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DOE OSTI2021

Optimization of the Growth of the Van der Waals Materials Bi 2 Se 3 and (Bi 0.5 In 0.5 ) 2 Se 3 by Molecular Beam Epitaxy

The naturally existing chalcogenide Bi 2 Se 3 is topologically nontrivial due to the band inversion caused by the strong spin-orbit coupling inside the bulk of the material. Here, the surface states are spin polarized, protected by the time-inversion symmetry, and thus robust to the scattering caused by nonmagnetic defects. A high-purity topological insulator thin film can be easily grown via molecular beam epitaxy (MBE) on various substrates to enable novel electronics, optics, and spintronics applications. However, the unique surface state properties have historically been limited by the film quality, which is evaluated by crystallinity, surface morphology, and transport data. Here we propose and investigate different MBE growth strategies to improve the quality of Bi 2 Se 3 thin films grown by MBE. Based on the surface passivation status, we have classified the substrates into two categories, self-passivated or unpassivated, and determine the optimal growth mechanisms on the representative sapphire and GaAs, respectively. For Bi 2 Se 3 on GaAs, the surface passivation status determines the dominant growth mechanism. In the end, growths of the topological trivial insulator (Bi 0.5 In 0.5 ) 2 Se 3 (BIS) on GaAs are investigated following the protocols proposed.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Pulsed laser deposition of niobium nitride thin films

Niobium nitride (NbN{sub x}) films were grown on Nb and Si(100) substrates using pulsed laser deposition. NbN{sub x} films were deposited on Nb substrates using PLD with a Q-switched Nd:YAG laser (λ = 1064 nm, ∼40 ns pulse width, and 10 Hz repetition rate) at different laser fluences, nitrogen background pressures and deposition substrate temperatures. When all the fabrication parameters are fixed, except for the laser fluence, the surface roughness, nitrogen content, and grain size increase with increasing laser fluence. Increasing nitrogen background pressure leads to a change in the phase structure of the NbN{sub x} films from mixed β-Nb{sub 2}N and cubic δ-NbN phases to single hexagonal β-Nb{sub 2}N. The substrate temperature affects the preferred orientation of the crystal structure. The structural and electronic, properties of NbN{sub x} deposited on Si(100) were also investigated. The NbN{sub x} films exhibited a cubic δ-NbN with a strong (111) orientation. A correlation between surface morphology, electronic, and superconducting properties was found. The observations establish guidelines for adjusting the deposition parameters to achieve the desired NbN{sub x} film morphology and phase.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2018

Optimization of electrical treatment strategy for surface roughness reduction in conducting thin films

The surface roughness of deposited conducting thin films is responsible for various materials reliability problems in nanoelectronics and nanofabrication technologies. In this work, we report a modeling and simulation study that aims at optimizing the electrical surface treatment of deposited conducting thin films as a physical processing strategy for their surface roughness reduction. Our research is based on a continuum model of film surface morphological evolution that accounts for the residual stress in the deposited conducting thin film, the film’s wetting of the substrate layer that it is deposited on, film texture and surface diffusional anisotropy, and surface electromigration. Through systematic linear stability analysis and dynamical simulation protocols, we examine in detail the effects of film surface crystallographic orientation and applied electric field direction toward minimizing the electric field strength required for film surface smoothening. We believe that the critical electric field strength requirement for surface roughness reduction on {110}, {100}, and {111} surfaces of face-centered cubic crystalline conducting thin films exhibits a very strong dependence on the applied electric field direction, expressed as the electric field misalignment with respect to the principal residual stress directions in the film and the fast surface diffusion directions. Due to these findings, we optimize the electrical treatment strategy for surface roughness reduction of conducting thin films with respect to all relevant processing and material parameters.

42 ENGINEERING↗

DOE OSTI2018

In situ characterization of the deposition of anatase TiO2 on rutile TiO2(110)

Growing additional TiO2 thin films on TiO2 substrates in ultrahigh vacuum (UHV)-compatible chambers have many applications for sample preparation, such as smoothing surface morphologies, templating, and covering impurities. However, there has been little study into how to control the morphology of TiO2 films deposited onto TiO2 substrates, especially using atomic layer deposition (ALD) precursors. Here, the authors show the growth of a TiO2 film on a rutile TiO2(110) surface using titanium tetraisopropoxide (TTIP) and water as the precursors at pressures well below those used in common ALD reactors. X-ray absorption spectroscopy suggests that the relatively low sample temperature (175 °C) results in an anatase film despite the rutile template of the substrate. Using ambient pressure x-ray photoelectron spectroscopy, the adsorption of TTIP was found to be self-limiting, even at room temperature. No molecular water was found to adsorb on the surface. The deposited thickness suggests that an alternate chemical vapor deposition growth mechanism may be dominating the growth process. This study highlights the possibility that metal oxide film deposition from molecular precursors is an option for sample preparations in common UHV-compatible chambers.

Head, Ashley R.↗

DOE OSTI2013

Phase transformations during the Ag-In plating and bonding of vertical diode elements of multijunction solar cells

The conditions of the bonding of silicon multijunction solar cells with vertical p-n junctions using Ag-In solder are studied. The compositions of electrodeposited indium films on silicon wafers silver plated by screen printing and silver and indium films fabricated by layer-by-layer electrochemical deposition onto the surface of silicon vertical diode cells silver plated in vacuum are studied. Studying the electrochemical-deposition conditions, structure, and surface morphology of the grown layers showed that guaranteed bonding is provided by 8-min heat treatment at 400 Degree-Sign C under the pressure of a stack of metallized silicon wafers; however, the ratio of the indium and silver layer thicknesses should not exceed 1: 3. As this condition is satisfied, the solder after wafer bonding has the InAg{sub 3} structure (or InAg{sub 3} with an Ag phase admixture), due to which the junction melting point exceeds 700 Degree-Sign C, which guarantees the functioning of such solar cells under concentrated illumination.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Singularities of Silicon Surface Nanostructuring due to Ultrafast Heating in Water by a Femtosecond Laser Pulse

Silicon surface morphology induced by a femtosecond laser pulse at near-threshold fluences in water environment is investigated by means of atomic-force microscopy (AFM). With increasing fluence, the silicon surface transforms into nanoscale ring-shaped and blister structures, as well as smooth and nanostructured microcraters with a minimum depth of 1 nm. The formation of starlike patterns imprinted at the surface of microcraters at fluences above the ablation threshold is observed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2016

Effect of surface nanostructuring on corrosion behavior of Ti–6Al–4V alloy

Surface nanostructure was induced in Ti–6Al–4V alloy by ultrasonic shot peening (USSP) for different durations, from 15 s to 30 min, and the modified surface was characterized by optical, scanning, atomic force and transmission electron microscopy. Nano size grains were observed to form on surface of the USSPed samples and surface roughness was increased with duration of USSP. Polarization study was carried out in Ringer's solution to examine the effect of surface nanostructuring on corrosion resistance of this alloy. Electrochemical corrosion was carried out for all the USSPed specimens as well as the non-USSPed sample in Ringer's solution. Surface morphology of the corroded samples was examined by SEM. In general, corrosion resistance was improved by USSP up to the duration of 15 min and there was maximum improvement in the specimen USSPed for 1 min. However, corrosion resistance was drastically reduced due to USSP for long duration of 30 min. - Highlights: •Nanostructure was induced by USSP on alloy Ti–6Al–4V of about 28 nm. •Grain refinement was confirmed by XRD and TEM. •USSP is an effective technique for the improvement in corrosion resistance. •Nanostructured surface promotes formation of protective surface layer of TiO{sub 2}.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Structural, morphological and electrical studies of lithium ion irradiated sodium potassium niobate single crystal grown by flux method

Single crystals of sodium potassium niobate (K{sub 0.5}Na{sub 0.5})NbO{sub 3} (KNN) were grown by flux method and crystals were irradiated with 45 MeV Li ions to modify the electrical properties. Energy of the irradiated heavy ion was lower than the threshold energy to produce columnar defect and only clusters of defect was observed. The surface morphology of the irradiated single crystals was studied using scanning electron microscope (SEM) and atomic force microscope (AFM). The results show that the surface roughness value was found to increase with increasing fluence.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Deciphering supramolecular and polymer-like behavior in metallogels: real-time insights into temperature-modulated gelation and rapid self-assembly dynamics

Bis(pyridyl) urea-based gelators, namely L2 and its isomeric mixture ( L1 + L2 ), are known to self-assemble into 1D architectures capable of inducing supramolecular gelation. Coordination with metal ions such as Ag( I ), Cu( II ), and Fe( III ) introduces structural reinforcement, enabling the formation of distinct 3D networks governed by metal-specific coordination geometries. Here, we present a comprehensive investigation into the temperature-responsive behavior (20–60 °C) of L2 and L1 + L2 , both in the absence and presence of Ag( I ), Dy( III ), Fe( III ), Cu( II ), and Ho( III ), using real-time small-angle neutron scattering (SANS). To probe long-term structural evolution/kinetics of self-assembly, real-time small-angle X-ray scattering (SAXS) was employed on L2 + Ag gels, complemented by differential scanning calorimetry (DSC) to evaluate thermal transitions. Our results reveal strikingly divergent gelation behaviors: L2 forms a highly rigid, covalent polymer-like network, while L1 + L2 exhibits remarkable thermal adaptability. Upon metal coordination, the assemblies exhibit pronounced crystallinity and exceptional thermal stability, as evidenced by persistent Bragg reflections and invariant d-spacings. Intriguingly, L2 : Fe (2 : 1) and L1 : L2 : Fe (0.5 : 0.5 : 1) in acetonitrile-d 3 (ACN-d 3 ) deviate from this trend, forming thermally labile amorphous gels. These systems show a complete loss of crystalline order, reduced Porod exponents—indicative of collapsed or branched fiber morphologies—and prominent melting and glass transition events in DSC. Fitting SANS and SAXS data to the correlation length model unveiled insightful nanostructural features. While most systems displayed minimal temperature-induced variation in mesh size or surface morphology, L2 : Ag in dimethyl sulfoxide-d 6 (DMSO-d 6 )/D 2 O and L2 : Fe (1 : 1) in ACN-d 3 exhibited a rare combination of thermally stable correlation lengths and increasing high- q exponents—strongly suggesting progressive fiber densification or surface smoothing within a robust gel framework. These findings highlight the tunability and structural resilience of supramolecular gels through precise control of ligand architecture, metal coordination, and temperature, offering valuable design principles for functional soft materials.

Pajoubpong, Jinnipha [Univ. of Cincinnati, OH (Uni↗

DOE OSTI2012

Electronic absorption band broadening and surface roughening of phthalocyanine double layers by saturated solvent vapor treatment

Variations in the electronic absorption (EA) and surface morphology of three types of phthalocyanine (Pc) thin film systems, i.e. copper phthalocyanine (CuPc) single layer, zinc phthalocyanine (ZnPc) single layer, and ZnPc on CuPc (CuPc/ZnPc) double layer film, treated with saturated acetone vapor were investigated. For the treated CuPc single layer film, the surface roughness slightly increased and bundles of nanorods were formed, while the EA varied little. In contrast, for the ZnPc single layer film, the relatively high solubility of ZnPc led to a considerable shift in the absorption bands as well as a large increase in the surface roughness and formation of long and wide nano-beams, indicating a part of the ZnPc molecules dissolved in acetone, which altered their molecular stacking. For the CuPc/ZnPc film, the saturated acetone vapor treatment resulted in morphological changes in mainly the upper ZnPc layer due to the significantly low solubility of the underlying CuPc layer. The treatment also broadened the EA band, which involved a combination of unchanged CuPc and changed ZnPc absorption.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Improving qubit coherence time through detailed materials analysis

This study investigates the defects, imperfections, and variations in superconducting Nb thin films deposited on sapphire substrates. Two samples, W114 and W118, were fabricated using DC Magnetron Sputtering and Electron Cyclotron Resonance (ECR), respectively. Each sample was analyzed at five distinct spots to compare elemental homogeneity and thickness variations. Scanning Electron Microscopy (SEM) was employed to examine surface morphology, while Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Photoelectron Spectroscopy (XPS) provided elemental and chemical state analyses. SEM revealed distinct structures in W114 and a uniform surface in W118. EDS showed higher aluminum and oxygen signals in W118, indicating a thicker film. XPS detected a higher Nb₂O₅ signal in W118, attributed to a thicker oxygen layer. These findings highlight the critical role of precise material characterization in advancing quantum computing technologies.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

NASA NTRS1985

Characteristics of Basaltic Lava Flows on Venus

Some ideas relating to the formation of lava flows on Venus are reviewed. The surface morphological features seen in the panoramic images made by the Venera 13 and 14 landers are examined in detail. The major element compositions measured by the Soviet probes indicate that the surface rocks at the Venera 13 site resemble a terrestrial tholeite composite whereas the Venera 14 rocks are similar to terrestrial alkali basalts. Few data exist on the rheological properties of such magma types on Earth; these properties are a strong function of magma volatile content, and there are important gaps in our knowledge of the typical volatiles to be associated with the magmas on Venus. However, the suggestion that Venusian magmas may be water poor together with consideration of the fact that the high Venusian surface temperatures may cause magmas to experience up to 50 K less cooling during their rise to the surface than corresponding terrestrial counterparts, leads to the finding that Venusian magmas may typically have plastic viscosities, E, up to a factor of three greater than terrestrial counterparts on eruption. A similar analysis of yield strength variations with temperature, magma composition and volatile content suggests that temperature will exert the main control and that Venusian magma yield strengths, Y, may be a factor of several times smaller than those of terrestrial equivalents.

Wilson, L.↗

NASA NTRS2013

Design of a Uranium Dioxide Spheroidization System

The plasma spheroidization system (PSS) is the first process in the development of tungsten-uranium dioxide (W-UO2) fuel cermets. The PSS process improves particle spherocity and surface morphology for coating by chemical vapor deposition (CVD) process. Angular fully dense particles melt in an argon-hydrogen plasma jet at between 32-36 kW, and become spherical due to surface tension. Surrogate CeO2 powder was used in place of UO2 for system and process parameter development. Particles range in size from 100 - 50 microns in diameter. Student s t-test and hypothesis testing of two proportions statistical methods were applied to characterize and compare the spherocity of pre and post process powders. Particle spherocity was determined by irregularity parameter. Processed powders show great than 800% increase in the number of spherical particles over the stock powder with the mean spherocity only mildly improved. It is recommended that powders be processed two-three times in order to reach the desired spherocity, and that process parameters be optimized for a more narrow particles size range. Keywords: spherocity, spheroidization, plasma, uranium-dioxide, cermet, nuclear, propulsion

Cavender, Daniel P.↗

DOE OSTI2016

Investigation of the Effects of Hydrogen Atoms Concentration on the Tungsten Sigma 5 (310) Symmetric Tilt Grain Boundary Strength

Recently, strict policies are being made by several government agencies, environmentalists, and some people against the usage of fossil fuels as the source of energy generation. Not only because its supply does not meet the booming human population all around the world but also it is not pollution-free; just to mention a few. These setbacks attached to fossil fuels make nuclear fusion energy an important means of energy generation; it is characterized with clean and easy means of energy generation compared to other methods of power production such as hydropower and solar power. The success of fusion power depends on the design of modern fusion materials and the selection of the plasma facing materials (PFMs). ITER and Demonstration Power plant (DEMO) considered Tungsten (W) as part of their PFMs. W is the most preferred plasma facing material (PFM) for the future nuclear fusion reactors such as in the proposed DEMO and ITER- which is at the moment the largest Tokamak nuclear fusion reactor under construction in the world. Tungsten has excellent thermal properties, low-sputtering yield, and high melting point. Hydrogen (H) atoms have an affinity for tungsten grain boundary, and are trapped there permanently. In addition, it makes W prone to failure. In a fusion environment, W is exposed to extremely high fluences of H isotopes and irradiation. The low-energy H isotopes will be retained in the tungsten material leading to the formation of blisters in W and cause degradation of the mechanical and thermal properties of W. For safety reason, the effect of hydrogen atoms concentration at the tungsten S5 (310) grain boundary (GB) needs to be investigated and it will aid in better designing of fusion wall materials. Σ5 (310) is considered in this work because it is one of the most important and dominant GBs in the atomic distribution of materials. GBs affect the strength of W as well. The GBs with superior properties can be increased in the atomic distribution of W relative to others in order to achieve high overall material properties. GBs play a role in determining the properties of materials such as the thermal and electrical conductivity of a material. The crystallography description of the Σ5 (310) grain boundary comprises of Σ, tilt type- symmetric, crystallographic direction [001] and the GB plane. The Σ is related to the coincidence site lattice (CSL) model, which denotes that in a certain orientation between two grains, there are numbers of points where the atoms coincide. For the case of Σ5 (310), the misorientation between the two crystals is 36.9 degree along [001] direction and the GB plane is (310). GB properties differ as result of different sigma values and Σ is the reciprocal of CSL. Thus, Σ5 GB has 1/5 of the atoms in coincident sites. For the case of a tilt boundary, the lattice vector is embedded in the GB plane. Also for a tilt-symmetric GB, the grains directions are mirrored against the GB plane. The classic molecular dynamics method (MD) is an accurate numerical approach that adopts Newton's equation of motion to get atoms trajectories.Studies have been carried out on atomistic simulation of tungsten.The effect of H on GB migration in W was studied by using molecular dynamics simulation and it was discovered that H prevents the GB migration at different H concentrations and temperatures. Others investigated the migration, dissolution and trapping of H in W using MD and first principles method. Atomistic simulations have been used to predict the GB energy in Fe and Mo using embedded atom method (EAM) and it was concluded that the GB energies in the metals are affected more by the orientation of the GB plane than by the misorientation of the lattice. Study was done on symmetric and asymmetric tilt grain boundaries in Cu and Al using MD method and the GB structures and energies were established; EAM was adopted as well. The formation of hydrogen blisters and cracking processes for various tungsten materials were investigated and it was observed that, dopants increase the number of blisters and exfoliations for both stress relieved and recrystallized W. Investigation was carried out on the surface morphology changes in W caused by plasmas heat and particle loadings and their effects on material degradation in ITER. In addition, the study of interactions between low energetic hydrogen and tungsten surface was carried out using molecular dynamics simulations with analytical bond order potential (ABOP) and the results addressed irradiation damage in tungsten. Mechanism of blister formation on W surface was studied using experimental approach and it was observed that the amount of blisters formed depends on the beam fluence. This work investigates the effect of hydrogen atom concentrations at the W Σ5 (310) tilt-symmetric GB on the grain boundary energy and the GB pulling force. (authors)

36 MATERIALS SCIENCE↗

DOE OSTI2024

Improving Qubit Coherence Time Through Detailed Materials Analysis

This study investigates the defects, imperfections, and variations in Nb thin films deposited on sapphire substrates. Two samples, W114 and W118, were fabricated using DC Magnetron Sputtering and Electron Cyclotron Resonance (ECR), respectively. Each sample was analyzed at five distinct spots to compare elemental homogeneity and variations in oxide layers. Scanning Electron Microscopy (SEM) was employed to examine surface morphology, while Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Photoelectron Spectroscopy (XPS) provided elemental and chemical state analyses. SEM revealed distinct structures in W114 and a uniform surface in W118. EDS showed higher aluminum signals in W118, indicating a thinner film in comparison to W114. XPS detected a higher Nb₂O₅ signal in W118, in comparison to W114, which can be attributed to the presence of a thicker Nb₂O₅ layer in W118. These findings highlight the critical role of precise material characterization in advancing quantum computing technologies.

Rosado Bonilla, Cristy M.↗

DOE OSTI2014

Ferroelectric field effect of the bulk heterojunction in polymer solar cells

A ferroelectric field effect in the bulk heterojunction was found when an external electric field (EEF) was applied on the active layer of polymer solar cells (PSCs) during the annealing process of the active layer spin-coated with poly(3-hexylthiophene):[6,6]-phenyl-C{sub 61} butyric acid methyl ester. For one direction field, the short circuit current density of PSCs was improved from 7.2 to 8.0 mA/cm{sup 2}, the power conversion efficiency increased from 2.4% to 2.8%, and the incident photon-to-current conversion efficiency increased from 42% to 49% corresponding to the different EEF magnitude. For an opposite direction field, the applied EEF brought a minus effect on the performance mentioned above. EEF treatment can orientate molecular ordering of the polymer, and change the morphology of the active layer. The authors suggest a explanation that the ferroelectric field has been built in the active layer, and therefore it plays a key role in PSCs system. A needle-like surface morphology of the active film was also discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Optical properties of (Se{sub 80}Te{sub 20}){sub 100−x}Ag{sub x} (0 ≤ x ≤ 4) thin films

Thin films of (Se{sub 80}Te{sub 20}){sub 100−x}Ag{sub x} (0 ≤ x ≤ 4) glasses were prepared by thermal evaporation of the bulk samples. The transmittance (T) and reflection (R) spectra of amorphous thin films were obtained in the spectral region in the range 400–2500 nm. The optical band gap (E{sub g}) has been determined by Tauc’s extrapolation method. The surface morphology has been determined by the Scanning Electron Microscopy (SEM)

36 MATERIALS SCIENCE↗

DOE OSTI2011

III-V Nanowire Array Growth by Selective Area Epitaxy

III-V semiconductor nanowires are unique material phase due to their high aspect ratio, large surface area, and strong quantum confinement. This affords the opportunity to control charge transport and optical properties for electrical and photonic applications. Nanoscale selective area metalorganic chemical vapor deposition growth (NS-SAG) is a promising technique to maximize control of nanowire diameter and position, which are essential for device application. In this work, InP and GaAs nanowire arrays are grown by NS-SAG. We observe enhanced sidewall growth and array uniformity disorder in high growth rate condition. Disorder in surface morphology and array uniformity of InP nanowire array is explained by enhanced growth on the sidewall and stacking faults. We also find that AsH{sub 3} decomposition on the sidewall affects the growth behavior of GaAs nanowire arrays.

36 MATERIALS SCIENCE↗