the porous structure and doping effect of N atoms. More importantly, it is concluded that producing N-doped carbon materials from soybean dregs in molten salt medium using NaNO{sub 3} as etching agent could provide a promising approach for the synthesis of opened N-doped carbons of controlled porous structures and large specific surface areas based on biomass precursors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2024

Direct Fabrication of Atomically Defined Pores in MXenes Using Feedback-Driven STEM

Controlled fabrication of nanopores in 2D materials offer the means to create robust membranes needed for ion transport and nanofiltration. Techniques for creating nanopores have relied upon either plasma etching or direct irradiation; however, aberration-corrected scanning transmission electron microscopy (STEM) offers the advantage of combining a sub-Å sized electron beam for atomic manipulation along with atomic resolution imaging. Here, for this work, a method for automated nanopore fabrication is utilized with real-time atomic visualization to enhance the mechanistic understanding of beam-induced transformations. Additionally, an electron beam simulation technique, Electron-Beam Simulator (E-BeamSim) is developed to observe the atomic movements and interactions resulting from electron beam irradiation. Using the MXene Ti 3 C 2 T x , the influence of temperature on nanopore fabrication is explored by tracking atomic transformations and find that at room temperature the electron beam irradiation induces random displacement and results in titanium pileups at the nanopore edge, which is confirmed by E-BeamSim. At elevated temperatures, after removal of the surface functional groups and with the increased mobility of atoms results in atomic transformations that lead to the selective removal of atoms layer by layer. This work can lead to the development of defect engineering techniques within functionalized MXene layers and other 2D materials.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Enhancement to the conductivity of surface transfer-doped (111) diamond through thermochemical surface etching

The use of a transition metal catalyzed thermochemical etching method for improving the carrier transport properties of the near-surface two-dimensional (2D) hole gas in surface transfer-doped hydrogen-terminated (111) diamond is demonstrated. Using Ni 0.8 Cr 0.2 films deposited and annealed to a temperature of 900 °C, with up to three etch cycles, preferential (111) surface etching produces large terraces exceeding 10 μm in size with a surface microroughness, σ 2 RMS λ, that is two orders of magnitude lower than for the pre-etched (111) surface. Magnetotransport measurements on hydrogen-terminated Hall bars engineered on the pre- and post-etched surfaces and rendered conductive by the adsorbed water layer formed on exposure to ambient conditions demonstrate that this etching causes an improvement in the hole mobility by an order of magnitude, resulting in a measured sheet resistivity of 1.04 kΩ/sq at a temperature of 4.2 K without gating.

42 ENGINEERING↗