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At least 793 records · Page 44

Improvement of reliability and power consumption for SnSb{sub 4} phase change film composited with Ga{sub 3}Sb{sub 7} by superlattice-like method

Superlattice-like (SLL) SnSb{sub 4}/Ga{sub 3}Sb{sub 7} (SS/GS) thin films were investigated through in-situ film resistance measurement. The optical band gap was derived from the transmittance spectra by using a UV-visible-NIR (ultraviolet-visible-near infrared) spectrophotometer. Transmission electron microscopy was used to observe the micro-structure before and after annealing. Phase change memory cells based on the SLL [SS(3 nm)/GS(4.5 nm)]{sub 7} thin films were fabricated to test and verify the operation consumption and switching endurance. The scanning thermal microscopy was used to probe the nanoscale thermal property.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

An Overview of Nano Multilayers as Model Systems for Developing Nanoscale Microstructures

The microstructural transformations of binary nanometallic multilayers (NMMs) to equiaxed nanostructured materials were explored by characterizing a variety of nanoscale multilayer films. Four material systems of multilayer films, Hf-Ti, Ta-Hf, W-Cr, and Mo-Au, were synthesized by magnetron sputtering, heat treated at 1000 °C, and subsequently characterized by transmission electron microscopy. Binary systems were selected based on thermodynamic models predicting stable nanograin formation with similar global compositions around 20–30 at.%. All NMMs maintained nanocrystalline grain sizes after evolution into an equiaxed structure, where the systems with highly mobile incoherent interfaces or higher energy interfaces showed a more significant increase in grain size. Furthermore, varying segregation behaviors were observed, including grain boundary (GB) segregation, precipitation, and intermetallic formation depending on the material system selected. The pathway to tailored microstructures was found to be governed by key mechanisms and factors as determined by a film’s initial characteristics, including global and local composition, interface energy, layer structure, and material selection. This work presents a global evaluation of NMM systems and demonstrates their utility as foundation materials to promote tailored nanomaterials.

Appleget, Chelsea D.↗

Dielectric strength of parylene HT

The dielectric strength of parylene HT (PA-HT) films was studied at room temperature in a wide thickness range from 500 nm to 50 μm and was correlated with nano- and microstructure analyses. X-ray diffraction and polarized optical microscopy have revealed an enhancement of crystallization and spherulites development, respectively, with increasing the material thickness (d). Moreover, a critical thickness d{sub C} (between 5 and 10 μm) is identified corresponding to the beginning of spherulite developments in the films. Two distinct behaviors of the dielectric strength (F{sub B}) appear in the thickness range. For d ≥ d{sub C}, PA-HT films exhibit a decrease in the breakdown field following a negative slope (F{sub B} ∼ d{sup −0.4}), while for d < d{sub C}, it increases with increasing the thickness (F{sub B} ∼ d{sup 0.3}). An optimal thickness d{sub optim} ∼ 5 μm corresponding to a maximum dielectric strength (F{sub B} ∼ 10 MV/cm) is obtained. A model of spherulite development in PA-HT films with increasing the thickness is proposed. The decrease in F{sub B} above d{sub C} is explained by the spherulites development, whereas its increase below d{sub C} is induced by the crystallites growth. An annealing of the material shows both an enhancement of F{sub B} and an increase of the crystallites and spherulites dimensions, whatever the thickness. The breakdown field becomes thickness-independent below d{sub C} showing a strong influence of the nano-scale structural parameters. On the contrary, both nano- and micro-scale structural parameters appear as influent on F{sub B} for d ≥ d{sub C}.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Surface and grain boundary carbon heterogeneity in CH 3 NH 3 PbI 3 perovskites and its impact on optoelectronic properties

Rivaling state-of-the-art crystalline silicon, organic-inorganic hybrid perovskites have been intensely studied in recent years. Surface and interfacial engineering have been a focus for performance improvement. Even though significant progress has been made during the last decade in terms of the diversity and capability of perovskite-based devices, the structure-property relationship, particularly at the surface, which governs the real-world performance of these applications, is still unresolved. In the article, this issue was addressed by employing synchrotron-related experimental measurements, and a mechanism that correlates microstructure with surface chemistry was resolved. As a powerful and highly sensitive spectromicroscopy, soft x ray photoemission electron microscopy (X-PEEM) was used to probe the surface of perovskite films varying in post solvent annealing. Furthermore, static and in situ grazing incidence hard x ray diffraction (GIXD) was used to track the grain growth dynamics during the film formation process. It was found that the nature of the surfaces was dictated by the local chemistry that varied due to mass flow during the development of the microstructure. Combining optical and electronic characterizations, it was confirmed that a more homogenous chemistry, i.e., uniform chemical components and properties, along with reduced strain and grain boundary energies, yielded more defect-tolerant films. Grain boundaries were more favorable for screening carriers than those in the control film. Our findings underscore the importance of the uniformity in the surface for developing a chemistry-structure-property relationship in perovskite materials, as well as engineering local chemistry toward high-performance and stable devices.

42 ENGINEERING↗

Automated imaging of the annihilation of a transverse domain wall in patterned magnetic thin films

Imaging the magnetic domain wall behavior in patterned thin films under external stimuli can enable understanding the underlying energy landscape and the role of local microstructure and defects. We present an automated workflow for in situ Lorentz transmission electron microscopy to image magnetic domain walls at the nanometer length scale and at a time resolution in the sub-millisecond regime—the latter of which is limited by the speed of the available camera. Our workflow is modular and can be broadly applied to various types of in situ experiments, taking us a step closer to the future of autonomous imaging of nanomagnetic films with electron microscopy. Using our workflow, we show the transformation of a transverse domain wall with sub-millisecond time resolution under the application of an in situ transverse magnetic field, a study of whose dynamics are essential in the design of future domain wall mediated spintronic device applications.

Algebraic topology↗

Microstructure and 77K mechanical properties of electron beam welded Cu101- Inconel 625 joints

In developing large-scale next-generation superconducting radio frequency (SRF) linear accelerators using superconducting films on Cu, the design and development of dissimilar welding and joining metals, such as Cu to Inconel, stainless steel, and Nb, are essential. In this talk, we present the development of procedures for electron-beam welding of Cu¿Inconel 625 and evaluation of the microstructure and 77K mechanical properties of the weld and base material in the welded condition and heat treatments in the 750°C ¿950°C heat treatment range. The results will be presented in the context of developing joining techniques for low-temperature applications where high conductivity and strength, vacuum hygiene, and magnetic properties of the material need consideration. The methods presented here are being deployed to thin film SRF Cu cavities at Jefferson Lab. Acknowledgment: This material is based upon work supported by the U.S. Department of Energy, Office of Science, Office of Nuclear

Khanal, Bashu↗

Ternary systems based on PVDF, BaTiO{sub 3} and MWCNTs: Fabrication, characterization, electromagnetic simulation

In this work, ternary bulk systems based on polyvinylidene fluoride (PVDF), synthesised barium titanate (BaTiO{sub 3}, BT) nanopowder and multi walled carbon nanotubes (MWCNTs) were fabricated by film stacking technique, starting from solvent cast films. The main purpose was to investigate the influence of BT and MWCNTs addition to the polymeric matrix on its microstructural and dielectrical properties. In order to achieve it, different BT concentrations, ranging between the 60 and 75 %wt, were tested, whereas a MWCNTs content of 2 %wt was maintained constant. The morphology was studied by observation at scanning electron microscopy (SEM), the microstructure and crystalline phases investigated by X-Ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy, and the electromagnetic properties measured in the microwave region (8-12 GHz). The electromagnetic response of the investigated bulk systems was also simulated as function of the sample thickness.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Asymmetric “melting” and “freezing” kinetics of the magnetostructural phase transition in B2-ordered FeRh epilayers

Synchrotron X-ray diffraction was used to study the phase transformation processes during the magnetostructural transition in a B2-ordered FeRh (001)-oriented epilayer grown on MgO by sputtering. Out-of-plane lattice constant measurements within the hysteretic regime of the transition reveal a microstructure consistent with the coexistence of lattice-expanded and contracted phases in spatially distinct regions. It was found that the phase separation is more pronounced during cooling than heating. Furthermore, whilst lattice-expanded domains that span the height of the film can be undercooled by several kelvins, there is no equivalent superheating. This asymmetry between the cooling and heating processes in FeRh is consistent with the difference in the kinetics of generic freezing and melting transitions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Evolution of Local Microstructures: Spatial and Temporal Correlation in Clusters Undergoing 2-Dimensional Diffusion

Diffusion-limited, capillarity-driven, coarsening of precipitates is an important and intensively studied phenomenon. Coarsening can occur among several microstructural constituents ranging from the primary phases to widely dispersed precipitates. Moreover, coarsening of three-dimensional (3-D) phase domains, occurring via mass transport through a two-dimensional (2-D) diffusion field (called mixed-dimensional phase coarsening) is a cooperative phenomenon that is of practical importance, especially in thin film technologies and catalysis. A primary objective of our current work is to focus on the details of evolving microstructures through a study of 'island' formation in heteroepitaxial film/substrate systems. Whereas this work has been designed for space-based coarsening studies, which require long-duration quality microgravity to observe 3-D Ostwald ripening, a significant amount of work has been performed during ground-based studies to observe diffusional coarsening in a liquid-liquid two-phase system. We have performed the experiment at an isopycnic point to maximize exclusion of gravity-based system disturbance. This has allowed observations of 3-D droplets, immobilized by container wall contact, undergoing coarsening by 2-D diffusion for the required long times (approximately 4 months) using a holographic imaging technique. Although such systems may not be as reliant on long-duration microgravity processing as 3-D systems are, they are of direct relevance to so-called mixed-dimensional coarsening and to the study of heterostructures grown by thin-film technique

Curreri, Peter A.↗

Giant magnetoresistance and superparamagnetism in Dy{sub x}Fe{sub 100-x} nanogranular magnetic thin films at room temperature

In this article, Dy{sub x}Fe{sub 100-x} nanogranular (15 ≤ x ≤ 25) thin films have been prepared at ambient temperature by dc magnetron sputtering. The correlation between the microstructure, magneto transport and magnetization properties is discussed. The grain size of Dy (Dysprosium) and Fe (Iron) was measured to be about 2 to 3 nm, respectively and the distribution of grains was homogenous throughout the sample. The magnetoresistance is sensitive to microstructural changes (particle size as well as Dy concentration). At the room temperature, the magnetoresistance [MR %] increased from 0.2 to 2.2 with increase in atomic concentration of Dy from x = 15 to 25 and we obtained maximum 2.2 MR [%] for x = 25 in this series of samples. The magnetization studies have revealed that all the samples are superparamagnetic (SPM) at room temperature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Solid-State Sintering of Core-Shell Ceramic Powders Fabricated by Particle Atomic Layer Deposition

The properties of technical ceramics are highly dependent on their microstructure, which evolves during sintering. Sintering is the process by which ceramic parts are subjected to high temperatures to activate chemical diffusion and the consumption of porosity. During the initial stage of sintering, interparticle necks between neighboring particles form and subsequently increase in size, consuming porosity as the particle centers move closer together. To experimentally determine how this process depends on particle surface composition, particle atomic layer deposition (ALD) was used to deposit a thin film of amorphous aluminum oxide (Al2O3) onto yttria-stabilized tetragonal zirconia (3YSZ) particles, producing core-shell structured powders. The uniformity of the Al2O3 film was confirmed with transmission electron microscopy and energy dispersive spectroscopy. Scanning electron microscopy was used to observe microstructural evolution during sintering, and the dihedral angles of Al2O3 and 3YSZ grains were measured to determine the ratio of interfacial energies between the 3YSZ|3YSZ, 3YSZ|Al2O3, and Al2O3|Al2O3 interfaces. Analysis of the densification kinetics revealed that the initial stage of densification is dependent on the material at the surface of the particles (ie, the Al2O3 film) and is controlled by the diffusion of Al3+ cations through Al2O3. Once the Al2O3 film has coalesced, the sintering behavior is controlled by the densification of the core material (3YSZ). Thus, core-shell powders fabricated by particle ALD sinter by a two-step process where the kinetics are dependent on the material present at interparticle contacts.

alumina↗

Ag induced electromagnetic interference shielding of Ag-graphite/PVDF flexible nanocomposites thinfilms

We report Ag nanoparticle induced Electromagnetic Interference (EMI) shielding in a flexible composite films of Ag nanoparticles incorporated graphite/poly-vinylidene difluoride (PVDF). PVDF nanocomposite thin-films were synthesized by intercalating Ag in Graphite (GIC) followed by dispersing GIC in PVDF. The X-ray diffraction analysis and the high-resolution transmission electron microscope clearly dictate the microstructure of silver nanoparticles in graphite intercalated composite of PVDF matrix. The conductivity values of nanocomposites are increased upto 2.5 times when compared to neat PVDF having a value of 2.70 S/cm at 1 MHz. The presence of Ag broadly enhanced the dielectric constant and lowers the dielectric loss of PVDF matrix proportional to Ag content. The EMI shielding effectiveness of the composites is 29.1 dB at 12.4 GHz for the sample having 5 wt. % Ag and 10 wt. % graphite in PVDF.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Effect of synthesis temperature on the phase formation of NiTiAlFeCr compositionally complex alloy thin films

Here, the synthesis temperature dependent phase formation of Ni 10 Ti 10 Al 25 Fe 35 Cr 20 thin films is compared to a bulk processed sample of identical composition. The as-cast alloy exhibits a dual-phase microstructure which is composed of a disordered BCC phase and AlNiTi-based B2- and/or L2 1 -ordered phase(s). Formation of the BCC phase as well as an ordered AlNi-based B2 phase is observed for a thin film synthesised at 500 °C (ratio of synthesis temperature of thin film to melting temperature of bulk alloy: T/T m = 0.49), which is attributed to both surface and bulk diffusion mediated growth. Post deposition annealing at 900 °C (T/T m = 0.75) of a thin film deposited without intentional heating results in the formation of NiAlTi-based B2 and/or L2 1 -phase(s) similar to the bulk sample, which is attributed to bulk diffusion. Depositions conducted at room temperature without intentional substrate heating (T/T m = 0.20) resulted in the formation of an X-ray amorphous phase, while a substrate temperature increase to 175 °C (T/T m = 0.28) causes the formation of a BCC phase. Atom probe tomography of the thin films deposited without intentional substrate heating and at 175 °C indicates the formation of ~5 nm and ~10 nm FeAl-rich domains, respectively. This can be rationalized based on the activation energy for surface diffusion, as Ti and Ni exhibt 2.5 to 4 times larger activation energy barriers than Al, Fe and Cr. It is evident from the homologous temperature that the phase formation observed at 500 °C (T/T m = 0.49) is a result of both surface and bulk diffusion. As the temperature is reduced, the formation of FeAl-rich domains can be understood based on the differences in activation energy for surface diffusion and is consistent with kinetically limited thin film growth.

36 MATERIALS SCIENCE↗

Sol–gel preparation of well-adhered films and long range ordered inverse opal films of BaTiO{sub 3} and Bi{sub 2}Ti{sub 2}O{sub 7}

Highlights: • Highly adaptable sols are presented for processing of the electroceramic materials BaTiO{sub 3} and Bi{sub 2}Ti{sub 2}O{sub 7}. • High quality thin films are produced by dip coating with good phase control. • Infiltration of cross-linked polystyrene templates led to high quality inverse opals. - Abstract: Barium and bismuth titanate thin films and well-ordered inverse opal films are produced by dip coating from sols containing titanium alkoxides with acetic acid, acetylacetone, methoxyethanol and water. The inverse opal preparations used crosslinked polystyrene opal templates. Heat treatment in air produced tetragonal BaTiO{sub 3} or mixtures of the hexagonal and tetragonal phases, or phase pure Bi{sub 2}Ti{sub 2}O{sub 7}. Good quality films were obtained with a thickness of 5 μm from a single dipping, and the thickness could be increased by dipping multiple times. Inverse opals were well ordered and exhibited opalescence and photonic stop band effects.

36 MATERIALS SCIENCE↗

Niobium addition improves the corrosion resistance of TiHfZrNb x high-entropy alloys in Hanks’ solution

High-strength TiHfZrNb x high-entropy alloys could become the ideal materials for small-diameter endovascular stents once their corrosion resistance in the physiological milieu is confirmed. Here, this work aims at evaluating the corrosion resistance of a TiHfZrNb x high-entropy-alloys family in Hanks’ solution at 37 °C and revealing the influence of niobium on the mechanisms of dissolution and passivation. The alloys were subjected to a series of static and dynamic electrochemical tests and surface characterization, employing the static/dynamic/cyclic polarizations, impedance spectroscopy, XPS, AFM, and SEM. Results confirm a higher corrosion resistance of the alloys compared to that of CP-Ti and Ti6Al4V. The addition of niobium considerably improves the microstructural homogeneity that ensures a low dissolution rate and a greater resistance of the film due to the lower concentration of point defects. The passive film behaves as an n-type semiconductor and is composed of a mixture of TiO 2 , Nb 2 O 5 , ZrO 2 , and HfO 2 oxides, with the presence of metallic hydroxides on the outermost layer. A detailed description of the niobium influence on the mechanisms of the dissolution and passivation is presented in this work.

36 MATERIALS SCIENCE↗

Enhancing the tensile properties of EBM as-built thin parts: Effect of HIP and chemical etching

Highlights: • The EBM process leads to important cross section variations in thin parts. • Stress calculation must be based on the average section in order to be relevant. • As-built state has a detrimental effect on every mechanical property. • Mechanical properties of machined samples are met with chemical etching. • HIP has a beneficial effect on the ductility. - Abstract: As-built Ti-6Al-4 V thin parts were manufactured using Electron Beam Melting (EBM) and characterized by optical microscopy and laboratory X-ray tomography in order to observe their microstructure, pore distribution and surface aspect. Chemical etching and HIP post-treatments were applied to as-built samples and their effect on the material and static mechanical properties were studied. Tensile tests were performed on both as-built and post-treated samples and their results compared to the ones reported in the literature for machined EBM samples. Because of the significant variations of the cross section observed along the gauge length, the calculation of the tensile stresses is not straightforward. Three simple sections were measured from the tomography scans. The average section along the gauge length was considered as the most suitable. The tensile mechanical properties of the as-built samples were studied and a detrimental effect of the surface state on the yield strength, ultimate tensile strength and elongation to failure was observed. Smoothing of the surface irregularities induced by chemical etching provoked an increase of those mechanical properties whereas the change of the microstructure generated by the HIP treatment leads to a decrease of the material strength that goes along with an increase of the ductility. Down scaling factors were proposed in order to take into account the sample state, as-built or post-treated.

36 MATERIALS SCIENCE↗

Ga lithography in sputtered niobium for superconductive micro and nanowires

This work demonstrates the use of focused ion beam (FIB) implanted Ga as a lithographic mask for plasma etching of Nb films. Using a highly collimated Ga beam of a FIB, Nb is implanted 12 nm deep with a 14 nm thick Ga layer providing etch selectivity better than 15:1 with fluorine based etch chemistry. Implanted square test patterns, both 10 μm by 10 μm and 100 μm by 100 μm, demonstrate that doses above than 7.5 × 10{sup 15 }cm{sup −2} at 30 kV provide adequate mask protection for a 205 nm thick, sputtered Nb film. The resolution of this dry lithographic technique is demonstrated by fabrication of nanowires 75 nm wide by 10 μm long connected to 50 μm wide contact pads. The residual resistance ratio of patterned Nb films was 3. The superconducting transition temperature (T{sub c}) = 7.7 K was measured using a magnetic properties measurement system. This nanoscale, dry lithographic technique was extended to sputtered TiN and Ta here and could be used on other fluorine etched superconductors such as NbN, NbSi, and NbTi.

77 NANOSCIENCE AND NANOTECHNOLOGY↗