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DOE OSTI2024

Epitaxial Growth of Ga2O3: A Review

Beta-phase gallium oxide (β-Ga2O3) is a cutting-edge ultrawide bandgap (UWBG) semiconductor, featuring a bandgap energy of around 4.8 eV and a highly critical electric field strength of about 8 MV/cm. These properties make it highly suitable for next-generation power electronics and deep ultraviolet optoelectronics. Key advantages of β-Ga2O3 include the availability of large-size single-crystal bulk native substrates produced from melt and the precise control of n-type doping during both bulk growth and thin-film epitaxy. A comprehensive understanding of the fundamental growth processes, control parameters, and underlying mechanisms is essential to enable scalable manufacturing of high-performance epitaxial structures. This review highlights recent advancements in the epitaxial growth of β-Ga2O3 through various techniques, including Molecular Beam Epitaxy (MBE), Metal-Organic Chemical Vapor Deposition (MOCVD), Hydride Vapor Phase Epitaxy (HVPE), Mist Chemical Vapor Deposition (Mist CVD), Pulsed Laser Deposition (PLD), and Low-Pressure Chemical Vapor Deposition (LPCVD). This review concentrates on the progress of Ga2O3 growth in achieving high growth rates, low defect densities, excellent crystalline quality, and high carrier mobilities through different approaches. It aims to advance the development of device-grade epitaxial Ga2O3 thin films and serves as a crucial resource for researchers and engineers focused on UWBG semiconductors and the future of power electronics.

Chemistry↗

DOE OSTI2022

Coherent Coupling of Two Remote Magnonic Resonators Mediated by Superconducting Circuits

We demonstrate microwave-mediated distant magnon-magnon coupling on a superconducting circuit platform, incorporating chip-mounted single-crystal Y 3 Fe 5 O 12 (YIG) spheres. Coherent level repulsion and dissipative level attraction between the magnon modes of the two YIG spheres are demonstrated. The former is mediated by cavity photons of a superconducting resonator, and the latter is mediated by propagating photons of a coplanar waveguide. Overall, our results open new avenues toward exploring integrated hybrid magnonic networks for coherent information processing on a quantum-compatible superconducting platform.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2025

Additively-manufactured monocrystalline YBCO superconductor

Abstract Single-crystal microstructures enable high-performance YBa 2 Cu 3 O 7-x superconductors which are however limited to simple shapes due to their brittleness. Additive manufacturing can fabricate YBa 2 Cu 3 O 7-x superconductor with complex shapes, albeit with a polycrystalline microstructure. Here, we demonstrate a route to grow single-crystals from 3D-ink-printed, polycrystalline, sintered superconducting YBa 2 Cu 3 O 7-x (YBCO or Y123) + Y 2 BaCuO 5 (Y211), manufacturing objects with complex architectures displaying both high critical current density (J c =2.1 × 10 4 A . cm –2 , 77 K) and high critical temperature (T c = 88-89.5 K). An ink containing precursor powders (Y 2 O 3 , BaCO 3 , and CuO) is 3D-extruded into complex geometries and then reaction-sintered to obtain polycrystalline Y123 + Y211. A seed is then utilized to transform these 3D-printed parts from polycrystal to monocrystal via the melt growth method. The geometric details of 3D-printed parts survive the process without slumping, sagging or collapse, despite the long-term presence of liquid above the peritectic temperature. Origami structures can be created by sheet folding after 3D-printing. This additive approach enables the facile fabrication of superconducting devices with complex shapes and architectures, such as advanced undulator magnets to generate synchrotron radiation and microwave cavities for dark-matter axion search. This work highlights the potential of additive manufacturing for producing monocrystalline cuprate superconductors and opens the door to additive manufacturing of other monocrystalline functional ceramic or semiconductor materials.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2024

Magnetic anisotropy in single-crystalline antiferromagnetic Mn 2 Au

Multiple recent studies have identified the metallic antiferromagnet Mn 2 ⁢Au to be a candidate for spintronic applications due to apparent in-plane anisotropy, preserved magnetic properties above room temperature, and current-induced Néel vector switching. Crystal growth is complicated by the fact that Mn 2 ⁢Au melts incongruently. We present a bismuth flux method to grow millimeter-scale bulk single crystals of Mn 2 ⁢Au in order to examine the intrinsic anisotropic electrical and magnetic properties. Flux quenching experiments reveal that the Mn 2 ⁢Au crystals precipitate below 550°⁢C, about 100⁢°⁢C below the decomposition temperature of Mn 2 ⁢Au. Bulk Mn 2 ⁢Au crystals have a room-temperature resistivity of 16–19 µ⁢Ωcm and a residual resistivity ratio of 41. Mn 2 ⁢Au crystals have a dimensionless susceptibility on the order of 10 –4 (SI units), comparable to calculated and experimental reports on powder samples. Single-crystal neutron diffraction confirms the in-plane magnetic structure. The tetragonal symmetry of Mn 2 ⁢Au constrains the ab-plane magnetic susceptibility to be constant, meaning that χ 100 =χ 110 in the low-field limit, below any spin-flop transition. We find that three measured magnetic susceptibilities χ 100 , χ 110 , and χ 001 are the same order of magnitude and agree with the calculated prediction, meaning the low-field susceptibility of Mn 2 ⁢Au is quite isotropic, despite clear differences in ab-plane and ac-plane magnetocrystalline anisotropy. Mn 2 ⁢Au is calculated to have an extremely high in-plane spin-flop field above 30 T, which is much larger than that of another in-plane antiferromagnet, Fe 2 ⁢As (less than 1 T). Finally, the subtle anisotropy of intrinsic susceptibilities may lead to dominating effects from shape, crystalline texture, strain, and defects in devices that attempt spin readout in Mn 2⁢ Au.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Artifact identification in X-ray diffraction data using machine learning methods

In situ synchrotron high-energy X-ray powder diffraction (XRD) is highly utilized by researchers to analyze the crystallographic structures of materials in functional devices ( e.g. battery materials) or in complex sample environments ( e.g. diamond anvil cells or syntheses reactors). An atomic structure of a material can be identified by its diffraction pattern along with a detailed analysis of the Rietveld refinement which yields rich information on the structure and the material, such as crystallite size, microstrain and defects. For in situ experiments, a series of XRD images is usually collected on the same sample under different conditions ( e.g. adiabatic conditions) yielding different states of matter, or is simply collected continuously as a function of time to track the change of a sample during a chemical or physical process. In situ experiments are usually performed with area detectors and collect images composed of diffraction patterns. For an ideal powder, the diffraction pattern should be a series of concentric Debye–Scherrer rings with evenly distributed intensities in each ring. For a realistic sample, one may observe different characteristics other than the typical ring pattern, such as textures or preferred orientations and single-crystal diffraction spots. Textures or preferred orientations usually have several parts of a ring that are more intense than the rest, whereas single-crystal diffraction spots are localized intense spots owing to diffraction of large crystals, typically >10 µm. In this work, an investigation of machine learning methods is presented for fast and reliable identification and separation of the single-crystal diffraction spots in XRD images. The exclusion of artifacts during an XRD image integration process allows a precise analysis of the powder diffraction rings of interest. When it is trained with small subsets of highly diverse datasets, the gradient boosting method can consistently produce high-accuracy results. The method dramatically decreases the amount of time spent identifying and separating single-crystal diffraction spots in comparison with the conventional method.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2022

Selective amorphization of SiGe in Si/SiGe nanostructures via high energy Si+ implant

Here, the selective amorphization of SiGe in Si/SiGe nanostructures via a 1 MeV Si + implant was investigated, resulting in single-crystal Si nanowires (NWs) and quantum dots (QDs) encapsulated in amorphous SiGe fins and pillars, respectively. The Si NWs and QDs are formed during high-temperature dry oxidation of single-crystal Si/SiGe heterostructure fins and pillars, during which Ge diffuses along the nanostructure sidewalls and encapsulates the Si layers. The fins and pillars were then subjected to a 3 × 10 15 ions/cm 2 1 MeV Si + implant, resulting in the amorphization of SiGe, while leaving the encapsulated Si crystalline for larger, 65-nm wide NWs and QDs. Interestingly, the 26-nm diameter Si QDs amorphize, while the 28-nm wide NWs remain crystalline during the same high energy ion implant. This result suggests that the Si/SiGe pillars have a lower threshold for Si-induced amorphization compared to their Si/SiGe fin counterparts. However, Monte Carlo simulations of ion implantation into the Si/SiGe nanostructures reveal similar predicted levels of displacements per cm 3 . Molecular dynamics simulations suggest that the total stress magnitude in Si QDs encapsulated in crystalline SiGe is higher than the total stress magnitude in Si NWs, which may lead to greater crystalline instability in the QDs during ion implant. The potential lower amorphization threshold of QDs compared to NWs is of special importance to applications that require robust QD devices in a variety of radiation environments.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Electron-Deficient Phenazines: Synthesis, Structures, Redox, and Optoelectronic Properties in the Gas Phase, in Solution, and in the Solid State

High-temperature gas-phase reactions of 1,4-C4F8I2 with phenazine (PHNZ) afforded new thermally- and air-stable derivatives with cyclo-C4F8 substituents, viz. 1,2-PHNZ(C4F8), 2,3-PHNZ(C4F8), 1,2:6,7-PHNZ(C4F8)2, 1,2:7,8-PHNZ(C4F8)2, and 1,2:8,9-PHNZ(C4F8)2. Reactions in the presence of Cu powder resulted in reductive-defluorination/aromatization of some of the cyclo-C4F8 substituents to produce 2,3-PHNZ(C4F4), 2,3-PHNZ(C4HF3), and 1,2:6,7-PHNZ(C4F8)(C4F4), which are formally tri- or tetrafluoro derivatives of benzo[a]phenazine. Single-crystal X-ray diffraction structures of these compounds demonstrate the planarity of 2,3-PHNZ(C4F4) and 2,3-PHNZ(C4HF3) and ordered p-stacking in 1,2-PHNZ(C4HF3), 1,2-PHNZ(C4F4), 1,2-PHNZ(C4F8), and 2,3-PHNZ(C4F8). Low-temperature gas-phase photoelectron spectra of the PHNZ(C4F8)1,2 compounds show that they are strong electron acceptors, with the three PHNZ(C4F8)2 isomers having electron affinities exceeding that of C60. Cyclic voltammetry in acetonitrile show that the five PHNZ(C4F8)1,2 compounds exhibit reversible one-electron reductions with large positive shifts in their reduction potentials relative to unsubstituted PHNZ. Spectroelectrochemical absorption and EPR spectra of PHNZ(C4F8)1,2- • anion radicals and extensive DFT calculations revealed the significant role that the different substitution patterns have on determining the optoelectronic properties of the PHNZ(C4F8)1,2 derivatives and PHNZ(C4F8)1,2- • anion radicals. Time-resolved microwave conductivity measurements and photoluminescence spectra of blends of the PHNZ(C4F8)1,2 derivatives with the donor poly(3-hexylthiophene) (P3HT) were recorded to assess the possible use of the new compounds in optoelectronic devices.

Balser, Sebastian↗

DOE OSTI2022

Title Coherent X-ray Studies of Surface Growth and Patterning Processes

X-ray Photon Correlation Spectroscopy (XPCS) is being developed as a tool to study nanoscale dynamics of fluctuations during thin film growth and surface patterning. XPCS examines the evolution of the X-ray scattering speckle pattern in reciprocal space to reveal dynamics information not accessible through any other means. Unlike low-coherence conventional X-ray scattering, which incoherently averages over different regions of a sample, coherent X-ray scattering is sensitive to the detailed structure of a given sample at that moment in time. In thin film growth processes, heterodyning, which occurs due to coherent mixing of two scattered signals, can be used to investigate the relationship between surface growth velocity and defect propagation. And, for polycrystalline thin film growth, the spatial coherence of the X-ray beam can substitute for the missing spatial coherence of the growth process to track layered growth in detail, even in a growth regime in which there are no conventional growth oscillations of the X-ray intensity. This has opened the door for detailed dynamics studies of individual atomic layers during real-world growth and patterning, not just in perfect single-crystal growth cases, which greatly expands the applicability of in-situ X-ray scattering methods. Step-flow dynamics in mounded polycrystalline growth has been studied separately for two thin film organic semiconductors deposited by thermal deposition in a vacuum environment, C60 and diindenoperylene (DIP). Highly oriented polycrystalline thin films are readily obtained in both systems, where mounds are composed of crystalline monolayer-height steps and terraces in a so-called wedding cake morphology. The formation of mounds is understood to be due to significant Ehrlich-Schwoebel step edge barriers that inhibit molecules from hopping down from one layer to the one below. The mounds exhibit local step flow, which can be monitored using coherent X-ray scattering. This is made possible due to heterodyning between scattering from the average mounds and the moving steps, which becomes visible in XPCS analysis. The effect of desorption, i.e. re-evaporation of deposited molecules is found to be important for understanding these processes. The impact of this work is to enable testing of models of step dynamics, the shape of mounds, and merging of mounds to form continuous thin films. Highly ordered polycrystalline thin films deposited on inexpensive substrates have applications in thin film solar cells and other organic electronic devices. In a separate set of experiments, speckle analysis during self-organized ion beam nanopatterning reveals memory stretching back to the beginning of patterning in the early stages and enables measurement of the velocity of self-organized patterns across surfaces providing the possibility of stringent new tests of the theory of pattern formation and motion.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Spectra-Orthogonal Optical Anisotropy in Wafer-Scale Molecular Crystal Monolayers

Controlling the spectral and polarization response of two-dimensional (2D) crystals is vital for developing ultrathin platforms for compact optoelectronic devices. However, independently tuning optical anisotropy and spectral response remains challenging in conventional semiconductors due to the intertwined nature of their lattice and electronic structures. Here, we report spectra-orthogonal optical anisotropy─where polarization anisotropy is tuned independently of spectral response─in wafer-scale, one-atom-thick 2D molecular crystal (2DMC) monolayers synthesized on monolayer transition-metal dichalcogenide (TMD) crystals. Utilizing the concomitant spectral consistency and structural tunability of perylene derivatives, we demonstrate tunable optical polarization anisotropy in 2DMCs with similar spectral profiles, as confirmed by room-temperature scanning tunneling microscopy and cross-polarized reflectance microscopy. Additional angle-dependent analysis of the single-crystal and polycrystalline molecular domains reveals an epitaxial relationship between the 2DMC and TMD. In conclusion, our results establish a scalable, molecule-based 2D crystalline platform for unique and tunable functionalities unattainable in covalent 2D solids.

2D materials↗

DOE OSTI2024

Giant Uniaxial Magnetocrystalline Anisotropy in SmCrGe 3

Explore the source record for details and available documents.

Xu, Mingyu↗

DOE OSTI2023

Energy conversion and storage via photoinduced polarization change in non-ferroelectric molecular [CoGa] crystals

To alleviate the energy and environmental crisis, in the last decades, energy harvesting by utilizing optical control has emerged as a promising solution. Here we report a polar crystal that exhibits photoenergy conversion and energy storage upon light irradiation. The polar crystal consists of dinuclear [CoGa] molecules, which are oriented in a uniform direction inside the crystal lattice. Irradiation with green light induces a directional intramolecular electron transfer from the ligand to a low-spin Co III centre, and the resultant light-induced high-spin Co II excited state is trapped at low temperature, realizing energy storage. Additionally, electric current release is observed during relaxation from the trapped light-induced metastable state to the ground state, because the intramolecular electron transfer in the relaxation process is accompanied with macroscopic polarization switching at the single-crystal level. It demonstrates that energy storage and conversion to electrical energy is realized in the [CoGa] crystals, which is different from typical polar pyroelectric compounds that exhibit the conversion of thermal energy into electricity.

25 ENERGY STORAGE↗

DOE OSTI2022

Charge transport and antiferromagnetic ordering in nitroxide radical crystals

Nonconjugated radical polymers and small molecules are employed as functional materials in organic electronic devices. Furthermore, the unpaired electrons on these materials have permanent magnetic moments, making these materials promising candidates for organic magnets. Through molecular design, strong antiferromagnetic and ferromagnetic ordering have been achieved in conjugated materials. However, the magnetic properties of nonconjugated radical polymers have only shown weak magnetic interactions among the open-shell sites due to the large mean separation between radicals in typical materials. Here, we have designed, synthesized, and crystalized two open-shell molecules that used molecular engineering to control the assembly of the open-shell sites into a strong antiferromagnetically ordered network. The strong antiferromagnetic interaction is evidenced by a high paramagnetic-to-antiferromagnetic transition temperature of ~40 K. This high transition temperature was a result of a high spin exchange coupling constant J of about –20 cm –1 , which was suggested by both experimental and computed coupling parameters given by the energy difference between high-spin and low-spin broken-symmetry structures. In addition, a single-crystal electrical conductivity of ~10 –3 S m –1 was achieved, which indicated the potential of this material in electronic applications. As a result, this work provides an insight into a design strategy for radical-based electronic and magnetic materials through proper molecular structure modifications.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Microscopic piezoelectric behavior of clamped and membrane (001) PMN-30PT thin films

Bulk single-crystal relaxor-ferroelectrics, like Pb(Mg 1/3 Nb 2/3 )O- 3 -PbTiO 3 (PMN-PT), are widely known for their large piezoelectricity. This is attributed to polarization rotation, which is facilitated by the presence of various crystal symmetries for compositions near a morphotropic phase boundary. Relaxor-ferroelectric thin films, which are necessary for low-voltage applications, suffer a reduction in their piezoelectric response due to clamping by the passive substrate. To understand the microscopic behavior of this adverse phenomenon, we employ the AC electric field driven in-operando synchrotron x-ray diffraction on patterned device structures to investigate the piezoelectric domain behavior under an electric field for both a clamped (001) PMN-PT thin film on Si and a (001) PMN-PT membrane released from its substrate. In the clamped film, the substrate inhibits the field-induced rhombohedral (R) to tetragonal (T) phase transition resulting in a reversible R to Monoclinic (M) transition with a reduced longitudinal piezoelectric coefficient d 33 < 100 pm/V. Releasing the film from the substrate results in recovery of the R to T transition and results in a d 33 > 1000 pm/V. Here, using diffraction with spatial mapping, we find that lateral constraints imposed by the boundary between the active and inactive materials also inhibit the R to T transition. Phase-field calculations on both clamped and released PMN-PT thin films simulate our experimental findings. Resolving the suppression of thin film piezoelectric response is critical to their application in piezo-driven technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2022

PIONEER, a high-resolution single-crystal polarized neutron diffractometer

PIONEER is a high Q-resolution, single-crystal, polarized neutron diffractometer at the Second Target Station (STS), Oak Ridge National Laboratory. It will provide the unprecedented capability of measuring tiny crystals (0.001 mm 3 , i.e., x-ray diffraction size), ultra-thin films (10 nm thickness), and weak structural and magnetic transitions. PIONEER benefits from the increased peak brightness of STS cold-neutron sources and uses advanced Montel mirrors that are able to deliver a focused beam with a high brilliance transfer, a homogeneous profile, and a low background. Monte Carlo simulations suggest that the optimized instrument has a high theoretical peak brilliance of 2.9 × 10 12 n cm -2 sr -1 Å -1 s -1 at 2.5 Å at the sample position, within a 5 × 5 mm 2 region and a ±0.3° divergence range. The moderator-to-sample distance is 60 m, providing a nominal wavelength band of 4.3 Å with a wavelength resolution better than 0.2% in the wavelength range of 1.0–6.0 Å. PIONEER is capable of characterizing large-scale periodic structures up to 200 Å. With a sample-to-detector distance of 0.8 m, PIONEER accommodates various sample environments, including low/high temperature, high pressure, and high magnetic/electric field. Additionally, a large cylindrical detector array (4.0 sr) with a radial collimator is planned to suppress the background scattering from sample environments. Bottom detector banks provide an additional 0.4 sr coverage or can be removed if needed to accommodate special sample environments. We present virtual experimental results to demonstrate the scientific performance of PIONEER in measuring tiny samples.

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

Epitaxial growth of conducting perovskite SrTiO3 on (0001) c-axis sapphire using a γ-Al2O3 intermediate layer

Epitaxial growth of complex oxides on large-area wafers, such as sapphire and silicon, represents a key step toward scalable oxide device production. Solid phase epitaxy allows the synthesis of γ-Al 2 O 3 on α-Al 2 O 3 and provides a template with a matched lattice constant and appropriate cubic symmetry for subsequent heteroepitaxial growth of perovskite complex oxides. Nb-doped SrTiO 3 thin films were deposited epitaxially on (111)-oriented γ-Al 2 O 3 intermediate layers on (0001) c-axis-oriented sapphire α-Al 2 O 3 crystals using pulsed laser deposition. The Nb:SrTiO 3 thin films with a thickness of 53 nm, grown at 700 °C on γ-Al 2 O 3 , reached fully relaxed lattice parameters and were epitaxially oriented with respect to the substrate. Nb:SrTiO 3 layers deposited using identical deposition conditions directly on α-Al 2 O 3 , without the γ-Al 2 O 3 intermediate layer, were polycrystalline. The sheet conductivity of Nb:SrTiO 3 grown on γ-Al 2 O 3 /α-Al 2 O 3 is more than ten times higher than that of Nb:SrTiO 3 grown directly on α-Al 2 O 3 without the γ-Al 2 O 3 layer. The results point to new directions for the integration of (111)-oriented pseudocubic perovskite complex oxides and the integration of epitaxial complex oxides over larger areas using α-Al 2 O 3 single-crystal substrates.

Atomic force microscopy↗

DOE OSTI2022

Multiplication of freestanding III-V semiconductor membranes from a single wafer by alternating growth with amorphous graphene interlayer

Freestanding single-crystalline III-V compound semiconductors are important building blocks for functional devices due to their high electron mobilities, a wide range of bandgaps, and excellent optoelectronic properties. Despite efforts to produce such membranes by detaching epitaxial layers from donor wafers, current methods suffer from either slow processes or poor material quality. Here, we demonstrate a technique to grow and harvest multiple epitaxial membranes with extremely high throughput at the wafer scale. For this, a process to directly grow amorphous graphene on III-V substrates in metal-organic chemical vapor deposition reactors is developed, which enables an advanced remote epitaxy scheme comprised of multiple alternating layers of amorphous graphene and III-V epitaxial layers that can be formed by a single epitaxy run. Each epilayer in the multi-stack structure is then harvested by layer-by-layer peeling, producing multiple freestanding membranes with unprecedented throughput from a single wafer. Because amorphous graphene provides a weak van der Waals interface that allows peeling at the interface without damaging the epilayer or the substrate, wafers can be reused for subsequent membrane production. Therefore, this work represents a meaningful step toward high-throughput and low-cost production of single-crystal membranes that can be heterointegrated.

Han, Ne Myo↗

DOE OSTI2022

Multiplication of freestanding III-V semiconductor membranes from a single wafer by alternating growth with amorphous graphene interlayer

Han, Ne Myo↗

DOE OSTI2024

Dopant Segregation in Single-Crystal Optical Fiber Grown via the Laser-Heated Pedestal Growth Technique

Single crystal (SC) optical fiber has promising potential to be used for optical fiber sensing applications in harsh conditions due to its robustness to high temperature, high radioactivity, and resistance to chemical corrosion as compared to optical sensors using silica fiber. However, SC fiber grown via the laser-heated pedestal growth (LHPG) technique innately does not have a core-cladding structure found in standard optical fiber, resulting in optical losses. In this work we investigate optimization of the growth parameters of a two LHPG process used to grow SC fiber with a graded index via introduction of dopants to the feedstock material. Feedstock material is fabricated with the first LHPG device, then sol-gel dip-coated to create outer films of dopant material. The dip-coated feedstock is used to grow SC fiber in which segregation of the dopant constituents occurs, resulting in a graded index of refraction across the fiber, and an effective core-cladding structure. Hardware and software improvements to both LHPG systems are presented and the growth parameters for short pieces of ~320-330 μm diameter YAG fiber has been established. Characterization techniques/procedures have also been established for future grown SC fiber. These improvements and preparations are anticipated to result in a significant increase in grown fiber quality with a similar growth rate to that previously established.

Lander, Gary↗