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DOE OSTI2018

In-situ packaging ultra-uniform 3D hematite nanotubes by polyaniline and their improved gas sensing properties

Highlights: • Ultra-uniform 3D α-Fe{sub 2}O{sub 3} nanotubes were packaged by PANI through the two-stage solution processes. • PANI/α-Fe{sub 2}O{sub 3}-based sensor could detect low concentration of acetone (1 ppm) at lower temperature of 180 °C. • The unique structure of α-Fe{sub 2}O{sub 3} support and its synergetic effect with PANI layers improved the sensor performances. - Abstract: This paper reports the PANI (polyaniline)-packaged three-dimensional (3D) α-Fe{sub 2}O{sub 3} nanotubes P/N heterojunction, which was constructed successfully though a facile hydrothermal reaction without adding any surfactant followed by in-situ chemical polymerization in the liquid phase. The structure and morphology of the products were characterized by means of FESEM, XRD, TEM & HRTEM, TGA and FT-IR. Gas sensing test results found that, the PANI/α-Fe{sub 2}O{sub 3} nanocomposite sensor exhibited obviously higher response, lower working temperature (180 °C), fast response and recovery speeds, good selectivity and excellent stability to acetone gas, indicating its promising application for high-performance acetone sensors. The enhanced gas sensing performances can be attributed to the factors like ultra-uniform 3D nanotube-like structure for α-Fe{sub 2}O{sub 3}, the noticeable advantages of PANI, as well as the construction of heterojunction barrier at their interface. The as-prepared PANI/α-Fe{sub 2}O{sub 3} nanocomposite may be also applied in other areas like photocatalysis, water purification, ion batteries, optical devices, and so on.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2016

Effects of Cd Diffusion and Doping in High-Performance Perovskite Solar Cells Using CdS as Electron Transport Layer

Perovskite solar cells with stabilized power conversion efficiency exceeding 15% have been achieved, using a methylammonium lead iodide (MAPbI 3 ) absorber and CdS as the electron transport layer. X-ray photoelectron spectroscopy reveals a small presence of Cd at the surface of most perovskite films fabricated on CdS. In this work, perovskite films were deliberately doped with Cd to understand the possible impacts of Cd diffusion into the perovskite absorber layer. Doping substantially increases the grain size of the perovskite films but also reduces device performance through the formation of an electrical barrier, as inferred by the S-shape of their $J–V$ curves. Time-resolved photoluminescence measurements of the doped films do not indicate substantial nonradiative recombination due to bulk defects, but a secondary phase is evident in these films, which experiments have revealed to be the organic–inorganic hybrid material methylammonium cadmium iodide, (CH 3 NH 3 ) 2 CdI 4 . It is further demonstrated that this compound can form via the reaction of CdS with methylammonium iodide and may form as a competing phase during deposition of the perovskite. Buildup of this insulating compound may act as an electrical barrier at perovskite interfaces, accounting for the drop in device performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Nonmetal to Metal Transition and Ultrafast Charge Carrier Dynamics of Zn Clusters on p-Si(100) by fs-XUV Photoemission Spectroscopy

Understanding the electronic structure and charge carrier dynamics of supported clusters is important due to their many potential applications in photochemistry and catalysis. In this investigation, photoemission spectroscopy, in conjunction with femtosecond extreme ultraviolet (XUV) laser pulses, is used to investigate the electronic structure and ultrafast charge carrier dynamics at a Si(100) surface decorated with Zn clusters. Static photoemission spectroscopy is used to investigate the changes in the electronic structure as the dimensionality of the Zn is increased from small clusters composed of a very few atoms to metallic Zn particles. Furthermore, femtosecond optical-pump XUV-probe photoemission spectroscopy is employed to induce a charge transfer from the p-Si(100) substrate to the Zn clusters and to measure in real time the charge trapping at the Zn cluster as well as the subsequent charge relaxation. The ultrafast charge carrier dynamics are also investigated for small clusters and metallic Zn particles. Significant transient charging of the Zn clusters after excitation of the Si(100) substrate by 800 nm light is observed for Zn coverages greater than 0.12 ML Zn, which coincides with the formation of a Schottky barrier at the interface between the Zn particle and the p-Si(100) substrate. The transient signals show that the charge trapping time at the Zn cluster varies with the cluster size, which is rationalized based on the electronic structure of the cluster as well as the band energy alignment at the Zn cluster-Si(100) junction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Mechanism of the Accelerated Water Formation Reaction under Interfacial Confinement

Subnanoscale spaces at the interface between weakly coupled thin films and their metal supports offer exciting opportunities for studying chemical reactions under confinement. Here, we investigated the kinetics of water formation (from hydrogen and chemisorbed oxygen) in the confined space at the interface between bilayer (BL) silica and a Ru(0001) support, compared to the reaction on the bare Ru(0001) surface. Ambient pressure X-ray photoelectron spectroscopy (AP-XPS) experiments were carried out at different temperatures at elevated pressures of H 2 to follow the reaction kinetics. The apparent activation energy at the BL-silica/Ru(0001) interface was found to be 0.38 eV lower than that on bare Ru(0001), consistent with a recent report by Prieto et al. (Angew. Chem., Int. Ed.2018, 57(28), 8749–8753) carried out at lower H 2 pressures using low-energy electron microscopy. Density functional theory calculations revealed that the rate-limiting step in the direct hydrogenation pathway on the Ru(0001) surface is the first hydrogen addition step (*H + *O ↔ *OH). The confinement at the BL-silica/Ru(0001) interface only marginally affects the energy barrier of the first hydrogen addition. Instead, it activates an alternative disproportionation reaction pathway (*H 2 O + *O ↔ 2*OH). On the bare Ru(0001) surface, the disproportionation pathway can only occur at cryogenic temperatures or under high water vapor pressures. However, the presence of the BL-silica increases the desorption barrier for water molecules at the interface. The increased residence time allows trapped water molecules to react with chemisorbed oxygen to produce two *OH per H 2 O with an activation energy 0.25 eV lower than that of the first hydrogen addition step. Finally, this work reveals the origin of the observed accelerated water formation reaction at the BL-silica/Ru(0001) interface in the low-temperature regime (T < 350 K) and points to a route to engineer chemical reaction pathways by leveraging subnanoscale confined spaces at metal–oxide interfaces.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Merged-Element Transmon

Transmon qubits are ubiquitous in the pursuit of quantum computing using superconducting circuits. However, they have some drawbacks that still need to be addressed. Most importantly, the scalability of transmons is limited by the large device footprint needed to reduce the participation of the lossy capacitive parts of the circuit. In this work, we investigate and evaluate losses in an alternative device geometry, namely, the merged-element transmon (mergemon). To this end, we replace the large external shunt capacitor of a traditional transmon with the intrinsic capacitance of a Josephson junction and achieve an approximately 100 times reduction in qubit dimensions. We report the implementation of the mergemon using a sputtered Nb–amorphous-Si–Nb trilayer film. In an experiment below 10 mK, the frequency of the readout resonator, capacitively coupled to the mergemon, exhibits a qubit-state-dependent shift in the low-power regime. The device also demonstrates the single-photon and multiphoton transitions that represent a weakly anharmonic system in two-tone spectroscopy. The transition spectra are explained well with master-equation simulations. Here, a participation-ratio analysis identifies the dielectric loss of the amorphous-Si tunnel barrier and its interfaces as the dominant source for qubit relaxation. We expect the mergemon to achieve high coherence for relatively small device dimensions when implemented with a low-loss, epitaxially grown, and lattice-matched trilayer.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

Evaluation of soil manipulation to prepare engineered earthen waste covers for revegetation

Seven ripping treatments designed to improve soil physical conditions for revegetation were compared on a test pad simulating an earthen cover for a waste disposal cell. The field test was part of study of methods to convert compacted-soil waste covers into evapotranspiration covers. The test pad consisted of a compacted layer of fine-textured soil simulating a barrier protection layer overlain by a gravelly sand bedding layer and a cobble armor layer. Treatments included combinations of soil-ripping implements (conventional shank [CS], wing-tipped shank [WTS], and parabolic oscillating shank with wings [POS]), ripping depths, and number of passes. Dimensions, dry density, moisture content, and particle size distribution of disturbance zones were determined in two trenches excavated across rip rows. The goal was to create a root-zone dry density between 1.2 and 1.6 Mg m-3 and a seedbed soil texture ranging from clay loam to sandy loam with low rock content. All treatments created V-shaped disturbance zones as measured on trench faces. Disturbance zone size was most influenced by ripping depth. Winged implements created larger disturbance zones. All treatments lifted fines into the bedding layer, moved gravel and cobble down into the fine-textured protection layer, and thereby disrupted the capillary barrier at the interface. Changes in dry density within disturbance zones were comparable for the CS and WTS treatments but were highly variable among POS treatments. Water content increased in the bedding layer and decreased in the protection layer after ripping. The POS at 1.2-m depth and two passes created the largest zone with a low dry density (1.24 Mg m-3) and the most favorable seedbed soil texture (gravely silt loam). Furthermore, ripping also created large soil aggregates and voids in the protection layer that may produce preferential flow paths and reduce water storage capacity.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1981

Degradation of a two-layer thermal barrier coating under thermal cycling

A two-layer plasma-sprayed thermal barrier coating on a directionally solidified nickel-base eutectic alloy substrate was characterized prior to and after thermal cycling to 1095 C in an accelerated furnace test. The coating was comprised of an inner layer of Ni-16.4Cr-5.1Al-0.15Y (wt%) bond coat and an outer layer of ZrO2-7.9Y2O3 (wt%) thermal barrier. Characterization of the bond coat revealed that substantial amounts of yttrium and aluminum were oxidized during plasma-spraying in air. The oxidation of these elements reduced the protective capacity of the bond coat so that, on thermal exposure, severe degradation of the bond coat resulted and large amounts of nickel oxide formed. This nickel oxide was demonstrated to grow outward into the thermal barrier, which appears to have increased the stresses in the thermal barrier and contributed to its failure near the thermal barrier-bond coat interface.

Maier, R. D.↗

NASA NTRS1989

High temperature creep behavior of single crystal gamma prime and gamma alloys

The creep behavior of single crystals of gamma-prime and gamma alloys were investigated and compared to the response of two-phase superalloys tested previously. High temperature deformation in the gamma alloys was characteristic of a climb-controlled mechanism, whereas the gamma-prime based materials exhibited glide-controlled creep behavior. The superalloys were much more creep resistant than their constituent phases, which indicates the importance of the gamma/gamma-prime interface as a barrier for dislocation motion during creep.

Nathal, M. V.↗

NASA NTRS1991

Fracture of single crystals of the nickel-base superalloy PWA 1480E in helium at 22 C

The fracture behavior and deformation of He-charged (at 22 C) single crystals of PWA 1480E Ni-base superalloy were investigated using SEM and TEM techniques to observe the behavior of tensile fractures in notched single crystals with seven different crystal growth orientations: 100-line, 110-line, 111-line, 013-line, 112-line, 123-line, and 223-line. To identify the cleavage plane orientation, a stereoscopic technique, combined with the use of planar gamma-prime morphologies, was applied. It was found that gamma-prime particles were orderly and closely aligned with edges along the 100-line, 010-line, and 001-line-oriented directions of the gamma matrix. Different crystal growth orientations were found not to affect the morphology of gamma-prime particles. The accumulation of dislocations around gamma/gamma-prime interfaces formed strong barriers to subsequent dislocation movement and was the primary strengthening mechanism at room temperature.

Chen, P. S.↗

NASA NTRS1992

Role of interfacial thermal barrier in the transverse thermal conductivity of uniaxial SiC fiber-reinforced reaction bonded silicon nitride

The transverse thermal conductivity of reaction-bonded Si3N4 is significantly affected by an interfacial barrier at the interface formed with SiC reinforcing fibers. A comparative study of composites with and without reinforcing-fiber carbon coatings found the coating to reduce effective thermal conductivity by a factor of about 2; this, however, is partially due to a thermal expansion-mismatch gap between fiber and matrix. HIPing of composites with coated fibers led to an enhancement of thermal conductivity via improved interfacial thermal contact and greater grain size and crystallinity of the fibers.

Bhatt, H.↗

DOE OSTI2014

Enhanced Cover Assessment Project:Soil Manipulation and Revegetation Tests

The U.S. Department of Energy Office of Legacy Management is evaluating methods to enhance natural changes that are essentially converting conventional disposal cell covers for uranium mill tailings into water balance covers. Conventional covers rely on a layer of compacted clayey soil to limit exhalation of radon gas and percolation of rainwater. Water balance covers rely on a less compacted soil “sponge” to store rainwater, and on soil evaporation and plant transpiration (evapotranspiration) to remove stored water and thereby limit percolation. Over time, natural soil-forming and ecological processes are changing conventional covers by increasing hydraulic conductivity, loosening compaction, and increasing evapotranspiration. The rock armor on conventional covers creates a favorable habitat for vegetation by slowing soil evaporation, increasing soil water storage, and trapping dust and organic matter, thereby providing the water and nutrients needed for plant germination, survival, and sustainable transpiration. Goals and Objectives Our overall goal is to determine if allowing or enhancing these natural changes could improve cover performance and reduce maintenance costs over the long term. This test pad study focuses on cover soil hydrology and ecology. Companion studies are evaluating effects of natural and enhanced changes in covers on radon attenuation, erosion, and biointrusion. We constructed a test cover at the Grand Junction disposal site to evaluate soil manipulation and revegetation methods. The engineering design, construction, and properties of the test cover match the upper three layers of the nearby disposal cell cover: a 1-foot armoring of rock riprap, a 6-inch bedding layer of coarse sand and gravel, and a 2-foot protection layer of compacted fine soil. The test cover does not have a radon barrier—cover enhancement tests leave the radon barrier intact. We tested furrowing and ripping as means for creating depressions parallel to the slope contour, bringing soil up into the rock riprap layer, and loosening and blending compacted fine soil with coarse sand and gravel layers. Objectives of these manipulations include (1) enhancing root growth, (2) increasing seed-soil contact, (3) catching runoff water for plant germination and growth, (4) increasing soil water storage capacity, and (5) enhancing deep drying by disrupting the capillary barrier at the interface of the bedding and protection layers.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

Measurement techniques of thermoelectric devices and modules

Thermoelectric (TE) energy conversion devices are designed based on measured material transport properties. Although an ideal device efficiency can be calculated using the figure of merit, zT, the actual efficiency of a thermoelectric module is smaller and must be measured. TE device performance testing techniques and procedures are reviewed with a focus on energy conversion efficiency. One of the areas that attract less attention in the literature is the transition from basic thermoelectric materials research to the production of modules and devices. The effects of interface layers, diffusion barriers, thermal insulations, and heat sinks are reviewed. Finally, device performance from single couples to standard modules and long-term reliability are discussed.

Wang, Hsin↗

DOE OSTI2013

Schottky barrier height reduction for metal/n-InP by inserting ultra-thin atomic layer deposited high-k dielectrics

Fermi level pinning at metal/n-InP interface and effective Schottky barrier height (Φ{sub B,eff}) were optimized by inserting ultrathin dielectrics in this work. Comparing the inserted monolayer and bilayer high-k dielectrics, we demonstrated that the introduction of bilayer dielectrics can further reduce Φ{sub B,eff} (from 0.49 eV to 0.22 eV) than the monolayer dielectric (from 0.49 eV to 0.32 eV) even though the overall dielectric thickness was thicker. The additional dipole formed at high-k/high-k interfaces could be used to expound the mechanism. This work proposed an effective solution to reduce resistance contacts for InP based transistors and Schottky barrier transistors.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Investigating the effect of aluminum oxide fixed charge on Schottky barrier height in molybdenum oxide-based selective contacts

A tunneling atomic layer deposited (ALD) AlO x layer was inserted in a Si|SiO x |AlO x |MoO x |metal tunnel diode structure to investigate the impact of fixed interface charge on Schottky barrier height. ALD AlO x provides a synthesis-tunable fixed charge and can provide excellent field effect passivation at the SiO x |AlO x interface. A large (>1 × 10 12 q.cm –2 ) negative fixed charge density was expected to decrease Schottky barrier height on p-type silicon and increase Schottky barrier height on n-type silicon by up to 0.4 eV based on an electrostatic model. Fixed charge density and interface trap state density were measured using a thick layer of AlO x in metal oxide semiconductor capacitor structures (MOSCAPs); Schottky barrier height and specific contact resistivity were measured using a tunneling-active layer of AlO x in contacted structures with MoO x . In some samples, HfO x interface layers were inserted between AlO x and silicon to quench the fixed negative charge. The Schottky barrier height was found to vary with processing conditions but did not have a strong correlation with expected fixed charge density. Here, while fixed charge may play a role in determining the Schottky barrier height, other parameters also have significant affect. Further work is needed to minimize contact resistivity and elucidate other factors impacting the Schottky barrier height.

14 SOLAR ENERGY↗

DOE OSTI2020

Microstructure geometry for thermal barrier coatings to mitigate CMAS attack

Thermal barrier coatings and methods to make such coatings present improved resistance to CMAS infiltration. The method for forming a thermal barrier coating includes applying a layer of the thermal barrier coating to a component having a surface, forming a plurality of first channels in the thermal barrier coating, and forming a plurality of second channels in the thermal barrier coating. The first channels extend through a thickness of the thermal barrier coating from an interface with the surface of the component to a free surface opposite the interface. The second channels are disposed between the free surface and the interface and extending lengthwise generally parallel to the free surface of the thermal barrier coating.

Jordan, Eric↗

DOE OSTI2023

Microstructure geometry for thermal barrier coatings to mitigate CMAS attack

Jordan, Eric↗

DOE OSTI2015

Effects of graphene defect on electronic structures of its interface with organic semiconductor

Electronic structures of copper hexadecafluorophthalocyanine (F{sub 16}CuPc)/graphene with different defect density were studied with ultra-violet photoelectron spectroscopy. We showed that the charge transfer interaction and charge flow direction can be interestingly tuned by controlling the defect density of graphene through time-controlled H{sub 2} plasma treatment. By increasing the treatment time of H{sub 2} plasma from 30 s to 5 min, both the interface surface dipole and the electron transporting barrier at F{sub 16}CuPc/graphene interface are significantly reduced from 0.86 to 0.56 eV and 0.71 to 0.29 eV, respectively. These results suggested that graphene's defect control is a simple approach for tuning electronic properties of organic/graphene interfaces.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS1975

Oscillations in MOS tunneling

Oscillatory deviations from Fowler-Nordheim tunneling currents were measured in MOS capacitors with oxide thicknesses ranging from 30 to 75 A. The observed variation of oscillation phases and amplitudes with oxide thickness indicates that the Si-SiO2 interface is independent of oxide thickness only for thicknesses greater than 65 A. At lower thicknesses, the barrier height at the interface decreases gradually with oxide thickness at a rate on the order of 10 mV/A. At higher thicknesses, the barrier height is 4.08 eV. The energy dispersion relation with the SiO2 conduction band is parabolic. The mean free path within the SiO2 conduction band is on the order of 13 A.

Lewicki, G.↗