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At least 613 records · Page 34

Morphology and property tuning in ZnO–Ni hybrid metamaterials in vertically aligned nanocomposite (VAN) form

ZnO thin films have attracted significant interest in the past decades owing to their unique wide band gap properties, piezoelectric properties, non-linearity and plasmonic properties. Recent efforts have been made in coupling ZnO with secondary phases to enhance its functionalities, such as Au–ZnO nanocomposite thin films with tunable optical and plasmonic properties. In this work, magnetic nanostructures of Ni are incorporated in ZnO thin films in a vertically aligned nanocomposite (VAN) form to couple magnetic and plasmonic response in a complex hybrid metamaterial system. Nickel (Ni) is of interest due to its ferromagnetic and plasmonic properties along with gold (Au) which is also plasmonic. Therefore, two approaches, namely, tuning of the deposition pressure and use of a ZnO–Au seeding layer have been attempted to achieve unique Ni nanostructures in addition to tuning of the microstructure. Together, both approaches demonstrate a range of microstructures such as core–shell, nanodisk, nanocup, and nanocube-like morphologies not previously attempted. Additionally, there is effective tuning of properties. Specifically, the seeding layer thickness causes hyperbolic behavior as well as redshift in the surface plasmon resonance (SPR) wavelength. The addition of the ZnO–Au seeding layer directly influences the optical properties. Plus, regardless of the different approaches, the films demonstrate magnetic anisotropy based on the composition and microstructure of the film which impacted the saturation magnetization and coercivity. This study demonstrates the potential of ZnO-based complex hybrid metamaterials with coupled electro-magneto-optical properties for integrated photonic devices.

Bhatt, Nirali A. [Purdue Univ., West Lafayette, IN↗

Fabrications and application of single crystalline GaN for high-performance deep UV photodetectors

High-quality single crystalline Gallium Nitride (GaN) semiconductor has been synthesized using molecule beam epitaxy (MBE) technique for development of high-performance deep ultraviolet (UV) photodetectors. Thickness of the films was estimated by using surface profile meter and scanning electron microscope. Electronic states and elemental composition of the films were obtained using Raman scattering spectroscopy. The orientation, crystal structure and phase purity of the films were examined using a Siemens x-ray diffractometer radiation. The surface microstructure was studied using high resolution scanning electron microscopy (SEM). Two types of metal pairs: Al-Al, Al-Cu or Cu-Cu were used for interdigital electrodes on GaN film in order to examine the Schottky properties of the GaN based photodetector. The characterizations of the fabricated prototype include the stability, responsivity, response and recovery times. Typical time dependent photoresponsivity by switching different UV light source on and off five times for each 240 seconds at a bias of 2V, respectively, have been obtained. The detector appears to be highly sensitive to various UV wavelengths of light with very stable baseline and repeatability. The obtained photoresponsivity was up to 354 mA/W at the bias 2V. Higher photoresponsivity could be obtained if higher bias was applied but it would unavoidably result in a higher dark current. Thermal effect on the fabricated GaN based prototype was discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

An embedded interfacial network stabilizes inorganic CsPbI3 perovskite thin films

Abstract The black perovskite phase of CsPbI 3 is promising for optoelectronic applications; however, it is unstable under ambient conditions, transforming within minutes into an optically inactive yellow phase, a fact that has so far prevented its widespread adoption. Here we use coarse photolithography to embed a PbI 2 -based interfacial microstructure into otherwise-unstable CsPbI 3 perovskite thin films and devices. Films fitted with a tessellating microgrid are rendered resistant to moisture-triggered decay and exhibit enhanced long-term stability of the black phase (beyond 2.5 years in a dry environment), due to increasing the phase transition energy barrier and limiting the spread of potential yellow phase formation to structurally isolated domains of the grid. This stabilizing effect is readily achieved at the device level, where unencapsulated CsPbI 3 perovskite photodetectors display ambient-stable operation. These findings provide insights into the nature of phase destabilization in emerging CsPbI 3 perovskite devices and demonstrate an effective stabilization procedure which is entirely orthogonal to existing approaches.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The structure of ion plated films in relation to coating properties

Ion plating is an ion assisted or glow discharge deposition technique, where ions or energetic atoms transfer energy, momentum and charge to the substrate and the growing film in a manner which can be controlled to favorably modify surface, subsurface chemistry, and microstructure. The glow discharge energizing effects from the initial nucleation stages to the final film growth are discussed. As a result, adherence, coherence, internal stresses, density and morphology of the coatings are significantly improved, over the conventional (nonion-assisted) techniques which in turn favorably affect the surface initiated failures caused by friction, wear, erosion, corrosion and fatigue. Ion plated films because of their graded coating/substrate interface, fine, uniform, densely packed film structure also induce a surface strengthening effect which improved the mechanical properties such as yield, tensile strength and fatigue life. Since a uniform, continuous film can be obtained at lower nominal film thickness, this effect is of great importance in solid film lubrication and in corrosion protection.

Spalvins, T.↗

The Microstructure and Pitting Resistance of Weld Joints of 2205 Duplex Stainless Steel

2205 duplex stainless steel (DSS) was welded by submerged arc welding. The effects of both heat input and groove type on the ferrite/austenite ratio and elemental diffusion of weld joints were investigated. The relationships among welding joint preparation, ferrite/austenite ratio, elemental diffusion, and pitting corrosion resistance of weld joints were analyzed. When the Ni content of the weld wire deposit was at minimum 2–4% higher than that of 2205 DSS base metal, the desired ratio of ferrite/austenite and elemental partitioning between the austenite and ferrite phases were obtained. While the pitting sensitivity of weld metal was higher than that of base metal, the self-healing capability of the passive film of weld metal was better than that of the base metal when a single V-type groove was used. Furthermore, the heat input should be carefully controlled since pitting corrosion occurred readily in the coarse-grained heat-affected zone near the fusion line of welded joints.

36 MATERIALS SCIENCE↗

The effect of annealing on optical transmittance and structure of ZLANI fluorozirconate glass thin films

In this work, we report the effect of thermal annealing on structure, composition, optical transmittance and thickness of a novel fluorozirconate glass (ZLANI) containing Zr, La, Al, Na and In fluorides. In this work, pulsed laser depo- sition was used to grow thin films of ZLANI, and thermal annealing at different temperatures was performed on the films. Annealing did not change the composition, but a clear structural evolution of the ZLANI glass was observed by transmission electron microscopy (TEM), showing that we can control microstructure independent of composition. An increase in transmittance after the film was subject to a 100 °C thermal anneal was ascribed to the removal of defects and structural relaxation in the amorphous state. Following an anneal of 200 °C, the transmittance decreases due to heterogeneous formation of crystalline nuclei and changes in the local bonding. After the final annealing at 300 °C, a wider-scale crystallization occurred, with some major crystal phases formed as Zr 2 F 8 (H 2 O) 6 and ZrO 2 , which alters the shape of the transmittance curve. The crystalline content of the crystal phases that form in the annealed films was quantified using hollow cone dark field TEM imaging. The 100 °C or 200 °C annealing decreases the film thickness by inducing structural relaxation and densification of the amorphous films, while the thickness increase of the 300 °C annealed film resulted from the formed large crystals. These results provide insights for the design of multilayer nanocomposites with a ZLANI glass matrix, which have potential applications as up-/down-conversion luminescent materials and X-ray storage phosphors.

36 MATERIALS SCIENCE↗

Titanium-deposition assisted brazing of SiC ceramics using inactive AgCu filler

Highlights: • Reliable joint of SiC ceramics was achieved via Titanium-deposition assisted brazing using inactive AgCu filler metal. • Microstructure characteristic of deposited-SiC brazed joint was investigated in detail. • Ti-deposition assisted brazing inhibited the formation of numerous intermetallic compounds. - Abstract: In this study, active titanium element film was designed to deposit on SiC ceramics directly to enhance the brazability of inactive AgCu brazing alloy on ceramics. The result showed the reliable joint was successfully obtained and the deposition of titanium film on SiC directly inhibited the formation of amounts of intermetallic compounds effectively in the brazing seam. Detailed interfacial microstructure of joint investigated by scanning electron microscope equipped with energy dispersive spectrum analysis and transmission electron microscope revealed that the interfacial reactions were based on deposited Ti film. The typical joint was SiC/TiCu + Ti{sub 2}Cu/TiC/Ti{sub 5}Si{sub 3} containing TiC particles/Ag(s,s) + Cu(s,s)/Ti{sub 5}Si{sub 3} containing TiC particles/TiC/TiCu + Ti{sub 2}Cu/SiC.

36 MATERIALS SCIENCE↗

Effect of Heat Treatment on Microstructure and Mechanical Properties of Stellite 12 Fabricated by Laser Additive Manufacturing

Microstructure evolution and wear resistance of Stellite 12 produced by laser additive manufacturing were studied in untreated and heat-treated conditions. In untreated conditions, cobalt matrix dendrites and inter-dendritic eutectic carbides were the primary microstructure, blocky and lamellar eutectic carbides can be found, and M{sub 7}C{sub 3} and M{sub 23}C{sub 6} are the primary carbides. Heat treatment can modify the microstructure of this alloy. Primary carbides were dissolved into the cobalt matrix after solution treatment. Aging treatment resulted in the precipitation of carbides, the transformation of M{sub 7}C{sub 3} into M{sub 23}C{sub 6} carbides, and the increase in microhardness. Solution and aging treatment can also cause the precipitation of carbides, but the morphology and distribution of carbides were absolutely different. The wear resistance of untreated samples at room temperature (RT) and 600 °C is better than that at 200 and 400 °C due to the high hardness at RT and the formation of oxide film at 600 °C. The wear resistance of heat-treated samples was tested at 600 °C; it was dominated by the formation and flake-off of oxide film. The sample that underwent solution plus aging treatment has a superior wear resistance.

36 MATERIALS SCIENCE↗

Microstructural, Oxidation, and Mechanical Behavior of NbTi-Based Refractory Alloys with 5 to 10 Pct Co, Cr, and Ni Additions

NbTi-based refractory alloys with additions of Co, Cr, and Ni represent an interesting medium-entropy alloy system with potential for protective oxide film formation, high strength, and ductility. This study investigates the microstructural evolution, oxidation behavior, and mechanical properties of NbTi-based alloys containing 5 to 10 at. pct Co, Cr, and Ni. CALPHAD predictions suggest that this composition range can be heat treated to obtain a predominantly body-centered cubic matrix phase. Mechanical properties, including microhardness, yield strength, maximum strength, and specific strength are evaluated through isothermal compression tests conducted between room temperature and 800 °C. The oxidation kinetics of these alloys are assessed through discontinuous oxidation tests. Parabolic oxidation kinetics were observed for NbTi–10Ni and NbTi–5Co, while linear oxidation kinetics were found for NbTi–10Cr and NbTi–10(CoCrNi). Microstructures and oxide layers are characterized using X-ray diffraction, electron backscatter diffraction, energy-dispersive X-ray spectroscopy, and scanning electron microscopy. All alloys exhibit significant mechanical softening between room temperature and 800 °C, with elastic-perfectly plastic flow observed at 800 °C. The addition of 10 pct Cr to NbTi resulted in two BCC phases up to 1050 °C, conflicting with CALPHAD predictions of a single-phase solid solution at this temperature, and resulting in higher flow stress at 800 °C. NbTi–10(CoCrNi) exhibited the lowest flow stress at 800 °C despite having more ‘cocktail effect’ potential and insufficient molar fractions of Co, Cr, or Ni to form a desirable protective oxide film.

36 MATERIALS SCIENCE↗

Microstructural characterization of Charpy-impact-tested nanostructured bainite

In this work, a possible cause of the extraordinary low impact toughness of nanostructured bainite has been investigated. The microstructure of nanostructured bainite consisted chiefly of carbide-free bainitic ferrite with retained austenite films. X-ray diffractometry (XRD) measurement indicated that no retained austenite existed in the fractured surface of the Charpy-impact-tested specimens. Fractographs showed that cracks propagated mainly along bainitic ferrite platelet boundaries. The change in microstructure after impact loading was verified by transmission electron microscopy (TEM) observations, confirming that retained austenite was completely transformed to strain-induced martensite during the Charpy impact test. However, the zone affected by strained-induced martensite was found to be extremely shallow, only to a depth of several micrometers from the fracture surface. It is appropriately concluded that upon impact, as the crack forms and propagates, strain-induced martensitic transformation immediately occurs ahead of the advancing crack tip. The successive martensitic transformation profoundly facilitates the crack propagation, resulting in the extremely low impact toughness of nanostructured bainite. Retained austenite, in contrast to its well-known beneficial role, has a deteriorating effect on toughness during the course of Charpy impact. - Highlights: • The microstructure of nanostructured bainite consisted of nano-sized bainitic ferrite subunits with retained austenite films. • Special sample preparations for SEM, XRD and TEM were made, and the strain-affected structures have been explored. • Retained austenite films were found to transform into martensite after impact loading, as evidenced by XRD and TEM results. • The zone of strain-induced martensite was found to extend to only several micrometers from the fracture surface. • The poor Charpy impact toughness is associated with the fracture of martensite at a high strain rate during impact loading.

36 MATERIALS SCIENCE↗

Solid-Solution CrCoCuFeNi High-Entropy Alloy Thin Films Synthesized by Sputter Deposition

The concept of high configurationally entropy requires that the high-entropy alloys (HEAs) yield single-phase solid solutions. However, phase separations are quite common in bulk HEAs. A five-element alloy, CrCoCuFeNi, was deposited via radio frequency magnetron sputtering and confirmed to be a single-phase solid solution through the high-energy synchrotron X-ray diffraction, energy-dispersive spectroscopy, wavelength-dispersive spectroscopy, and transmission election microscopy. The formation of the solid-solution phase is presumed to be due to the high cooling rate of the sputter-deposition process.

Microstructure↗

Surface Layers of Zr-18%Nb Alloy Modified by Ultrasonic Impact Treatment: Microstructure, Hardness and Corrosion

Near-surface layers in Zr-18%Nb alloy were modified using ultrasonic impact treatment (UIT). The effects of the UIT processing time on a microstructural formation, omega/alpha precipitations, microhardness and corrosion are analyzed. XRD analysis, TEM and SEM observations and EDX characterization allow establishing the links between the microstructure, microhardness and corrosion behavior of the surface layers formed. At the strain extent up to e ≈ 0.3, structural formation occurs under influence of deformation induced heating, which facilitates omega precipitation in beta phase and mechanically induced oxygen transport and oxide formation. XRD analysis reveals moderate compressive residual stresses (− 160 MPa) and pronounced {110} texture after the UIT process. Generation of dislocations and hindering of their movement by nanoscale omega precipitates manifest themselves as the broadening of diffraction peaks occurred mainly owing to the lattice microstrains, and they provide marked strain hardening. The enhanced anticorrosion properties of Zr-18%Nb alloy in saline solution were concluded to be a result of the formation of a protective oxide film, {110} texture and compressive stresses.

36 MATERIALS SCIENCE↗

Exploring the relationship between deposition method, microstructure, and performance of Nb/Si-based superconducting coplanar waveguide resonators

Superconducting quantum circuits (SQC) are one of the most promising hardware platforms for quantum computing, yet their performance is currently limited by the presence of various structural defects inside the circuit's structure. Despite impressive progress in the past decade, a precise understanding of the origin of these defects from various fabrication processes and their impact on coherence is still lacking. Here, in this study, we performed a comprehensive investigation on the microstructure, superconductivity, and resonator quality factor of Nb films deposited by high-power impulse magnetron sputtering (HiPIMS) and direct current (DC) magnetron sputtering. A suite of characterization techniques, including electron microscopy with spectroscopy, secondary ion mass spectrometry, magneto-optical microscopy, and pump-probe reflectivity spectroscopy is used. We reveal that niobium (Nb) resonators fabricated using HiPIMS exhibit a smaller average grain size, thicker surface oxide with larger thickness variations (rougher surface), and a thicker amorphous Nb/Si interface layer compared to samples deposited by DC sputtering. We identified that the amorphous Nb oxides (mainly located at the Nb surface and along the grain boundaries) and Nb-Si amorphous layers (at the Nb/Si interface) are major and potential sources of two-level system (TLS), while off-stochiometric oxides and suboxides of Nb close to the surface, crystalline defects (i.e., dislocations at grain boundary, point defects introduced during deposition) are main contributors of non-TLS sources. Our findings clarify the relationship between different defects and coherence loss mechanisms, highlighting the importance of material microstructure control on performance optimization in SQC.

36 MATERIALS SCIENCE↗

Optical properties of Mn-Co-Ni-O thin films prepared by radio frequency sputtering deposition

Mn{sub 1.4}Co{sub 1.0}Ni{sub 0.6}O{sub 4} (MCN) thin films are prepared by RF sputtering deposition method on amorphous Al{sub 2}O{sub 3} substrate. Microstructure and X-ray photoelectron spectroscopy analyses suggest improvements in crystallinity and stoichiometry for MCN films with post-annealed process. Infrared (IR) optical constants of the MCN films are obtained by IR spectroscopic ellipsometer (SE) in the range of 1500 cm{sup −1} to 3200 cm{sup −1} (2.8–6.7 μm). The derived effective charge supports the increase of the oxidation after annealing. The dielectric function of the films is also extracted by SE in the range of 300–1000 nm adopting a double Lorentz model together with a Tauc–Lorentz model. The mechanism in electronic transition process is discussed based on the variation observed in the optical absorption spectra of the as-grown and post-annealed samples. The optical absorption peaks located at 1.7 eV, 2.4–2.6 eV, and 3.5–4 eV are attributed to the charge-transfer transitions of 2p electrons of oxygen ions and 3d electrons of Mn and Co ions. Our results are very important to understand the optoelectronic mechanism and exploit applications of metal oxides.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Exploring the First High-Entropy Thin Film Libraries: Composition Spread-Controlled Crystalline Structure

Thin films of two types of high-entropy oxides (HEOs) have been deposited on 76.2 mm Si wafers using combinatorial sputter deposition. In one type of the oxides, (MgZnMnCoNi)O x , all the metals have a stable divalent oxidation state and similar cationic radii. In the second type of oxides, (CrFeMnCoNi)O x , the metals are more diverse in the atomic radius and valence state, and have good solubility in their sub-binary and ternary oxide systems. Therefore, the resulting HEO thin films were characterized using several high-throughput analytical techniques. The microstructure, composition, and electrical conductivity obtained on defined grid maps were obtained for the first time across large compositional ranges. The crystalline structure of the films was observed as a function of the metallic elements in the composition spreads, that is, the Mn and Zn in (MgZnMnCoNi)O x and Mn and Ni in (CrFeMnCoNi)O x . The (MgZnMnCoNi)O x sample was observed to form two-phase structures, except single spinel structure was found in (MgZnMnCoNi)O x over a range of Mn > 12 at. % and Zn < 44 at. %, while (CrFeMnCoNi)O x was always observed to form two-phase structures. Composition-controlled crystalline structure is not only experimentally demonstrated but also supported by density function theory calculation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Two-Magnon Relaxation Processes in Nanocrystalline Thin Magnetic Films

Numerical analysis of the micromagnetic model was used to reveal the ‘resonance’ feature of relaxation processes in nanocrystalline thin magnetic films. This feature manifests itself in the form of sharp broadening of the ferromagnetic resonance (FMR) line at a certain frequency f{sub 1} depending on magnetic characteristics of the film, and is observed only in films the thickness of which exceeds some threshold value d{sub min}. Sharp broadening of the FMR line is accompanied by significant shift of the resonance field, whereas the shift value changes the sign at frequency ~ f{sub 1}. It was shown analytically that the nature of observed effects is associated with the two-magnon process of spin waves scattering on quasi-periodic magnetic microstructure – magnetization ‘ripple’. Obtained expressions for the threshold value of film thickness d{sub min} and frequency of maximum broadening of FMR line f{sub 1} agree well with the results of numerical computation of micromagnetic model.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Evaluation of Alternative Atomistic Models for the Incipient Growth of ZnO by Atomic Layer Deposition

ZnO thin films are interesting for applications in several technological fields, including optoelectronics and renewable energies. Nanodevice applications require controlled synthesis of ZnO structures at nanometer scale, which can be achieved via atomic layer deposition (ALD). However, the mechanisms governing the initial stages of ALD had not been addressed until very recently. Investigations into the initial nucleation and growth as well as the atomic structure of the heterointerface are crucial to optimize the ALD process and understand the structure-property relationships for ZnO. We have used a complementary suite of in situ synchrotron x-ray techniques to investigate both the structural and chemical evolution during ZnO growth by ALD on two different substrates, i.e., SiO2 and Al2O3, which led us to formulate an atomistic model of the incipient growth of ZnO. The model relies on the formation of nanoscale islands of different size and aspect ratio and consequent disorder induced in the Zn neighbors' distribution. However, endorsement of our model requires testing and discussion of possible alternative models which could account for the experimental results. In this work, we review, test, and rule out several alternative models; the results confirm our view of the atomistic mechanisms at play, which influence the overall microstructure and resulting properties of the final thin film.

ALD↗

Phase evolution and amorphous stability upon solid-state reaction in superlattice like Ge–Sb–Te combinatorial thin-film

In this paper, the superlattice-like (SLL) Ge–Sb–Te combinatorial thin films were prepared by using a high-throughput ion beam sputtering system. The phase evolution and amorphous stability of such films undergoing heat treatment as a function of the coating sequence and modulation period were systematically studied. The composition structure diagram was constructed via an automated process of data obtained by high-throughput synchrotron micro-X-ray diffraction and lab-based micro-X-ray fluorescence. Furthermore, the element distribution and microstructure in the depth direction of the SLL thin films were characterized with time-of-flight secondary ion mass spectrometry and transmission electron microscopy, respectively. These studies demonstrated that the coating sequence has a significant effect on the element distribution in the as-deposited SLL thin films and the structure of the final product upon solid-state reaction. Reducing the modulation period of the SLL thin film improves the stability of the amorphous Ge–Sb–Te phase. This work lays a solid foundation for the rational design of SLL Ge–Sb–Te thin films to improve their performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗