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At least 469 records · Page 26

Facile synthesis of graphene/ZnO nanocomposites by low temperature hydrothermal method

Highlights: ► Graphene/ZnO nanocomposites were prepared by low temperature hydrothermal method. ► Rhodamine-B degraded by using graphene/ZnO nanocomposites. ► ZnO anchored well on the surface of graphene. -- Abstract: Graphene/ZnO nanocomposites have been synthesized using hydrothermal method at two different temperatures 80 and 90 °C. The structure, morphology and optical properties of as synthesized nanocomposites were analyzed through X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy, transmission electron microscopy (TEM) and UV–vis absorbance spectroscopy. The XRD pattern confirmed the formation of graphene decorated by hexagonal ZnO with high crystallinity. FESEM image revealed that the sheet like graphene decorated with ZnO in homogeneously. Decoration of quasi-spherical ZnO nanoparticles on graphene sheet was confirmed by TEM. The characteristic absorbance peaks of graphene/ZnO nanocomposites were observed in UV visible spectra. The photocatalytic degradation experiment was performed against rhodamine-B dye and showed good catalytic activity for both samples. The graphene/ZnO nanocomposites showed higher catalytic activity then ZnO nanoparticles. The GZN-90 sample showed more catalytic activity than GZN-80 due to higher density of ZnO in graphene surface generates large number of photo-induced electron.

36 MATERIALS SCIENCE↗

Femtosecond laser-induced phase transformations in amorphous Cu{sub 77}Ni{sub 6}Sn{sub 10}P{sub 7} alloy

In this study, the femtosecond laser-induced crystallization of CuNiSnP amorphous ribbons was investigated by utilizing an amplified Ti:sapphire laser system. X-ray diffraction and scanning electronic microscope were applied to examine the phase and morphology changes of the amorphous ribbons. Micromachining without crystallization, surface patterning, and selective crystallization were successfully achieved by changing laser parameters. Obvious crystallization occurred under the condition that the laser fluence was smaller than the ablation threshold, indicating that the structural evolution of the material depends strongly on the laser parameters. Back cooling method was used to inhibit heat accumulation; a reversible transformation between the disordered amorphous and crystalline phases can be achieved by using this method.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Two-Dimensional Molecular Charge Density Waves in Single-Layer-Thick Islands of a Dirac Fermion System

Charge density waves have been intensely studied in inorganic materials such as transition metal dichalcogenides however its counterpart in organic materials has yet to be explored in detail. Here we report the finding of a robust two dimensional charge density waves in molecular layers formed by α-(BEDT-TTF) 2 -I 3 on a Ag(111) surface. Low temperature scanning tunnelling microscopy images of a multi-layer thick α-(BEDT-TTF) 2 -I 3 on Ag(111) substrate reveal coexistence of 5a0 x 5a0 and √31 a0 x √31 a0 R9° charge density wave patterns commensurate with the underlying molecular lattice at 80 K. Both charge density wave patterns remain in nano-size molecular islands with just a single constituent molecular-layer thickness at 80 K and 5 K. Local tunneling spectroscopy measurements reveal the variation of the gap from 244 meV to 288 meV between the maximum and minimum charge density wave locations. Density functional theory calculations further confirm a vertical positioning of BEDT-TTF molecules in the molecular layer. While the observed charge density wave patterns are stable for the defect sites, they can be reversely switched for one molecular lattice site by means of inelastic tunnelling electron energy transfer with the electron energies exceeding 400 meV using a scanning tunneling microscope manipulation scheme.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A variable-temperature nanostencil compatible with a low-temperature scanning tunneling microscope/atomic force microscope

We describe a nanostencil lithography tool capable of operating at variable temperatures down to 30 K. The setup is compatible with a combined low-temperature scanning tunneling microscope/atomic force microscope located within the same ultra-high-vacuum apparatus. The lateral movement capability of the mask allows the patterning of complex structures. To demonstrate operational functionality of the tool and estimate temperature drift and blurring, we fabricated LiF and NaCl nanostructures on Cu(111) at 77 K.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Characterization of intermetallics in aluminum to zinc coated interstitial free steel joining by pulsed MIG brazing for automotive application

In order to meet the demand for lighter and more fuel efficient vehicles, a significant attempt is currently being focused toward the substitution of aluminum for steel in the car body structure. It generates vital challenge with respect to the methods of joining to be used for fabrication. However, the conventional fusion joining has its own difficulty owing to formation of the brittle intermetallic phases. In this present study AA6061-T6 of 2 mm and HIF-GA steel sheet of 1 mm thick are metal inert gas (MIG) brazed with 0.8 mm Al–5Si filler wire under three different heat inputs. The effect of the heat inputs on bead geometry, microstructure and joint properties of MIG brazed Al-steel joints were exclusively studied and characterized by X-ray diffraction, field emission scanning electron microscopy (FESEM), electron probe micro analyzer (EPMA) and high resolution transmission electron microscopy (HRTEM) assisted X-ray spectroscopy (EDS) and selective area diffraction pattern. Finally microstructures were correlated with the performance of the joint. Diffusion induced intermetallic thickness measured by FESEM image and concentration profile agreed well with the numerically calculated one. HRTEM assisted EDS study was used to identify the large size FeAl{sub 3} and small size Fe{sub 2}Al{sub 5} type intermetallic compounds at the interface. The growth of these two phases in A2 (heat input: 182 J mm{sup −1}) is attributed to the slower cooling rate with higher diffusion time (~ 61 s) along the interface in comparison to the same for A1 (heat input: 155 J mm{sup −1}) with faster cooling rate and shorter diffusion time (~ 24 s). The joint efficiency as high as 65% of steel base metal is achieved for A2 which is the optimized parameter in the present study. - Highlights: • AA 6061 and HIF-GA could be successfully joined by MIG brazing. • Intermetallics are exclusively studied and characterized by XRD, FESEM and EPMA. • Intermetallic formation by diffusion is worth considering or not. • HRTEM-EDS, SAD pattern identifies the morphologies and size of intermetallics. • A compromise concerning formation of IMC is necessary.

36 MATERIALS SCIENCE↗

AC Susceptibility and Superconducting Properties of Graphene Added YBa{sub 2}Cu{sub 3}O{sub 7−d}

The effect of graphene (G) addition on YBa{sub 2}Cu{sub 3}O{sub 7−δ}(G){sub x} (x = 0 − 0.03 wt%) has been studied using the X-ray diffraction method, scanning electron microscopy, electrical resistance versus temperature, transport critical current density J{sub c}, and AC susceptibility measurements. XRD patterns showed single-phase YBa{sub 2}Cu{sub 3}O{sub 7−δ} (YBCO) for all samples. SEM micrographs showed filling of the voids between YBa{sub 2}Cu{sub 3}O{sub 7−δ} grains as graphene was added. The temperature-dependent electrical resistance curves showed metallic normal state behavior and onset transition temperature T{sub conset} between 90 and 92 K for all samples. AC susceptibility measurement showed transition temperature T{sub cχ{sup ′}} between 90 and 93 K. T{sub cχ{sup ′}} was maintained or improved slightly as graphene was added. The x = 0.001 wt% showed the highest J{sub c}, i.e., 2750 A cm{sup −2} at 77 K and 5570 mA cm{sup −2} at 30 K which was 13 and 40 times higher than that of the non-added YBCO, respectively. The peak temperature T{sub p} of the imaginary part of the susceptibility χ{sup ″} was around 78–82 K for all samples indicating grain coupling was not weakened as graphene was added.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Hydrothermal synthesis of hexagonal magnesium hydroxide nanoflakes

Graphical abstract: Hexagonal Mg(OH){sub 2} nanoflakes were synthesized via hydrothermal method in the presence of PEG-20,000. Results show that PEG-20,000 plays an important role in the formation of this kind of nanostructure. The SAED patterns taken from the different positions on a single hexagonal Mg(OH){sub 2} nanoflake yielded different crystalline structures. The structure of the nanoflakes are polycrystalline and the probable formation mechanism of Mg(OH){sub 2} nanoflakes is discussed. - Highlights: • Hexagonal Mg(OH){sub 2} nanoflakes were synthesized via hydrothermal method. • PEG-20,000 plays an important role in the formation of hexagonal nanostructure. • Mg(OH){sub 2} nanoflakes show different crystalline structures at different positions. • The probable formation mechanism of hexagonal Mg(OH){sub 2} nanoflakes was reported. - Abstract: Hexagonal magnesium hydroxide (Mg(OH){sub 2}) nanoflakes were successfully synthesized via hydrothermal method in the presence of the surfactant polyethylene glycol 20,000 (PEG-20,000). Results show that PEG-20,000 plays an important role in the formation of this kind of nanostructure. The composition, morphologies and structure of the Mg(OH){sub 2} nanoflakes were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED). The SAED patterns taken from the different positions on a single hexagonal Mg(OH){sub 2} nanoflake show different crystalline structures. The structure of the nanoflakes are polycrystalline and the probable formation mechanism of Mg(OH){sub 2} nanoflakes is discussed. Brunauer–Emmett–Teller (BET) analysis were performed to investigate the porous structure and surface area of the as-obtained nanoflakes.

36 MATERIALS SCIENCE↗

Synthesis and characterization of nano ZnO rods via microwave assisted chemical precipitation method

A microwave assisted chemical precipitation method has been employed for the synthesis of nano zinc oxide rods by reacting zinc nitrate and potassium hydroxide. The amount of potassium hydroxide was adjusted for three different pHs to achieve ZnO nano rods with varying aspect ratio. The mechanism of growth of nano rods is explained briefly. The average crystallite size of the as synthesized samples was analyzed by means of powder XRD pattern and estimated to vary from 25.6 nm to 43.1 nm. The existence of rods was confirmed using scanning electron microscopy (SEM). The samples were also analyzed using FT-IR. The optical properties of the samples were also studied by means of UV-visible spectra and Room Temperature Photo Luminescence studies. The band gap of the samples was determined from the DRS spectrum. A strong near band emission peaks due to surface defects are observed in the PL spectrum. - Graphical abstract: At the solution pH of 11 and 9, tetrapod-like and flower-like ZnO nano rods were formed along with separated rods respectively due to the formation of activated nuclei of different sizes. Highlights: Black-Right-Pointing-Pointer Increase in alkalinity of the precursor solution results in longer rods. Black-Right-Pointing-Pointer Beyond a saturation limit, the excess of added OH{sup -} ions inhibited the growth of rods. Black-Right-Pointing-Pointer Keeping all parameters the same, the alkalinity can only modify the aspect ratio of the rods and not their morphology.

36 MATERIALS SCIENCE↗

Alignment of sample position and rotation during in situ synchrotron X-ray micro-diffraction experiments using a Laue cross-correlation approach

Laue micro-diffraction has proven to be able to reveal material properties at the sub-grain scale for many polycrystalline materials and is now routinely available at several synchrotron facilities, providing an approach for nondestructive three-dimensional probing of the microstructures and mechanical states of materials. However, for in situ experiments, maintaining the positioning of the sample throughout the experiment, to achieve a good alignment of the characterized volumes, is a challenging issue. The aim of the present work is to address this problem by developing an approach based on digital image correlation of focused-beam Laue diffraction patterns. The method uses small changes in the diffraction signal as a focused X-ray beam is scanned over a surface region to allow corrections to be made for both sample lateral movement and rotation. The method is demonstrated using a tensile deformation experiment on an Al sample with 2.5 µm average grain size. The results demonstrate an accuracy of 0.5 µm for sample position registration and a precision in sample rotation of ~0.01°. Finally, the proposed method is fast to implement and does not require the use of additional surface markers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Three Dimensional Assembly in Directed Self-assembly of Block Copolymers

The three-dimensional assembly of poly (styrene-b-methyl methacrylate) (PS-b-PMMA) in chemoepitaxy and graphoepitaxy directed self-assembly (DSA) was investigated using scanning transmission electron microscopy (STEM) tomography. The tomographic characterization revealed hidden morphologies and defects at the BCP- chemical pattern interface in lamellar DSA, and probed the formation of cylinders at the bottom of cylindrical DSA for contact hole shrink. Lastly, future work will include control over 3D assembly in sub-10 nm processes.

36 MATERIALS SCIENCE↗

Antiferromagnetic-ferromagnetic phase domain development in nanopatterned FeRh islands

The antiferromagnetic-to-ferromagnetic phase transition in B2-ordered FeRh is imaged in laterally confined nanopatterned islands using photoemission electron microscopy with x-ray magnetic circular dichroism contrast. The resulting magnetic images directly detail the progression in the shape and size of the FM phase domains during heating and cooling through the transition. In 5-μm-square islands this domain development during heating is shown to proceed in three distinct modes - nucleation, growth, and merging - each with subsequently greater energy costs. In 0.5-μm islands, which are smaller than the typical final domain size, the growth mode is stunted and the transition temperature is found to be reduced by 20 K. The modification to the transition temperature is found by high-resolution scanning transmission electron microscopy to be due to a 100-nm chemically disordered edge grain present as a result of ion implantation damage during the patterning. FeRh has unique possibilities for magnetic memory applications; the inevitable changes to its magnetic properties due to subtractive nanofabrication will need to be addressed in future work in order to progress from sheet films to suitable patterned devices.

36 MATERIALS SCIENCE↗

Periodic nanoscale patterning of polyelectrolytes over square centimeter areas using block copolymer templates

Nano-patterned materials are beneficial for applications such as solar cells, opto-electronics, and sensing owing to their periodic structure and high interfacial area. We present a non-lithographic approach for assembling polyelectrolytes into periodic nanoscale patterns over cm 2 -scale areas. We used chemically modified block copolymer thin films featuring alternating charged and neutral domains as patterned substrates for electrostatic self-assembly. In-depth characterization of the deposition process using spectroscopy and microscopy techniques, including the state-of-the-art scanning transmission X-ray microscopy (STXM), reveals both the selective deposition of the polyelectrolyte on the charged copolymer domains as well as gradual changes in the film topography that arise from further penetration of the solvent molecules and possibly also the polyelectrolyte into these domains. Our results demonstrate the feasibility of creating nano-patterned polyelectrolyte layers, which opens up new opportunities for structured functional coating fabrication.

36 MATERIALS SCIENCE↗

SU-F-J-77: Variations in the Displacement Vector Fields Calculated by Different Deformable Image Registration Algorithms Used in Helical, Axial and Cone-Beam CT Images of a Mobile

Purpose: To investigate quantitatively the displacement-vector-fields (DVF) obtained from different deformable image registration algorithms (DIR) in helical (HCT), axial (ACT) and cone-beam CT (CBCT) to register CT images of a mobile phantom and its correlation with motion amplitudes and frequencies. Methods: HCT, ACT and CBCT are used to image a mobile phantom which includes three targets with different sizes that are manufactured from water-equivalent material and embedded in low density foam. The phantom is moved with controlled motion patterns where a range of motion amplitudes (0–40mm) and frequencies (0.125–0.5Hz) are used. The CT images obtained from scanning of the mobile phantom are registered with the stationary CT-images using four deformable image registration algorithms including demons, fast-demons, Horn-Schunk and Locas-Kanade from DIRART software. Results: The DVF calculated by the different algorithms correlate well with the motion amplitudes that are applied on the mobile phantom where maximal DVF increase linearly with the motion amplitudes of the mobile phantom in CBCT. Similarly in HCT, DVF increase linearly with motion amplitude, however, its correlation is weaker than CBCT. In ACT, the DVF’s do not correlate well with the motion amplitudes where motion induces strong image artifacts and DIR algorithms are not able to deform the ACT image of the mobile targets to the stationary targets. Three DIR-algorithms produce comparable values and patterns of the DVF for certain CT imaging modality. However, DVF from fast-demons deviated strongly from other algorithms at large motion amplitudes. Conclusion: In CBCT and HCT, the DVF correlate well with the motion amplitude of the mobile phantom. However, in ACT, DVF do not correlate with motion amplitudes. Correlations of DVF with motion amplitude as in CBCT and HCT imaging techniques can provide information about unknown motion parameters of the mobile organs in real patients as demonstrated in this phantom visibility study.

60 APPLIED LIFE SCIENCES↗

Anti-adhesive characteristics of CHF{sub 3}/O{sub 2} and C{sub 4}F{sub 8}/O{sub 2} plasma-modified silicon molds for nanoimprint lithography

The anti-adhesive characteristics of a plasma-modified silicon mold surface for nanoimprint lithography are presented. Both CHF{sub 3}/O{sub 2} and C{sub 4}F{sub 8}/O{sub 2} plasma were used to form an anti-adhesive layer on silicon mold surfaces. The gas mixing ratios of CHF{sub 3}/O{sub 2} and C{sub 4}F{sub 8}/O{sub 2} were experimentally changed between 0% and 80% to optimize the plasma conditions to obtain a low surface energy of the silicon mold. The plasma characteristics were examined by optical emission spectroscopy (OES). In order to investigate the changes in surface energy and surface chemistry of the anti-adhesive layer during repeated demolding cycles, contact angle measurements and X-ray photoelectron spectroscopy (XPS) were performed on the plasma-modified silicon mold surface. Simultaneously, the surface morphology of the demolded resists was evaluated by field-emission scanning electron microscope (FE-SEM) in order to examine the effect of the anti-adhesive layers on the duplicated patterns of the resists. It was observed that the anti-adhesive layer formed by CHF{sub 3}/O{sub 2} plasma treatment was worn out more easily during repeated demolding cycles than the film formed by C{sub 4}F{sub 8}/O{sub 2} plasma treatment, because CHF{sub 3}/O{sub 2} gas plasma formed a thinner plasma-polymerized film over the same plasma treatment time.

36 MATERIALS SCIENCE↗

Combustion-assisted ink-jet printing of nuclear targets

Advances in target fabrication are critical to high-precision measurements in nuclear physics. This work details the preparation of patterned CeO 2 and ThO 2 architectures and thin-film targets via ink-jet deposition of combustible solutions. The produced targets were characterized by scanning electron microscopy (SEM), and by alpha-particle spectroscopy for radioactive targets to determine densities. Ink jet printing of the targets, used both ethanol and 2-methoxyethanol as solvents, with cerium or thorium nitrate as the oxidizer and acetylacetone as the fuel. Additionally, we found that the distance between each droplet dispersion (step size) played the most significant role in determining the final pattern uniformity and thickness. A 50 μm step size leads to relatively thick targets with a density of 350 μg/cm 2 . Significant overlap in droplet sizes leads to a heterogeneous target with an undesirable cracked surface structure. In contrast, 150 μm spacing yields thinner (20 μg/cm 2 ) patterned structures with excellent surface coverage. This method of Ink-jet printing provides a straightforward, scalable, and high-efficiency pathway to prepare custom made, high-quality targets for nuclear physics experiments.

CeO2↗

Random forest prediction of crystal structure from electron diffraction patterns incorporating multiple scattering

Diffraction is the most common method to solve for unknown or partially known crystal structures. However, it remains a challenge to determine the crystal structure of a new material that may have nanoscale size or heterogeneities. Here, in this study, we train an architecture of hierarchical random forest models capable of predicting the crystal system, space group, and lattice parameters from one or more unknown two-dimensional electron diffraction patterns. Our initial model correctly identifies the crystal system of a simulated electron diffraction pattern from a 20-nm-thick specimen of arbitrary orientation 67% of the time. We achieve a topline accuracy of 79% when aggregating predictions from ten patterns of the same material but different zone axes. The space group and lattice predictions range from 70% to 90% accuracy and median errors of 0.01-0.5Å, respectively, for cubic, hexagonal, trigonal, and tetragonal crystal systems while being less reliable on orthorhombic and monoclinic systems. We apply this architecture to a four-dimensional scanning transmission electron microscopy scan of gold nanoparticles, where it accurately predicts the crystal structure and lattice constants. These random forest models can be used to significantly accelerate the analysis of electron diffraction patterns, particularly in the case of unknown crystal structures. Additionally, due to the speed of inference, these models could be integrated into live transmission electron microscopy experiments, allowing real-Time labeling of a specimen.

36 MATERIALS SCIENCE↗

Power Electronics Materials and Bonded Interfaces - Reliability and Lifetime

The need for reliable bonded interface materials is critical to realize the performance benefits of wide-bandgap devices in power electronic modules, especially in operating temperatures greater than 150 degrees Celsius. In this paper, we investigate the thermomechanical performance of sintered copper (Cu) as a large-area attachment, bonded between Cu baseplates and active-metal-bonded substrates, under accelerated thermal shock (-40 degrees Celsius to 200 degrees Celsius) conditions. In the fabrication phase of the samples, we used different stencil patterns and found out that the grid and stripe patterns resulted in a better outgassing of the residual organics during the sintering process, thereby ensuring a substantially improved bond quality than a full-area print. The paste consisted of Cu microflakes and we performed sintering using a Budatec SP300 sintering press at 275 degrees Celsius with 15 MPa of bonding pressure for 5 minutes in a nitrogen atmosphere. Under accelerated experiments, we monitored the degradation of the sintered Cu bond in the samples through C-mode scanning acoustic microscope (C-SAM) images. To quantify the defect percentage in C-SAM images, we investigated image denoising techniques to exclude the pattern prints. Finally, we cross-sectioned a sample and obtained digital microscope images, which revealed adhesive fracture as the dominant failure mechanism.

ADVANCED PROPULSION SYSTEMS↗

Electrical and structure properties for the alloy system Ce{sub x}La{sub 1−x}O{sub y} nanostructure thin films

Highlights: • Glassy Ce{sub x}La{sub 1−x}O{sub y} nanostructure films were grown on Si(1 0 0) substrate using the sol–gel method. • G{sub p} = ωϵ{sub 0}ϵ′ tan(δ) was calculated at different temperatures. • Electrical and structural the Ce{sub x}La{sub 1−x}O{sub y} samples were studied. • The conductivity-temperature study shows that the compound obeys the Arrhenius law. - Abstract: The Ce{sub x}La{sub 1−x}O{sub y} samples are synthesized, characterized and their electrical properties are reported at different molar ratios in the frequency range of 10{sup −1}–10{sup +5} Hz. Ac conductivity and permittivity data are analyzed by using conductivity formalism. The values of capacitance and tan(δ) were recorded with respect to different frequencies and temperatures. X-ray diffraction (XRD) patterns of the films show that the films posses crystalline phases. Surface morphology of the films is analyzed by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The energy dispersive X-ray (EDX) and X-ray photoelectron spectroscopy (XPS) analyses reveal that elemental composition is in right stoichiometry. Electrical characterizations of the Ce{sub x}La{sub 1−x}O{sub y} samples were done by capacitance–voltage (C–V) and current density–voltage (J–V) measurements of MOS structures. Investigation showed high value of k = 44.80 and low leakage current (∼1 × 10{sup −5} A/cm{sup 2}) of the Ce{sub 0.4}La{sub 0.6}O{sub y} film.

36 MATERIALS SCIENCE↗