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At least 1,045 records · Page 58
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Metalorganic vapor phase epitaxy of AlN on sapphire with low etch pit density

Using metalorganic vapor phase epitaxy, methods were developed to achieve AlN films on sapphire with low etch pit density (EPD). Key to this achievement was using the same AlN growth recipe and only varying the pre-growth conditioning of the quartz-ware. After AlN growth, the quartz-ware was removed from the growth chamber and either exposed to room air or moved into the N2 purged glove box and exposed to H2O vapor. After the quartz-ware was exposed to room air or H2O, the AlN film growth was found to be more reproducible, resulting in films with (0002) and (10–12) x-ray diffraction (XRD) rocking curve linewidths of 200 and 500 arc sec, respectively, and EPDs < 100 cm−2. The EPD was found to correlate with (0002) linewidths, suggesting that the etch pits are associated with open core screw dislocations similar to GaN films. Once reproducible AlN conditions were established using the H2O pre-treatment, it was found that even small doses of trimethylaluminum (TMAl)/NH3 on the quartz-ware surfaces generated AlN films with higher EPDs. The presence of these residual TMAl/NH3-derived coatings in metalorganic vapor phase epitaxy (MOVPE) systems and their impact on the sapphire surface during heating might explain why reproducible growth of AlN on sapphire is difficult.

Koleske, D. D.↗
DOE OSTI2017

δ -Doping of oxygen vacancies dictated by thermodynamics in epitaxial SrTiO 3 films

Homoepitaxial SrTiO 3 (110) film is grown by molecular beam epitaxy in ultra-high vacuum with oxygen diffusing from substrate as the only oxidant. The resulted oxygen vacancies (V O s ) are found to be spatially confined within few subsurface layers only, forming a quasi-two-dimensional doped region with a tunable high concentration. Such a δ-function distribution of V O s is essentially determined by the thermodynamics associated with the surface reconstruction, and facilitated by the relatively high growth temperature. Here, our results demonstrate that it is feasible to tune V O s distribution at the atomic scale by controlling the lattice structure of oxide surfaces. Transition metal oxide interfaces have exhibited a variety of novel phenomena, including the high-mobility two-dimensional electron gas, superconductivity and unusual magnetism. While these phenomena are inherently related to the artificially designed architecture, oxygen vacancies (V O s ) are recognized to be particularly important in determining the exotic behaviors of the oxides systems. As electron donors in oxides, V O s were observed to be one of the major factors for the high carrier density at the LaAlO 3 /SrTiO 3 interface. V O s induce ferromagnetism in the epitaxial LaCoO 3 films via the ordering of excess electrons in Co 3d orbit. It was also suggested that the existence of V O s plays an important role in the formation of undesirable insulating phase in ultrathin films of many metallic oxide materials, referred to as the “dead layer” behavior. How V O s are involved in such complex phenomena is still unclear. One essential issue toward the design of emergent properties of oxide films is how to characterize and control V O s at the atomic scale. Recently, quantitative measurements of V O concentration have been realized with high spatial resolution benefited by the development of the state-of-the-art aberration-corrected scanning transmission microscope (STEM) and related spectroscopy techniques. However, tuning the V O density precisely by growth control is still extremely challenging. Different oxidants, i.e., molecular O 2 , O 3 and atomic O, have been used with different feeding pressure during the growth. This approach is limited by thermodynamics of the material since the pressure of oxidant has to coordinate with temperature and other parameters in order to ensure the formation of the desired phase. In many cases the optimal condition for oxygen stoichiometry cannot be reached, and residual V O s are inevitably formed. It has been reported that V O s even form inhomogeneous clusters in SrTiO 3 (STO) films. Post annealing is another thermodynamic approach and seems to be effective to reduce the V O density. However, it does not allow the precise control of V O s distribution at the atomic scale either. In the current work, to study the control of V O s at the atomic scale, we grow SrTiO 3 homoepitaxial films along the polar [110] direction. Atomically well-defined (4 × 1) reconstruction is maintained on the surface all through the growth [see Fig. 1 (a) and (b)], which compensates the polarity. More importantly, the energy configuration associated with the surface reconstruction results in the spatial confinement of V O s within only few subsurface layers of the film, while their concentration remains extremely low on the topmost surface and in the bulk of STO substrate. In conclusion, we show that such a quasi-two-dimensional (2D) V O -doped layer, mimicking the δ-doping case in conventional semiconductors, can be precisely controlled.

36 MATERIALS SCIENCE↗
DOE OSTI2017

An all-perovskite p-n junction based on transparent conducting p -La 1-x Sr x CrO 3 epitaxial layers

Transparent, conducting p -La 1-x Sr x CrO 3 epitaxial layers were deposited on Nb-doped SrTiO 3 (001) by oxygen-assisted molecular beam epitaxy to form structurally coherent p-n junctions. X-ray photoelectron spectroscopy reveals a type II or “staggered” band alignment, with valence and conduction band offsets of 2.0 eV and 0.9 eV, respectively. Diodes fabricated from these heterojunctions exhibit rectifying behavior, and the I-V characteristics are different from those for traditional semiconductor p-n junctions. A rather large ideality factor is ascribed to the complex nature of the interface.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Structural and electrical properties of single crystalline SrZrO 3 epitaxially grown on Ge (001)

Here, we present structural and electrical characterization of SrZrO 3 that has been epitaxially grown on Ge(001) by oxide molecular beam epitaxy. Single crystalline SrZrO 3 can be nucleated on Ge via deposition at low temperatures followed by annealing at 550 ºC in ultra-high vacuum. Photoemission spectroscopy measurements reveal that SrZrO 3 exhibits a type-I band arrangement with respect to Ge, with conduction and valence band offsets of 1.4 eV and 3.65 eV, respectively. As a standalone film, SrZrO 3 exhibits several characteristics that are ideal for applications as a gate dielectric on Ge. We find that 4 nm thick films exhibit low leakage current densities, and a dielectric constant of κ ~ 25 that corresponds to an equivalent oxide thickness of 0.70 nm.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2018

Reconstruction-stabilized epitaxy of LaCoO 3 /SrTiO 3 (111) heterostructures by pulsed laser deposition

Unlike widely explored complex oxide heterostructures grown along [001], the study of [111]-oriented heterointerfaces is very limited thus far. One of the main challenges is to overcome the polar discontinuity that hinders the epitaxy of atomically sharp interfaces. Here, by taking LaCoO 3 /SrTiO 3 (111) as a prototype, we show that the reconstruction, which effectively compensates the surface polarity, can stabilize the epitaxy of the heterostructure with polar discontinuity. A reconstructed substrate surface is prepared, while the growth is controlled to form reconstruction on the film surface. To suppress the chemical diffusion across the interface, the growth is interrupted between each unit cell layer to allow the lattice relaxation at a lowered temperature. In this way, high quality two-dimensional growth is realized and the heterointerfaces exhibit sharpness at the atomic scale. As a result, our work provides a path to precisely control the growth of complex oxide heterostructures along polar orientations that exhibit emergent quantum phenomena.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Relaxation of asymmetric crystallographic tilt: In situ x-ray diffraction studies of epitaxial electrodeposition of bismuth on GaAs (110)

High quality, epitaxial thin-films are key components of almost all modern electronic devices. During deposition, lattice mismatch between the substrate and the film generates elastic strain. The strain energy grows with film thickness until a defect is generated that relieves the strain. The strain relaxation mechanism is critical in epitaxial electrodeposition. Here, we study how a metal (bismuth) film growing via electrodeposition on a semiconductor substrate [GaAs(110)] relaxes the lattice mismatch-induced strain. Using in situ synchrotron-based X-ray techniques, we monitor the crystallographic orientation and grain size of the growing film during electrochemical deposition. We (1) confirm that a single crystallographic orientation of the film, with ($01\bar{1}8$) as the oriented plane, can be selected by controlling the overpotential, η, and (2) find that, after a threshold thickness is reached, the tilt angle varies monotonically with film thickness. Our data are consistent with the film relaxing the strain by forming low-energy, asymmetric tilt boundaries.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Electronic structure of epitaxial half-Heusler Co 1-x Ni x TiSb across the semiconductor to metal transition

In this paper, we report on the growth, electronic, and surface properties of the electron-doped half-Heusler series Co 1-x Ni x TiSb (001) grown by molecular beam epitaxy. High-quality epitaxial growth of thin films is achieved on InP (001) substrates using an InAlAs buffer layer for all nickel concentrations. The semiconductor to metal transition as a function of substitutional alloying was examined using electrical transport, Seebeck measurements, and angle-resolved photoemission spectroscopy (ARPES). Temperature-dependent electrical transport measurements of films with composition x ≤ 0.1 exhibit thermally activated behavior while x > 0.1 exhibit metallic behavior. Smooth, highly ordered film surfaces can be achieved following ex-situ transfer of the films and subsequent desorption of a sacrificial, protective antimony capping layer. Using this transfer technique, ARPES experiments were performed to investigate the effects of nickel alloying on the electronic band structure. Finally, an electron pocket is observed below the Fermi level at the bulk X point for compositions x > 0.1, in accordance with the crossover from semiconducting to metallic behavior observed in the transport measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Cooperative effects of strain and electron correlation in epitaxial VO 2 and NbO 2

Here, we investigate the electronic structure of the epitaxial VO 2 films in the rutile phase using the density functional theory combined with the slave spin method (DFT+SS). In DFT-SS, the multiorbital Hubbard interactions are added to a DFT-fit tight-binding model, and we employ the slave-spin method to treat the electron correlation. We find that while stretching the system along the rutile c-axis results in a band structure favoring an anisotropic orbital fillings, the electron correlation favors an equal electron filling among t 2 g orbitals. These two distinct effects cooperatively induce interesting orbital-dependent redistributions of the electron occupations and the spectral weights, which pushes the strained VO 2 toward an orbital selective Mott transition (OSMT). The simulated single-particle spectral functions are directly compared to V L-edge resonant X-ray photoemission spectroscopy of epitaxial 10 nm VO 2 /TiO 2 (001) and (100) strain orientations. Excellent agreement is observed between the simulations and experimental data regarding the strain-induced evolution of the lower Hubbard band. Simulations of rutile NbO 2 under similar strain conditions as VO 2 are performed, and we predict that OSMT will not occur in rutile NbO 2 . Our results indicates that the electron correlation in VO 2 is important and can be modulated even in the rutile phase before the Peierls instability sets in.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Systematic control of strain-induced perpendicular magnetic anisotropy in epitaxial europium and terbium iron garnet thin films

We show tunable strain-induced perpendicular magnetic anisotropy (PMA) over a wide range of thicknesses in epitaxial ferrimagnetic insulator Eu 3 Fe 5 O 12 (EuIG) and Tb 3 Fe 5 O 12 (TbIG) thin films grown by pulsed-laser deposition on Gd 3 Ga 5 O 12 with (001) and (111) orientations, respectively. The PMA field is determined by measuring the induced anomalous Hall loops in Pt deposited on the garnet films. Due to positive magnetostriction constants, compressive in-plane strain induces a PMA field as large as 32.9 kOe for 4 nm thick EuIG and 66.7 kOe for 5 nm thick TbIG at 300 K and relaxes extremely slowly as the garnet film thickness increases. In bilayers consisting of Pt and EuIG or Pt and TbIG, robust PMA is revealed by squared anomalous Hall hysteresis loops in Pt, the magnitude of which appears to be only related to the net magnetic moment of iron sublattices. Furthermore, the magnetostriction constant is found to be 2.7 × 10 -5 for EuIG and 1.35 × 10 -5 for TbIG, comparable with the values for bulk crystals. Our results demonstrate a general approach of tailoring magnetic anisotropy of rare earth iron garnets by utilizing modulated strain via epitaxial growth.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Hard x-ray standing-wave photoemission insights into the structure of an epitaxial Fe/MgO multilayer magnetic tunnel junction

The Fe/MgO magnetic tunnel junction is a classic spintronic system, with current importance technologically and interest for future innovation. The key magnetic properties are linked directly to the structure of hard-to-access buried interfaces, and the Fe and MgO components near the surface are unstable when exposed to air, making a deeper probing, nondestructive, in-situ measurement ideal for this system. We have thus applied hard X-ray photoemission spectroscopy (HXPS) and standing-wave (SW) HXPS in the few kilo-electron-volt energy range to probe the structure of an epitaxially grown MgO/Fe superlattice. The superlattice consists of 9 repeats of MgO grown on Fe by magnetron sputtering on an MgO(001) substrate, with a protective Al 2 O 3 capping layer. We determine through SW-HXPS that 8 of the 9 repeats are similar and ordered, with a period of 33 ± 4 Å, with the minor presence of FeO at the interfaces and a significantly distorted top bilayer with ca. 3 times the oxidation of the lower layers at the top MgO/Fe interface. There is evidence of asymmetrical oxidation on the top and bottom of the Fe layers. We find agreement with dark-field scanning transmission electron microscope (STEM) and X-ray reflectivity measurements. Through the STEM measurements, we confirm an overall epitaxial stack with dislocations and warping at the interfaces of ca. 5 Å. We also note a distinct difference in the top bilayer, especially MgO, with possible Fe inclusions. Finally, we thus demonstrate that SW-HXPS can be used to probe deep buried interfaces of novel magnetic devices with few-angstrom precision.

36 MATERIALS SCIENCE↗
DOE OSTI2019

A magnetic phase diagram for nanoscale epitaxial BiFeO 3 films

BiFeO 3 thin films have attracted considerable attention by virtue of their potential application in low-energy spintronic and magnonic devices. BiFeO 3 possesses an intricate magnetic structure, characterized by a spin cycloid with period ~62 nm that governs the functional magnonic response, and which can be modulated or even destroyed by strain, magnetic and electric fields, or chemical doping. The literature on (110)-oriented BiFeO 3 films is not explicit in defining the conditions under which this cycloid persists, as its presence depends on synthesis method and thin-film boundary conditions, especially in the sub-100 nm thickness regime. This report aims to end “trial and error” approaches in determining the conditions under which this cycloid and its associated functional magnonic response exist. We show that in specific crystallographic orientations of epitaxial BiFeO 3 , an unexplored strain parameter—the distortion in the ab plane of the monoclinic unit cell—significantly influences the spin structure. Combining Mössbauer spectroscopy and low-energy Raman spectroscopy with first-principles-based effective Hamiltonian calculations, we show that both average strain and this distortion destroy the cycloid. For films grown on (110)-oriented SrTiO 3 substrates, if the BiFeO 3 lattice parameters a and b differ by more than about 1.2%, the cycloid is destabilized, resulting in a pseudocollinear magnetic order ground state. We are thereby able to construct a phase diagram of the spin structure for nanoscale epitaxial BiFeO 3 films, which aims to resolve long-standing literature inconsistencies and provide powerful guidelines for the design of future magnonic and spintronic devices.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Competing phases in epitaxial vanadium dioxide at nanoscale

Phase competition in correlated oxides offers tantalizing opportunities as many intriguing physical phenomena occur near the phase transitions. Owing to a sharp metal-insulator transition (MIT) near room temperature, the correlated vanadium dioxide (VO 2 ) exhibits a strong competition between insulating and metallic phases, which is important for practical applications. However, the phase boundary undergoes a strong modification when strain is involved, yielding complex phase transitions. Here, we report the emergence of nanoscale M2 phase domains in VO 2 epitaxial films under anisotropic strain relaxation. The competing phases of the films are imaged by multilength-scale probes, detecting the structural and electrical properties in individual local domains. Competing evolution of the M1 and M2 phases indicates the critical role of lattice-strain on both the stability of the M2 Mott phase and the energetics of the MIT in VO 2 films. This study demonstrates how strain engineering can be utilized to design phase states, which allow deliberate control of MIT behavior at the nanoscale in epitaxial VO 2 films.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Epitaxial Er-doped Y 2 O 3 on silicon for quantum coherent devices

Rare-earth ions have incomplete 4f shells and possess narrow optical intra-4f transitions due to shielding from electrons in the 5s and 5p orbitals, making them good candidates for solid-state optical quantum memory. The emission of Er 3+ in the telecom C-band (1530 nm – 1565 nm) makes it especially attractive for this application. In order to build practical, scalable devices, the REI needs to be embedded in a non-interacting host material, preferably one that can be integrated with silicon. In this paper, we show that Er 3+ can be isovalently incorporated into epitaxial Y 2 O 3 thin films on Si (111). We report on the synthesis of epitaxial, single-crystalline Er:Y 2 O 3 on Si with a narrow inhomogeneous linewidth in the photoluminescence spectra, 5.1 GHz (<100 mK) and an optical excited state lifetime of 8.1 ms. The choice of Y 2 O 3 was driven by its low nuclear spin and small lattice mismatch with Si. Using photoluminescence (PL) and electron paramagnetic resonance, we show that Er 3+ substitutes for Y in the crystal lattice. The role of interfacial SiO x , diffusion of silicon into the film, and the effect of buffer layers on inhomogeneous PL linewidth are examined. We also find that the linewidth decreased monotonically with film thickness but surprisingly exhibits no correlation with the film crystalline quality as measured by the x-ray rocking curve scans suggesting other factors at play that limit the inhomogeneous broadening in Y 2 O 3 films.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Self-regulated growth of candidate topological superconducting parkerite by molecular beam epitaxy

Ternary chalcogenides, such as parkerites and shandites, are a broad class of materials exhibiting a rich diversity of transport and magnetic behavior and an array of topological phases, including Weyl and Dirac nodes. However, they remain largely unexplored as high-quality epitaxial thin films. Here, we report the self-regulated growth of thin films of the strong spin–orbit coupled superconductor Pd 3 Bi 2 Se 2 on SrTiO 3 by molecular beam epitaxy. Films are found to grow in a self-regulated fashion, where, in excess Se, the temperature and relative flux ratio of Pd to Bi control the formation of Pd 3 Bi 2 Se 2 due to the combined volatility of Bi, Se, and Bi–Se bonded phases. The resulting films are shown to be of high structural quality, and the stoichiometry is independent of the Pd:Bi and Se flux ratio and exhibits a superconducting transition temperature of 800 mK and a critical field of 17.7 ± 0.5 mT, as probed by transport and magnetometry. Understanding and navigating the growth of the chemically and structurally diverse classes of ternary chalcogenides open a vast space for discovering new phenomena and enabling new applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Strain- and thickness-dependent magnetic properties of epitaxial La 0.67 Sr 0.33 CoO 3 /La 0.67 Sr 0.33 MnO 3 bilayers

Magnetic properties and interfacial phenomena of epitaxial perovskite oxides depend sensitively on parameters such as film thickness and strain state. In this work, epitaxial La0 .67 Sr 0.33 CoO 3 (LSCO)/La 0.67 Sr 0.33 MnO 3 (LSMO) bilayers were grown on NdGaO 3 (NGO) and LaAlO 3 (LAO) substrates with a fixed LSMO thickness of 6 nm, and LSCO thickness (t LSCO ) varying from 2 to 10 nm. Soft x-ray magnetic spectroscopy revealed that magnetically active Co 2+ ions that strongly coupled to the LSMO layer were observed below a critical t LSCO for bilayers grown on both substrates. On LAO substrates, this critical thickness was 2 nm, above which the formation of Co 2+ ions was quickly suppressed leaving only a soft LSCO layer with mixed valence Co 3+ /Co 4+ ions. The magnetic properties of both LSCO and LSMO layers displayed strong t LSCO dependence. This critical t LSCO increased to 4 nm on NGO substrates, and the magnetic properties of only the LSCO layer displayed t LSCO dependence. A non-magnetic layer characterized by Co 3+ ions and with a thickness below 2 nm exists at the LSCO/substrate interface for both substrates. Therefore, the results contribute to the understanding of interfacial exchange spring behavior needed for applications in next generation spintronic and magnetic memory devices.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Structural and optical characterization of dilute Bi-doped GaN nanostructures grown by molecular beam epitaxy

We have carried out detailed studies on the epitaxy and characterization of dilute Bi-doped GaN nanostructures. A comprehensive investigation of Bi-doped GaN nanowires and quasi-film epitaxial growth conditions has been performed. Scanning electron microscopy studies show that lowering the GaBiN growth temperature causes gradual changes in top c-plane nanowire morphology due to the incremental incorporation of foreign Bi atoms. This trend is further substantiated by the secondary ion mass spectroscopy analysis of a multi-layer Bi-doped GaN quasi-film. However, it is also found that the amount of Bi incorporation into the GaN lattice is relatively independent of the N2 flow rate variation under the growth conditions investigated. Furthermore, room-temperature micro-Raman spectra show that there are additional peaks near 530, 650, and 729 cm−1 wave numbers in the Bi-doped GaN samples, which can primarily be attributed to Bi local vibrational modes, indicative of a small amount of Bi incorporation in the GaN lattice. Moreover, phonon calculations with density functional theory indicate that Bi replacing the N sites is the likely origin of the experimentally measured Raman modes. X-ray photoelectron spectroscopy measurements have also been obtained to deduce the electronic interaction between the Bi dopant atom and the GaN nanostructure. Such one-dimensional nanowires permit the synthesis of dislocation-free highly mismatched alloys due to strain relaxation, allowing efficient light absorption and charge carrier extraction that is relevant for solar energy harvesting and artificial photosynthesis.

Materials Science↗
DOE OSTI2024

Nano-infrared imaging of epitaxial graphene on SiC revealing doping and thickness inhomogeneities

Here, we report on a nano-infrared (IR) imaging and spectroscopy study of epitaxial graphene on silicon carbide (SiC) by using scattering-type scanning near-field optical microscopy (s-SNOM). With nano-IR imaging, we reveal in real space microscopic domains with distinct IR contrasts. By analyzing the nano-IR, atomic force microscopy, and scanning tunneling microscopy imaging data, we conclude that the imaged domains correspond to single-layer graphene, bilayer graphene (BLG), and higher-doped BLG. With nano-IR spectroscopy, we find that graphene can screen the SiC phonon resonance, and the screening is stronger at more conductive sample regions. Our work offers insights into the rich surface properties of epitaxial graphene and demonstrates s-SNOM as an efficient and effective tool in characterizing graphene and possibly other two-dimensional materials.

2D materials↗
DOE OSTI2025

Ferroelectric epitaxial Al(Sc/B)N/Mo/SiC heterostructures for high operating temperature devices

Advances in wurtzite nitride ferroelectrics of Al 1-x M x N (⁠ M = Sc or B) have led to novel capabilities, which must be integrated into existing fabrication processes. In the case of electronics operating > 200°C, a movement toward SiC-based platforms enables better performance over conventional Si, primarily due to the higher bandgap and lower intrinsic carrier concentration of SiC. Hence, the challenge is to develop a deposition process to integrate Al 1-x M x M x N ferroelectrics with elevated temperature-compatible materials for high temperature electronics such as the non-volatile memory component. We demonstrate epitaxial Al M N/Mo/SiC heterostructures, which provides both the crystalline and surface features that promote high-quality ferroelectric nitride film growth. Omega scans of the Mo (110) reflection exhibit a full width at half max of < 0.02° (40 arc sec) and the (0002) peak of the subsequently grown nitride film had a value of 1.1° for 160 nm thick Al 0.7 Sc 0.3 N and 1.3° for 400 nm thick Al 0.94 B 0.06 N. The crystallographic relationships found between the Al M N, Mo, and SiC layers indicate an advancement in sputter deposition of epitaxial films. Ferroelectric switching is also shown at 400 °C in both samples via polarization-electric field hysteresis and pulsed measurements, which exhibited P r values >100 μC cm -2 and E c between 3 and 4 M V cm -1 ⁠, despite a large presence of oxygen in both Al M N films ranging between 4 and 5 at.%, revealed by compositional analysis. This study demonstrates the process for synthesizing high-crystal quality ferroelectric nitride films, which can be used in extremely high temperature applications.

74 ATOMIC AND MOLECULAR PHYSICS↗