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Electrical and physical characterization of the Al{sub 2}O{sub 3}/p-GaSb interface for 1%, 5%, 10%, and 22% (NH{sub 4}){sub 2}S surface treatments

In this work, the impact of ammonium sulfide ((NH{sub 4}){sub 2}S) surface treatment on the electrical passivation of the Al{sub 2}O{sub 3}/p-GaSb interface is studied for varying sulfide concentrations. Prior to atomic layer deposition of Al{sub 2}O{sub 3}, GaSb surfaces were treated in 1%, 5%, 10%, and 22% (NH{sub 4}){sub 2}S solutions for 10 min at 295 K. The smallest stretch-out and flatband voltage shifts coupled with the largest capacitance swing, as indicated by capacitance-voltage (CV) measurements, were obtained for the 1% treatment. The resulting interface defect trap density (D{sub it}) distribution showed a minimum value of 4 × 10{sup 12 }cm{sup −2}eV{sup −1} at E{sub v} + 0.27 eV. Transmission electron microscopy and atomic force microscopy examination revealed the formation of interfacial layers and increased roughness at the Al{sub 2}O{sub 3}/p-GaSb interface of samples treated with 10% and 22% (NH{sub 4}){sub 2}S. In combination, these effects degrade the interface quality as reflected in the CV characteristics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Nanofabrication of Doped, Complex Oxides

Complex oxides have many promising attributes, including wide band gaps for high temperature semiconductors, ion conducting electrolytes in fuel cells, ferroelectricity and ferromagnetism. Bulk and thin film oxides can be readily manufactured and tested however these physically hard and chemically inert materials cannot be nanofabricated by direct application of conventional methods. In order to study these materials at the nanoscale there must first be a simple and effective means to achieve the desired structures. Here we discuss the use of pulsed laser deposition at room temperature onto electron beam lithography defined templates of poly methyl methacrylate photoresist. Following a resist liftoff in organic solvents, a heat treatment was used to crystallize the nanostructures. The morphology of these structures was studied using scanning electron microscopy and atomic force microscopy. Crystallinity and composition as determined by x ray diffraction and photo-electron spectroscopy respectively is reported for thin film analogues of the nanostructured oxide. The oxide studied in this report is Nb doped SrTiO{sub 3}, which has been investigated for use as a high temperature thermoelectric material; however the approach used is not materials-dependent.

30 DIRECT ENERGY CONVERSION↗

Study of the Structural and Morphological Properties of HPHT Diamond Substrates

The morphological and structural properties of a series of high-pressure high-temperature (HPHT) single-crystal diamond substrates are comprehensively studied by white-light optical interference microscopy, atomic-force microscopy, and X-ray diffraction analysis. Procedures that provide a means for characterizing the substrate parameters most critical for epitaxial application with the laboratory equipment are described. It is shown that the jewelry-type characterization of diamond substrates is insufficient to assess the possibility of their use for the epitaxial growth of chemical-vapor-deposited (CVD) diamond.

36 MATERIALS SCIENCE↗

High quality InAlN single layers lattice-matched to GaN grown by molecular beam epitaxy

We report on properties of high quality {approx}60 nm thick InAlN layers nearly in-plane lattice-matched to GaN, grown on c-plane GaN-on-sapphire templates by plasma-assisted molecular beam epitaxy. Excellent crystalline quality and low surface roughness are confirmed by X-ray diffraction, transmission electron microscopy, and atomic force microscopy. High annular dark field observations reveal a periodic in-plane indium content variation (8 nm period), whereas optical measurements evidence certain residual absorption below the band-gap. The indium fluctuation is estimated to be {+-} 1.2% around the nominal 17% indium content via plasmon energy oscillations assessed by electron energy loss spectroscopy with sub-nanometric spatial resolution.

36 MATERIALS SCIENCE↗

Synthesis and characterization in AuCu–Si nanostructures

Au/Cu bilayers with different Au:Cu concentrations (25:75, 50:50 and 75:25 at.%) were deposited on Si(100) substrates by thermal evaporation. The thicknesses of all Au/Cu bilayers were 150 nm. The alloys were prepared by thermal diffusion into a vacuum oven with argon atmosphere at 690 K during 1 h. X-ray diffraction analysis revealed different phases of AuCu and CuSi alloys in the samples after annealing process. CuSi alloys were mainly obtained for 25:75 at.% samples, meanwhile the AuCuII phase dominates for samples prepared with 50:50 at.%. Additionally, the Au:Cu alloys with 75:25 at.%, produce Au{sub 2}Cu{sub 3} and Au{sub 3}Cu phases. The formed alloys were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) to study the morphology and the elemental concentration of the formed alloys. - Highlights: • AuCu/Si alloy thin films were prepared by thermal diffusion. • Alloys prepared with 50 at.% of Au produce the AuCuII phase. • Alloys prepared with 75 at.% of Au produce Au{sub 3}Cu and Au{sub 2}Cu{sub 3} phases. • All alloys present diffusion of Si and Cu through the CuSi alloy formation.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Growth of single and bilayer graphene by filtered cathodic vacuum arc technique

The authors present a viable process to grow the high quality graphene films with control over number of layers by the filtered cathodic vacuum arc (FCVA) technique. In the FCVA process, the different carbon concentrations can be controlled by precisely tuning the arc time (1–4 s). The arc generated carbon was deposited on the nickel catalyst at 800 °C, annealed for 10 min, and cooled down to room temperature in the presence of hydrogen gas, resulting in the graphene films with control over number of layers. Prior to arcing, hydrogen etching of nickel was carried out to clean the surface of the substrate. A growth model to prepare the high quality graphene has also been proposed. The as-grown graphene films were transferred to different substrates and are characterized by Raman spectroscopy, optical microscopy, high resolution transmission electron microscopy, and atomic force microscopy to determine the number of layers present in these films. Raman spectra of the prepared graphene films exhibit change in the G peak position from 1582.4 to 1578.1 cm{sup −1}, two-dimensional (2D) peak shifts from 2688.5 to 2703.8 cm{sup −1}, the value of I{sub 2D}/I{sub G} increased from 0.38 to 3.82, and the full width at half maxima of 2D peak changed from 41 to 70 cm{sup −1}, for different layers of graphene films. The high resolution transmission electron microscopy image revealed that the graphene films prepared for 1 and 2 s arc times have single and bi- or trilayered structures, respectively.

36 MATERIALS SCIENCE↗

Improvement of electron mobility in La:BaSnO{sub 3} thin films by insertion of an atomically flat insulating (Sr,Ba)SnO{sub 3} buffer layer

One perovskite oxide, ASnO{sub 3} (A = Sr, Ba), is a candidate for use as a transparent conductive oxide with high electron mobility in single crystalline form. However, the electron mobility of films grown on SrTiO{sub 3} substrates does not reach the bulk value, probably because of dislocation scattering that originates from the large lattice mismatch. This study investigates the effect of insertion of bilayer BaSnO{sub 3} / (Sr,Ba)SnO{sub 3} for buffering this large lattice mismatch between La:BaSnO{sub 3} and SrTiO{sub 3} substrate. The insertion of 200-nm-thick BaSnO{sub 3} on (Sr,Ba)SnO{sub 3} bilayer buffer structures reduces the number of dislocations and improves surface smoothness of the films after annealing as proved respectively by scanning transmission electron microscopy and atomic force microscopy. A systematic investigation of BaSnO{sub 3} buffer layer thickness dependence on Hall mobility of the electron transport in La:BaSnO{sub 3} shows that the highest obtained value of mobility is 78 cm{sup 2}V{sup −1}s{sup −1} because of its fewer dislocations. High electron mobility films based on perovskite BaSnO{sub 3} can provide a good platform for transparent-conducting-oxide electronic devices and for creation of fascinating perovskite heterostructures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Characterization of nanostructured iron selenide thin films grown by chemical route at room temperature

Highlights: ► Nanostructured FeSe thin films were successfully synthesized at room temperature by CBD method. ► The XRD and EDAX characterization confirms nanocrystalline nature of FeSe. ► The SEM and AFM show microporous morphology with nanorods and nanoplates of FeSe. -- Abstract: Iron selenide thin films have been deposited onto glass substrates by using chemical bath deposition technique. Structural characterization of iron selenide thin films was carried out by means of X-ray diffraction and Fourier transforms infrared spectrum. The morphological characterization of FeSe thin film was carried out using scanning electron microscopy and atomic force microscopy, which revealed porous grain morphology of FeSe with some nano rectangular rods and plates grown on it. The as-deposited thin films exhibited optical band gap energy 2.60 eV. The as deposited FeSe thin films are semiconducting in nature with p-type electrical conductivity. The room temperature electrical resistivity is of the order of 1.1 × 10{sup 5} Ω-cm with activation energy 0.26 and 0.95 eV, respectively, in low and high temperature region.

36 MATERIALS SCIENCE↗

Application of transmission electron microscopy for microstructural characterization of perfluoropentacene thin films

The crystalline structure and orientation of perfluoropentacene (C{sub 22}F{sub 14}, PFP) fibers formed upon thin-film deposition onto SiO{sub 2} substrates have been studied by means of transmission electron microscopy (TEM), atomic force microscopy (AFM), and x-ray diffraction. The synopsis of TEM micrographs and diffraction patterns enhances the understanding of local crystal orientation on small length scales. The relationship of the PFP fiber morphology with the crystalline arrangement of PFP molecules within single fibers was established using this technique. Radiation damage, which is a critical problem for TEM investigations of organic materials, is described and the sample morphology after TEM investigations is correlated with AFM measurements of samples previously examined by TEM.

36 MATERIALS SCIENCE↗

Structural and optical properties of ZnO thin films grown by rapid atmospheric mist chemical vapor technique

In this work, the effect of deposition time on the structural and optical properties of ZnO films deposited by Ultrasonic Spray Mist-CVD was studied aiming the application in perovskite solar cells, as holes blocking layer. Crystallinity, surface morphology and optical properties of the ZnO films were investigated by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), conventional and Photoluminescence (PL) spectroscopies, respectively. The XRD measurement proves the existence of the hexagonal wurtzite phase and a high degree of crystallinity with [001] preferential orientation. The SEM study shows that the films possess a compact structure. Smooth and homogenous surface was confirmed also by AFM. The obtained results indicate that ZnO films deposited by a simple, safe and cost-effective method present a great potential for application in perovskite solar cells.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Plasmonic welded single walled carbon nanotubes on monolayer graphene for sensing target protein

We developed plasmonic welded single walled carbon nanotubes (SWCNTs) on monolayer graphene as a biosensor to detect target antigen molecules, fc fusion protein without any treatment to generate binder groups for linker and antibody. This plasmonic welding induces atomic networks between SWCNTs as junctions containing carboxylic groups and improves the electrical sensitivity of a SWCNTs and the graphene membrane to detect target protein. We investigated generation of the atomic networks between SWCNTs by field-emission scanning electron microscopy and atomic force microscopy after plasmonic welding process. We compared the intensity ratios of D to G peaks from the Raman spectra and electrical sheet resistance of welded SWCNTs with the results of normal SWCNTs, which decreased from 0.115 to 0.086 and from 10.5 to 4.12, respectively. Additionally, we measured the drain current via source/drain voltage after binding of the antigen to the antibody molecules. This electrical sensitivity of the welded SWCNTs was 1.55 times larger than normal SWCNTs.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Diffusion and impurity segregation in hydrogen-implanted silicon carbide

Diffusion and segregation behavior of hydrogen and oxygen in silicon carbide subjected to H implantation and subsequent annealing were studied with a number of analytical techniques including Secondary Ion Mass Spectrometry (SIMS), Rutherford backscattering spectrometry in channeling geometry, field emission scanning electron microscopy, optical microscopy, cross-sectional transmission electron microscopy, and atomic force microscopy. H{sup +} implantation was carried out with energies of 200 keV, 500 keV, or 1 MeV to doses of 1 × 10{sup 16}, 1 × 10{sup 17}, or 2 × 10{sup 17} ion/cm{sup 2}, and thermal treatment was conducted in flowing argon for 1 to 2 h at temperatures of 740, 780, 1000, or 1100 °C. The process of migration and eventual loss of hydrogen in a point defect regime is postulated to proceed to a large extent through ionized vacancies. This conclusion was derived from the observed substantial difference in H mobilities in n- vs. p-type SiC as the population of ionized vacancies is governed by the Fermi-Dirac statistics, i.e., the position of the Fermi level. For higher doses, a well defined buried planar zone forms in SiC at the maximum of deposited energy, comprising numerous microvoids and platelets that are trapping sites for hydrogen atoms. At a certain temperature, a more or less complete exfoliation of the implanted layer is observed. For a 1 MeV implant heated to 1100 °C in nominally pure argon, SIMS profiling reveals a considerable oxygen peak of 10{sup 16} O atoms/cm{sup 2} situated at a depth close to that of the peak of the implanted H{sup +}. Similarly, 1100 °C annealing of a 200 keV implant induces the formation of a thin oxide (4 nm), located at the interface between the implanted layer and the substrate as evidenced by both SIMS and HRTEM. The measurements were taken on the part of the sample that remained un-exfoliated. In view of a lack of convincing evidence that a hexagonal SiC might contain substantial amounts of oxygen, further investigation is under way to elucidate its presence in the irradiation-damaged films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Development of Multifunctional Thin Film Based X-Ray Intensity Filters for Space-Based Payloads

We report the development, thorough characterizations and space worthiness studies of multifunctional aluminized film as x-ray intensity filter for space-based payloads, suitably designed to place in Sun–Earth Lagrangian (L1) point. The L1 point is the ideal location for uninterrupted observation of Sun to study the solar flares in hard x-rays. For our specific purpose, we make use of two different types of x-ray detectors (e.g., CdTe and CZT) which are generally used for hard x-ray studies in the energy band of 5 to 200 keV. Further, these aforesaid two detectors require specified thermal control characteristic for optimal performance. Aluminization of Kapton films is proposed which would satisfy the thermo-optical and x-ray transmission requirements of the proposed payload. The developed aluminized films are thoroughly studied by field emission scanning electron microscopy and atomic force microscopy techniques for micro-structural characteristic, x-ray diffraction for phase purity, nanoindentation for mechanical integrity at micro-structural length scale and spectrophotometer for thermo-optical properties. X-ray transmission test is carried out with two radioactive sources, namely {sup 55}Fe and {sup 241}Am, with various aluminized Kapton layer combinations. Finally, space worthiness of the aluminized Kapton films is examined by accelerated environments, e.g. humidity, thermal cycling and thermo-vacuum tests.

36 MATERIALS SCIENCE↗

Lipid and Protein Transfer between Nanolipoprotein Particles and Supported Lipid Bilayers

A nanolipoprotein particle (NLP) is a lipid bilayer disc stabilized by two amphipathic “scaffold” apolipoproteins. It has been most notably utilized as a tool for solubilizing a variety of membrane proteins while preserving structural and functional properties. Transfer of functional proteins from NLPs into model membrane systems such as supported lipid bilayers (SLBs) would enable new opportunities, for example, two-dimensional protein crystallization and studies on protein–protein interactions. Here we used fluorescence microscopy and atomic force microscopy to investigate the interaction between NLPs and SLBs. When incubated with SLBs, NLPs were found to spontaneously deliver lipid and protein cargo. The impact of membrane composition on lipid exchange was explored, revealing a positive correlation between the magnitude of lipid transfer and concentration of defects in the target SLB. Incorporation of lipids capable of binding specifically to polyhistidine tags encoded into the apolipoproteins also boosted transfer of NLP cargo. Optimal conditions for lipid and protein delivery from NLPs to SLBs are proposed based on interaction mechanisms.

59 BASIC BIOLOGICAL SCIENCES↗

Towards Low-Temperature CVD Synthesis and Characterization of Mono- or Few-Layer Molybdenum Disulfide

Molybdenum disulfide (MoS 2 ) transistors are a promising alternative for the semiconductor industry due to their large on/off current ratio (>10 10 ), immunity to short-channel effects, and unique switching characteristics. MoS 2 has drawn considerable interest due to its intriguing electrical, optical, sensing, and catalytic properties. Monolayer MoS 2 is a semiconducting material with a direct band gap of ~1.9 eV, which can be tuned. Commercially, the aim of synthesizing a novel material is to grow high-quality samples over a large area and at a low cost. Although chemical vapor deposition (CVD) growth techniques are associated with a low-cost pathway and large-area material growth, a drawback concerns meeting the high crystalline quality required for nanoelectronic and optoelectronic applications. This research presents a lower-temperature CVD for the repeatable synthesis of large-size mono- or few-layer MoS 2 using the direct vapor phase sulfurization of MoO 3 . The samples grown on Si/SiO 2 substrates demonstrate a uniform single-crystalline quality in Raman spectroscopy, photoluminescence (PL), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and scanning transmission electron microscopy. These characterization techniques were targeted to confirm the uniform thickness, stoichiometry, and lattice spacing of the MoS 2 layers. The MoS 2 crystals were deposited over the entire surface of the sample substrate. With a detailed discussion of the CVD setup and an explanation of the process parameters that influence nucleation and growth, this work opens a new platform for the repeatable synthesis of highly crystalline mono- or few-layer MoS 2 suitable for optoelectronic application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Amorphous iron–chromium oxide nanoparticles with long-term stability

Highlights: • Fe–Cr oxide nanoparticles with pre-established metals ratio were obtained. • The amorphous state and its long-term stability were highlighted by X-ray diffraction. • The average diameter of dried nanoparticles was 3.5 nm, as was estimated by TEM, AFM. • In hexane dispersion, nanoparticles with diameter in the range 2.33–4.85 nm were found. • Superparamagnetic state of NPs co-exists with diamagnetism of the organic layer. - Abstract: Iron–chromium nanoparticles (NPs) were obtained through the thermal decomposition of μ{sub 3}-oxo heterotrinuclear (FeCr{sub 2}O) acetate in the presence of sunflower oil and dodecylamine (DA) as surfactants. The average diameter of the NPs was 3.5 nm, as estimated on the basis of transmission electron microscopy and atomic force microscopy images. Both techniques revealed the formation of roughly approximated spheres with some irregularities and agglomerations in larger spherical assemblies of 50–100 nm. In hexane, NPs with diameters in the 2.33–4.85 nm range are individually dispersed, as emphasized by dynamic light scattering measurements. The amorphous nature of the product was emphasized by X-ray powder diffraction. The study of the magnetic properties shows the presence of superparamagnetic state of iron–chromium oxide NPs and the diamagnetic contribution from DA layer forming a shell of NPs.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Electrical and gas-sensitive properties of nanostructured SnO{sub 2}:ZrO{sub 2} semiconductor films

The results of a study of the effect of atomic composition of metal-oxide semiconductor composites SnO{sub 2}:ZrO{sub 2} on the surface morphology, polycrystal grain size, resistivity, concentration, free-carrier mobility, and gas-sensitive properties of thin films (0.5-2.5 {mu}m) are presented. Films SnO{sub 2} with ZrO{sub 2} additives (the Zr content was varied from 0.5 to 4.6 at %) are grown by reactive ion-beam sputtering of metal targets of different compositions in a controlled Ar + O{sub 2} atmosphere. Using transmission electron microscopy, atomic-force microscopy, and high-resolution transmission electron microscopy, it is experimentally shown that, as the Zr content increases in the SnO{sub 2}:ZrO{sub 2} film composition, the polycrystal grain size decreases from 45 to 10 nm, the free-carrier concentration decreases almost by four orders of magnitude and the mobility increases by approximately nine times. As the Zr content increases in the SnO{sub 2}:ZrO{sub 2} film from 0.5 to 4.6 at %, the temperature of maximum gas sensitivity of films to such gases as ethanol, isopropyl alcohol, and acetone decreases by 100-190 Degree-Sign C.

36 MATERIALS SCIENCE↗

Corrosion Behavior of Plasma-Nitrided 904L Austenitic Stainless Steel in Hydrofluoric Acid

A new type of high-chromium nickel molybdenum super austenitic stainless steel, 904L, has excellent corrosion resistance in acidic environments. However, the service life of 904L decreases significantly in a mixed acid system that includes hydrogen fluoride and sulfuric acid. In this article, different plasma nitriding processes were used to modify the surface of 904L stainless steel. X-ray diffraction was used to analyze the phase composition after nitriding; scanning electron microscopy and atomic force microscopy were used to examine the surface morphology after nitriding; electrochemical noise and electrochemical methods were used to study the localized corrosion behavior and the damage mechanism of the ion nitride layer; and the effect of the plasma nitride layer on the corrosion resistance was explored. The results show that with increasing nitriding time, the thickness of the nitride layer increased. Ion nitriding resulted in the coarsening of the 904L austenitic stainless steel surface. A long nitriding treatment time resulted in the precipitation of CrN in the modified layer, depleting the chromium from the matrix and remarkably reducing the corrosion resistance.

36 MATERIALS SCIENCE↗