X-ray Pole Figure Research Articles

Engineering wafer scale single-crystalline Si growth on epitaxial Gd2O3/Si(111) substrate using radio frequency sputtering for silicon on insulator application

Silicon on Insulator (SOI) technology has been the promising solution for the On-chip low-power mixed-signal systems. However, the traditional smart-cut method for SOI wafer fabrication is costly. Hence, in this work, we present an optimized methodology to fabricate a wafer scale single-crystalline Si on epitaxial Gd2O3/Si(111) substrate (SOXI) using a low-cost, high volume manufacturable (HVM)-friendly Radio Frequency magnetron sputtering technique for SOI application. The grown Si and Gd2O3 layers are physically characterized using high-resolution X-ray Diffraction and high-resolution Transmission Electron Microscopy (HRTEM). The Grazing Incidence X-ray Diffraction, Pole Figure, and HRTEM imaging confirm the formation of an epitaxial Top-Si layer on the epitaxial-Gd2O3/Si(111) substrate. Hence, we demonstrate a low-cost, HVM-friendly technique for the fabrication of SOXI wafers.

Heterogeneous microstructure development in additive friction-stir deposited Al-Mg-Si alloy

Aluminum alloy 6061-T6511 was printed by additive friction stir deposition onto a cast aluminum A206-T4 plate. Metallography, X-ray powder diffraction, X-ray pole figure analysis, and electron backscatter diffraction of the center, advancing side, and retreating side of the 6061 deposit reveals different texture and grain structure characteristics across the transverse direction and through each layer. These distinct microstructural domains are indicative of spatially varied temperature, strain rate, and strain accumulation during deposition, and consequently of regions differing in the fraction of dynamic recovery and dynamic recrystallization during deposition. Hardness mapping over the complete cross section at 0.75 mm resolution shows the alloy continues to age after active deposition, and hardness increases over the 5 mm nearest the final printed layer. Additional mapping at 0.10 mm resolution shows intralayer hardness variations of the deposit on the retreating side. These observations demonstrate that complex and non-uniform thermal-mechanical transients occur during additive friction stir deposition, resulting in spatially non-uniform microstructure and properties.

Preparation of Textured Polycrystalline La2NiO4+ δ Membranes and Their Oxygen-Transporting Properties

Due to its high chemical and thermal stability in CO2 atmosphere and its anisotropic crystal structure, the Ruddlesden-Popper phase La2NiO4+δ has attracted considerable attention in the research field of oxygen-transporting membranes. The anisotropic properties of La2NiO4+δ can be exploited in textured polycrystalline membranes to control the oxygen diffusion through this material. To fabricate textured La2NiO4+δ membranes, powder mixtures consisting of fine-grained equiaxial La2NiO4+δ matrix particles and large plate-like La2NiO4+δ template particles in different mass ratios were uniaxially pressed and then sintered in air. For this purpose, the anisotropic template particles were synthesized by molten-flux method using NaOH as flux [1]. In the powder mixture, the La2NiO4+δ template particles can be aligned perpendicular or parallel to the pressing direction, depending on the geometry of the pressing tool and the sample preparation. After the sintering process, textured La2NiO4+δ membranes were obtained, which was verified by measuring X-ray diffraction patterns and pole figures. Further X-ray diffraction measurements together with the calculation of the Lotgering orientation factor revealed that an increasing content of the template particles in the ceramic materials leads to a stronger texturing. Scanning electron microscopy micrographs show some individual plate-like La2NiO4+δ grains well embedded in the matrix. Homogeneous distribution of lanthanum, nickel and oxygen in the ceramics was confirmed by energy-dispersive X-ray spectroscopy. Finally, the influence of the template particle content in the La2NiO4+δ membranes on the oxygen permeation performance is discussed. [1] Escobar Cano, G.; Brinkmann, Y.; Zhao, Z.; Kißling, P.A.; Feldhoff, A. Sol–Gel-Process-Based Molten-Flux Synthesis of Plate-like La2NiO4+ δ Particles. Crystals 2022, 12, 1346. https://doi.org/10.3390/cryst12101346

Growth and optical properties of NiO thin films deposited by pulsed dc reactive magnetron sputtering

NiO thin films with varied oxygen contents are grown on Si(100) and c-Al2O3 at a substrate temperature of 300 °C using pulsed dc reactive magnetron sputtering. We characterize the structure and optical properties of NiO changes as functions of the oxygen content. NiO with the cubic structure, single phase, and predominant orientation along (111) is found on both substrates. X-ray diffraction and pole figure analysis further show that NiO on the Si(100) substrate exhibits fiber-textured growth, while twin domain epitaxy was achieved on c-Al2O3, with NiO(111)∥Al2O3(0001) and NiO[11¯0]∥Al2O3[101¯0] or NiO[1¯10]∥Al2O3[21¯1¯0] epitaxial relationship. The oxygen content in NiO films did not have a significant effect on the refractive index, extinction coefficient, and absorption coefficient. This suggests that the optical properties of NiO films remained unaffected by changes in the oxygen content.

Comparative Study of Flax and Pineapple Leaf Fiber Reinforced Poly(butylene succinate): Effect of Fiber Content on Mechanical Properties.

In this study, we compare the reinforcing efficiency of pineapple leaf fiber (PALF) and cultivated flax fiber in unidirectional poly(butylene succinate) composites. Flax, known for robust mechanical properties, is contrasted with PALF, a less studied but potentially sustainable alternative. Short fibers (6 mm) were incorporated at 10 and 20% wt. levels. After two-roll mill mixing, uniaxially aligned prepreg sheets were compression molded into composites. At 10 wt.%, PALF and flax exhibited virtually the same stress-strain curve. Interestingly, PALF excelled at 20 wt.%, defying its inherently lower tensile properties compared to flax. PALF/PBS reached 70.7 MPa flexural strength, 2.0 GPa flexural modulus, and 107.3 °C heat distortion temperature. Comparable values for flax/PBS were 57.8 MPa, 1.7 GPa, and 103.7 °C. X-ray pole figures indicated similar matrix orientations in both composites. An analysis of extracted fibers revealed differences in breakage behavior. This study highlights the potential of PALF as a sustainable reinforcement option. Encouraging the use of PALF in high-performance bio-composites aligns with environmental goals.

Homoepitaxial growth of β-Ga2O3 by halide vapor phase epitaxy

We demonstrated halide vapor phase epitaxy of β-Ga2O3 on a native substrate, which should be scalable and useful for the formation of vertical fins and trenches with smooth (100)-faceted sidewalls using plasma-free microfabrication techniques, e.g., selective area growth and gas etching, for use in power device applications. No misoriented domains were detected in the epiwafer during x-ray pole figure measurements. The full width at half maximum values of the x-ray rocking curves of the epiwafer were virtually the same as those of the bare substrate. No domain boundaries were found using scanning transmission electron microscopy at the film/substrate interface. The growth rate was as high as 23 μm h−1, which was comparable to the rate for a (001) epilayer that was grown simultaneously.

Elemental and Crystallographic Analysis of Trapiche Ruby using Micro X-ray Fluorescence Spectroscopy, X-ray Pole Figure Map, and Low Vacuum Type Field Emission Scanning Electron Microscopy.

Elemental and Crystallographic Analysis of Trapiche Ruby using Micro X-ray Fluorescence Spectroscopy, X-ray Pole Figure Map, and Low Vacuum Type Field Emission Scanning Electron Microscopy.

Effect of rolling routes on the microstructure, texture and mechanical properties of Mg-5Y binary alloy

ABSTRACT The present study examined the influence of rolling routes and strains on the microstructure, texture, and mechanical properties of Mg-5Y binary alloy. The specimens were hot-rolled at 420°C with varying rolling routes (i.e. unidirectional rolling (UR) and cross rolling (CR)) and rolling strain (10%–60%). The microstructural and textural evolution was studied using EBSD maps and X-ray pole figures. Further, the mechanical behaviour was examined using room temperature tensile tests. The results suggested that rolling strain increment leads to the increased recrystallized fraction in both UR and CR specimens. Alternatively, CR samples showed finer grain size with a higher fraction of recrystallized grains than UR samples at fixed strain. The texture of the former was found to be different as compared to the latter. Further, the mechanical properties of CR samples showed significant improvement than UR samples. This was attributed to fine grain size and altered basal texture.

X-ray Pole figure analysis for orienting TGSM grown bulk ZnTe crystal for Terahertz device applications

X-ray Pole figure analysis for orienting TGSM grown bulk ZnTe crystal for Terahertz device applications

The stress release of morphological change on thermochromic properties of nitrogen-incorporated VO2 thin films

VO2 thin films are fabricated by the reactive high power impulse magnetron sputtering technique. Their thermochromic properties are found to be greatly affected by the addition of nitrogen during the deposition process. These include an effect of localized surface plasmon resonance due to isolated island structures. Furthermore, low transition temperatures below 45 °C are observed due to oxygen-deficient conditions. Also, the transition temperature decreases with an increase in the thickness of the TiO2 buffer layer. The reduction in transition temperature could be as low as 39 °C with a solar modulating ability of 4% at a thicker buffer of 300 nm under a high gas ratio of 21.7% for nitrogen. The crystalline phase is identified by x-ray diffraction, showing that the intensity of monoclinic crystallites at a diffraction angle of 2θ = 27.8° for (011) phase decreases with an increase in the amount of nitrogen, whereas a relaxing shift is detected near the diffraction angle of 2θ = 37.0° for (2¯11) phase. Similar behavior is seen in the peak shift of the (004) phase for TiO2. The d-spacing of the crystallization phase with island structure is identified by high-resolution transmission electron microscopy. The evolution of stress release, which is strongly dependent on surface morphology, is consistent with x-ray pole figure representation. The visible transmittance and solar modulation ability as functions of the amount of nitrogen and the buffer thickness of TiO2 are discussed.

Epitaxial Electrodeposition of Wide Bandgap Cuprous Bromide on Silver via a Silver Bromide Buffer Layer

Cuprous halides are an important class of wide bandgap p-type semiconductors used in opto-electronics. Cuprous bromide (CuBr) shows potential for short-wavelength devices due to a large exciton binding energy (108 meV) and near-ultraviolet bandgap (3.1 eV). However, the growth of high-quality epitaxial CuBr films by electrodeposition has remained a challenge. Here, we introduce a low-cost electrochemical procedure for producing epitaxial CuBr(111) on a Ag(111) substrate by a [111]-oriented silver bromide (AgBr) buffer layer. The AgBr buffer layer forms during the electrodeposition of the CuBr. The mismatch between CuBr(111) and AgBr(111) is −1.3%. A plausible mechanism for nucleation and growth of the epitaxial CuBr is proposed. X-ray techniques including high resolution X-ray diffraction and X-ray pole figures are used to determine the epitaxial relationship. CuBr(100) is also produced on a Ag(100) surface by a AgBr(100) buffer layer that is rotated in-plane 45° relative to the Ag(100) surface. This in-plane rotation reduces the lattice mismatch from +39.5% for an unrotated film to −1.4% for a 45° rotated film.

Crystal quality improvement of ZnTe (1 1 0) thin film prepared on sapphire by increasing nuclei density on substrate surface

ZnTe thin films were prepared on r, S-plane nanofacet substrates to achieve a high-crystal-quality layer with a (110) orientation. Scanning electron microscopy was used to study the nucleation process. Selective formation of growth nuclei can be achieved by controlling the substrate temperature. The low-temperature grown amorphous layers changed to nuclei by annealing. The surface amorphous layer was completely removed when the annealing temperature was too high. Zn beam irradiation during the annealing removed materials selectively from the r-nanofacet. Migration-enhanced epitaxy (MEE) was introduced to enlarge the nuclei size, and a thick-layer growth by conventional molecular beam epitaxy (MBE) followed. The MEE sequence was increased up to 1200 cycles, and the substrate temperature for MEE and MBE was set to higher temperatures than the conventional MBE substrate temperature (the conventional substrate temperature was around 340 °C). The crystal quality of the thin film was analyzed using the X-ray pole figure, θ–2θ measurements and photoluminescence. (110) oriented layer formation perpendicular to the substrate surface was confirmed after introducing those techniques. The low-temperature photoluminescence measurement indicated the high quality of the thick layer.

The effect of orientation and pore size on nano mechanical behaviour of Ag thin films: a comparison between experiment and atomistic simulation

ABSTRACT This paper describes the thickness-dependent texture evolution during annealing in Ag thin films, commonly used in micro and nano-devices. The effect of porosity and crystal orientation on mechanical properties for the films deposited by the magnetron sputtering method is particularly addressed using nano-indentation experiment and atomistic simulation. X-ray pole figure analysis revealed that the films exhibited sharp fibre texture with a major <1 1 1> component accompanied by minor twin components of <5 1 1> and <5 7 13> and a weak component of <1 0 0>. The mechanical behaviour of the films was investigated experimentally using a Berkovich tip to measure the hardness (H) and modulus of elasticity (E) at each individual grain and porous region. The average Young’s modulus of strongly oriented [1 1 1] grain at porous and non-porous regions is estimated to be 44 ± 7 and 67 ± 5 GPa. Molecular Dynamics simulations have been performed on (1 1 1), (1 1 0), (0 0 1), (5 1 1), and (5 7 13) surfaces of Ag single crystal using a spherical indenter to investigate the anisotropic nature of hardness and elastic modulus from the Load∼Indentation depth curves. The mechanical properties of [1 1 1] oriented single crystal in the presence of a sub-surface void have been studied. Our results have demonstrated that the void acts as an efficient absorber of dislocation limiting the extension of the plastic zone. The simulated modulus of elasticity (E: 54.2 GPa) results obtained at a temperature of 300 K in the presence of a void are compared with experimentally measured values with a variation of around 6%.

Single-crystal-like germanium thin films on large-area, compliant, light-weight, flexible, single-crystal-like substrates.

Germanium (Ge) films were heteroepitaxially grown on flexible, large-area, single-crystal-like metallic substrates. Multiple, heteroepitaxial, buffer layers of nanoscale dimensions were deposited on the triaxially textured, single-crystal-like, thermo-mechanically processed Ni-W alloy substrates. Ge films were deposited on a CeO2-terminated, heteroepitaxial buffer stack on the metallic substrate using electron beam evaporation. X-ray diffraction θ-2θ scans showed a very strong Ge (400) peak and the full width at half-maximum (FWHM) of the Ge (400) rocking curve was 0.93°. The Ge (111) ϕ-scan showed a FWHM value ∼4°. Based on the X-ray ω-scan, ϕ-scan and (111), (110), and (001) X-ray pole-figures, the Ge film deposited on the flexible, metallic substrate had a cube-on-cube heteroepitaxial relationship with the single-crystal-like metallic substrate. Reflection-high-energy-diffraction (RHEED) patterns from the Ge layer was streaky indicative of a smooth and essentially single-crystal-like Ge film. Cross-section TEM examination revealed a sharp interface between the Ge film and the topmost buffer layer, CeO2, with a low defect density. The CeO2 layer serves as a highly compliant layer that modulates its lattice parameter to attain excellent lattice-matching to the heteroepitaxial Ge layer. Ge films grown on these flexible metal substrates exhibited electron mobilities in the range of 175-250 cm2V-1s-1. Such single-crystal-like semiconductor films on low-cost, flexible, large-area, scalable, single-crystal-like metallic substrates could potentially enable high-performance electronic devices for a range of applications.

Global Crystallographic Texture of Freshwater Bivalve Mollusks of the Unionidae Family from Eastern Europe Studied by Neutron Diffraction.

The crystallographic texture of the whole valves of bivalve mollusks from the family Unionidae Unio pictorum Linnaeus, 1758 and Anodonta cygnea Linnaeus, 1758 is studied using pole figures measured using neutron diffraction. The use of neutron diffraction, in contrast to X-rays, makes it possible to study the valves without destroying them. Thus, we can discuss the study of the global texture of the entire valve. It was revealed that the pole figures of aragonite in the valves repeat their shape. The pole density maxima for U. pictorum from the Danube Delta and the Gulf of Finland in the Baltic Sea, living at different salinities and temperatures, differs by 0.41 mrd. The maximum value of the crystallographic texture for A. cygnea from the Danube Delta was also measured (5.07 mrd). In terms of texture sharpness, it surpasses the shell of marine bivalve mollusks, which are partially or completely composed of aragonite. Although U. pictorum and Mya arenaria Linnaeus, 1758 have different microstructures, their pole figures are very similar in isolines pattern, but differ in pole density maxima. No relationship was found between the crystallographic texture and the microstructure in U. pictorum. In addition, we report good qualitative agreement between aragonite X-ray pole figures of Sinanodonta woodiana Lea, 1834 from the Czech river Luznice, and neutron pole figures of U. pictorum from the Danube Delta.

Oblique angle co-deposition of nanocolumnar tungsten thin films with two W sources: Effect of pressure and target current

Two series of tungsten thin films are sputtered on silicon and glass substrates by oblique angle co-deposition technique with an original configuration. Two opposite distinct tungsten targets are simultaneously used, both tilted with an oblique angle of 80°. The growth is performed at low (0.33 Pa) and high (1.5 Pa) argon sputtering pressure and the current intensity applied to the targets varies between 50 and 250 mA. The effect of these deposition parameters on the films microstructure and electrical properties is investigated by scanning and transmission electron microscopy, X-ray diffraction and pole figures, and van der Pauw method. Due to self-shadowing effect, all tungsten sputtered thin films are porous and columnar. At low pressure, the columnar tilt angle β can be tuned with the target current intensity until obtaining vertical columns. X-ray diffraction and pole figure analyses point out a A15 crystal structure (β-W) and a uniaxial fiber texture with a <100> growth direction. In contrast, tungsten thin films deposited at high pressure present a cauliflower structure and are poorly crystallized. Both deposition parameters also affect the films electrical resistivity and anisotropy. These behaviors are discussed and linked to the microstructure and crystallography.

Epitaxial Electrodeposition of 2D-Layered BiI3 and Conversion to Highly Ordered Bi-Based Organic−Inorganic Halide-Based Perovskites

Highly-ordered, epitaxial semiconductor thin films have low defect densities and excellent photo-physical properties that are desired for optoelectronic devices. Single crystalline perovskite materials are known to provide lower trap densities, a larger diffusion length, and higher photo-conversion efficiencies in perovskite solar cells.However, the preparation of cost-effective, highly ordered semiconductor films with a uniform surface morphology, low electron−hole recombination, and low trap densities remains a bottleneck to achieve higher device efficiencies in large-area electronics. Electrodeposition is a deposition route that is highly scalable and provides a variety of deposition parameters such as potential, pH, temperature, and additives that can be tuned to produce highly ordered epitaxial films with controlled morphologies.Bismuth triiodide, BiI3, is a 2D-metal halide semiconductor that crystallizes in a R3̅ (H) space group symmetry with lattice parameters of a = b = 0.7516 nm, c = 2.0718 nm. BiI3 possesses a structure with repeating units of the I−Bi−I plane, in which a monolayer of Bi atoms is sandwiched between two layers of iodide with strong Bi−I ionic bonds. We deposited epitaxial BiI3 films on Au(111) substrate electrochemically by reducing I2 in the presence of Bi3+. The epitaxial films of the solar light-absorbing perovskite (CH3NH3)3Bi2I9 are produced in a solution from BiI3 by topotactic transformation. Our deposition methods are outlined in figure 1. Epitaxially grown BiI3 on Au(111) shows highly ordered [001] out-of-plane orientation having the epitaxial relationship with the substrate as BiI3(0001)[1̅1̅20 ± 3°]//Au(111)[1̅1̅2], determined by X-ray pole figures. The lattice mismatch is minimized by the (±)3° rotation of the film relative to the substrate. The X-ray rocking curve shows that single-crystal-like BiI3 has a mosaic spread with full width at half-maximum (FWHM) of about ∼ 0.69°. The topotactic transformation of BiI3 produces a highly ordered [001]-oriented epitaxial perovskite (CH3NH3)3Bi2I9. The band gaps of BiI3 and converted (CH3NH3)3Bi2I9 film are measured using Tauc plot and found to be Eg ~ 1.76 eV and Eg ~ 2.15 eV.

New Features in Crystal Orientation and Phase Mapping for Transmission Electron Microscopy

ACOM/TEM is an automated electron diffraction pattern indexing tool that enables the structure, phase and crystallographic orientation of materials to be routinely determined. The software package, which is part of ACOM/TEM, has substantially evolved over the last fifteen years and has pioneered numerous additional functions with the constant objective of improving its capabilities to make the tremendous amount of information contained in the diffraction patterns easily available to the user. Initially devoted to the analysis of local crystallographic texture, and as an alternative to both X-ray pole figure measurement and EBSD accessories for scanning electron microscopes, it has rapidly proven itself effective to distinguish multiple different phases contained within a given sample, including amorphous phases. Different strategies were developed to bypass the inherent limitations of transmission electron diffraction patterns, such as 180° ambiguities or the complexity of patterns produced from overlapping grains. Post processing algorithms have also been developed to improve the angular resolution and to increase the computing rate. The present paper aims to review some of these facilities. On-going works on 3D reconstruction are also introduced.

Thermal conductivity across the van der Waals layers of α-MoO3 thin films composed of mosaic domains with in-plane 90° rotations

α-Molybdenum trioxide (α-MoO3) is a typical two-dimensional metal oxide material, in which the covalently bonded layers are bonded by van der Waals forces. Herein, the thermal conductivities across the van der Waals layers of α-MoO3 thin films with nominal thicknesses of 50, 100, and 125 nm were investigated. The α-MoO3 thin films were fabricated on the (100) plane of a single-crystalline SrTiO3 substrate heated up to 400 °C by DC reactive magnetron sputtering using a Mo metal target. The b-axis-oriented α-MoO3 thin films epitaxially grown on the SrTiO3 (100) plane were confirmed by x-ray diffraction and x-ray pole figure analyses. Electron diffraction patterns and plane-view transmission electron micrographs revealed that the α-MoO3 thin films were composed of mosaic domains with a diameter of ∼2 nm, with each domain rotated in-plane by 90° with respect to the neighboring one. The mean thermal conductivity across the van der Waals layers of the three α-MoO3 thin films was evaluated to be 1.2 ± 0.3 W m−1 K−1, which is comparable to the reported thermal conductivities of layered cobalt oxide thin films. The reduced thermal conductivity is mainly due to phonon scattering at domain boundaries lying in the in-plane direction.

Twinned growth of ScN thin films on lattice-matched GaN substrates

Scandium nitride (ScN) has attracted significant interest in recent years for diverse electronic and thermoelectric applications. Most ScN growth utilizes MgO and Al2O3 as substrates that lead to extended defects such as dislocations and grain boundaries. (0001) GaN exhibits less than 0.1% lattice mismatch with (111) ScN, and therefore, should result in single-crystalline ScN film growth. However, not much attention is devoted to understanding the microstructure of ScN on GaN substrates. In this work, we present (111) oriented lattice matched ScN film growth on (0001) GaN substrates. X-ray pole figure exhibited six spots for the (002) ScN superimposed on that of (101) GaN separated by 60° corresponding to twin domains of threefold symmetry for (111) ScN, which are furthermore directly imaged by lattice resolved microscopy images. The presence of twins is attributed to vertical dislocations originating at the GaN/Al2O3 interface and extending throughout the GaN film to its interface with ScN.