Direct observation of single-atom defects in monolayer two-dimensional materials by using electron ptychography at 200 kV acceleration voltage.

Electron ptychography has emerged as a popular technology for high-resolution imaging by combining the high coherence of electron sources with the ultra-fast scanning electron coil. However, the limitations of conventional pixelated detectors, including poor dynamic range and slow data readout speeds, have posed restrictions in the past on conducting electron ptychography experiments. We used the Gatan STELA pixelated detector to capture sequential diffraction data of monolayer two-dimensional (2D) materials for ptychographic reconstruction. By using the pixelated detector and electron ptychography, we demonstrate the observation of the radiation damage at atomic resolution in Transition Metal Dichalcogenides (TMDs).

High-resolution three-dimensional structural determination of unstained double-gyroid block copolymers through scanning transmission electron microscopy.

Block copolymer-based multicomponent materials have garnered considerable attention because of tunable properties due to their various constituents. The use of electron tomography through transmission electron microscopy (TEM) for the three-dimensional (3D) imaging of stained block copolymers is an established approach for investigating structure-property relationships. Recently, scanning transmission electron microscopy (STEM) with an annular dark-field (ADF) detector has emerged as a method for the 3D structural analysis of unstained block copolymers. However, because of a lack of electron contrast, only a few low-resolution 3D reconstructions were reported for light elements. Herein, we report the first 3D structural analysis of a 200-nm-thick film composed of unstained double-gyroid block copolymers-polystyrene-b-poly(2-vinylpyridine) (PS-P2VP)-at a resolution of 8.6 nm through spherical aberration Cs-corrected STEM. At this resolution, P2VP molecules can be distinguished from PS molecules in z-contrast 3D reconstructions obtained both experimentally and theoretically. The 3D reconstructions revealed structural differences between stained and unstained specimens.

Reusable TiN Substrate for Surface Plasmon Resonance Heterodyne Phase Interrogation Sensor.

A TiN-based substrate with high reusability presented high-sensitivity refractive index measurements in a home-built surface plasmon resonance (SPR) heterodyne phase interrogation system. TiN layers with and without additional inclined-deposited TiN (i-TiN) layers on glass substrates reached high bulk charge carrier densities of 1.28 × 1022 and 1.91 × 1022 cm-3, respectively. The additional 1.4 nm i-TiN layer of the nanorod array presented a detection limit of 6.1 × 10-7 RIU and was higher than that of the 46 nm TiN layer at 1.2 × 10-6 RIU when measuring the refractive index of a glucose solution. Furthermore, the long-term durability of the TiN-based substrate demonstrated by multiple processing experiments presented a high potential for various practical sensing applications.

Characterization of silicon oxynitride films deposited by a high-power impulse magnetron sputtering deposition technique.

In this research, silicon oxynitride films were prepared by high-power impulse magnetron sputtering with 45/955 pulse on/off time. The extinction coefficient was smaller than 1×10-3 from 250 to 700 nm after introducing 2.2 sccm O2 gas at room temperature. A three-layer of AlF3/SiOxNy AR coating was designed and fabricated on double-sided quartz, and a high transmittance of 99.2% was attained at 248 nm. The silicon oxynitride films deposited at 350°C had the better mechanical and optical properties in the visible range. The hardness of all deposited films was greater than 19 GPa, and the greatest hardness could reach to 29.8 GPa. A film structure of six-layer transparent hard coating/glass/four-layer AR coating was designed and deposited. Its average transmittance was 96.0% in the visible range, while its hardness was 21 GPa and its surface roughness was 0.23 nm.

CVD growth of large-area InS atomic layers and device applications.

Group-III monochalcogenides of two-dimensional (2D) layered materials have attracted widespread attention among scientists due to their unique electronic performance and interesting chemical and physical properties. Indium sulfide (InS) is attracting increasing interest from scientists because it has two distinct crystal structures. However, studies on the synthesis of highly crystalline, large-area, and atomically thin-film InS have not been reported thus far. Here, the chemical vapor deposition (CVD) synthesis method of atomic InS crystals has been reported in this paper. The direct chemical vapour phase reaction of metal oxides with chalcogen precursors produces a large-sized hexagonal crystal structure and atomic-thickness InS flakes or films. The InS atomic films are merged with a plurality of triangular InS crystals that are uniform and entire and have surface areas of 1 cm2 and controllable thicknesses in bilayers or trilayers. The properties of the as-grown highly crystalline samples were characterized by spectroscopic and microscopic measurements. The ion-gel gated InS field-effect transistors (FETs) reveal n-type transport behavior, and have an on-off current ratio of >103 and a room-temperature electron mobility of ∼2 cm2 V-1 s-1. Moreover, our CVD InS can be transferred from mica to any substrates, so various 2D materials can be reassembled into vertically stacked heterostructures, thus facilitating the development of heterojunctions and exploration of the properties and applications of their interactions.

Synthesis of Large-Area InSe Monolayers by Chemical Vapor Deposition.

Recently, 2D materials of indium selenide (InSe) layers have attracted much attention from the scientific community due to their high mobility transport and fascinating physical properties. To date, reports on the synthesis of high-quality and scalable InSe atomic films are limited. Here, a synthesis of InSe atomic layers by vapor phase selenization of In2 O3 in a chemical vapor deposition (CVD) system, resulting in large-area monolayer flakes or thin films, is reported. The atomic films are continuous and uniform over a large area of 1 × 1 cm2 , comprising of primarily InSe monolayers. Spectroscopic and microscopic measurements reveal the highly crystalline nature of the synthesized InSe monolayers. The ion-gel-gated field-effect transistors based on CVD InSe monolayers exhibit n-type channel behaviors, where the field effect electron mobility values can be up to ≈30 cm2 V-1 s-1 along with an on/off current ratio, of >104 at room temperature. In addition, the graphene can serve as a protection layer to prevent the oxidation between InSe and the ambient environment. Meanwhile, the synthesized InSe films can be transferred to arbitrary substrates, enabling the possibility of reassembly of various 2D materials into vertically stacked heterostructures, prompting research efforts to probe its characteristics and applications.

Interplay of mutual electric and magnetic couplings between three-dimensional split-ring resonators.

We experimentally and theoretically study the interplay between capacitive electric and inductive magnetic couplings in infrared metamaterials consisting of densely-packed three-dimensional (3D) meta-atoms. The meta-atom is made of metal-stress-driven assembled 3D split-ring resonators to exhibit strong bi-anisotropy, where electric and magnetic resonances occur simultaneously. By varying the spatial arrangement of the arrayed meta-atoms, the mutual coupling between meta-atoms dramatically modifies their mode profiles and resultant spectral responses. The corresponding numerical simulations evidently retrieved current densities and magnetic field strengths, as well as the transmittance, to reveal the important resonant behavior in the coupled meta-atom systems. We conclude that the mutual electric coupling between the neighboring meta-atoms plays a crucial role to the scattering behaviors of the bi-anisotropic metamaterials.

Preparation of Aluminum Oxide-Coated Glass Slides for Glycan Microarrays.

In this study, we report the fabrication of aluminum oxide-coated glass (ACG) slides for the preparation of glycan microarrays. Pure aluminum (Al, 300 nm) was coated on glass slides via electron-beam vapor deposition polymerization (VDP), followed by anodization to form a thin layer (50-65 nm) of aluminum oxide (Al-oxide) on the surface. The ACG slides prepared this way provide a smooth surface for arraying sugars covalently via phosphonate formation with controlled density and spatial distance. To evaluate this array system, a mannose derivative of α-5-pentylphosphonic acid was used as a model for the optimization of covalent arraying based on the fluorescence response of the surface mannose interacting with concanavalin A (ConA) tagged with the fluorescence probe A488. The ACG slide was characterized using scanning electron microscopy, atomic force microscopy (AFM), and ellipsometry, and the sugar loading capacity, uniformity, and structural conformation were also characterized using AFM, a GenePix scanner, and a confocal microscope. This study has demonstrated that the glycan array prepared from the ACG slide is more homogeneous with better spatial control compared with the commonly used glycan array prepared from the N-hydroxysuccinimide-activated glass slide.

Facile Preparation of a Platinum Silicide Nanoparticle-Modified Tip Apex for Scanning Kelvin Probe Microscopy.

In this study, we propose an ultra-facile approach to prepare a platinum silicide nanoparticle-modified tip apex (PSM tip) used for scanning Kelvin probe microscopy (SKPM). We combined a localized fluoride-assisted galvanic replacement reaction (LFAGRR) and atmospheric microwave annealing (AMA) to deposit a single platinum silicide nanoparticle with a diameter of 32 nm on the apex of a bare silicon tip of atomic force microscopy (AFM). The total process was completed in an ambient environment in less than 3 min. The improved potential resolution in the SKPM measurement was verified. Moreover, the resolution of the topography is comparable to that of a bare silicon tip. In addition, the negative charges found on the PSM tips suggest the possibility of exploring the use of current PSM tips to sense electric fields more precisely. The ultra-fast and cost-effective preparation of the PSM tips provides a new direction for the preparation of functional tips for scanning probe microscopy.

A facile approach to prepare silicon-based Pt-Ag tubular dendritic nano-forests (tDNFs) for solar-light-enhanced methanol oxidation reaction.

In this paper, a facile two-step Galvanic replacement reaction (GRR) is proposed to prepare Pt-Ag tubular dendritic nano-forests (tDNFs) in ambient condition for enhancing methanol oxidation reaction (MOR) under solar illumination. In the first GRR, a homogeneous layer of silver dendritic nano-forests (DNFs) with 10 µm in thickness was grown on Si wafer in 5 min in silver nitride (AgNO3) and buffer oxide etchant (BOE) solution. In the second GRR, we utilized chloroplatinic acid (H2PtCl6) as the precursor for platinum (Pt) deposition to further transform the prepared Ag DNFs into Pt-Ag tDNFs. The catalytic performance and solar response of the Pt-Ag tDNFs toward methanol electro-oxidation are also studied by cyclic voltammetry (CV) and chronoamperometry (CA). The methanol oxidation current was boosted by 6.4% under solar illumination on the Pt-Ag tDNFs due to the induced localized surface plasmon resonance (LSPR) on the dendritic structure. Current results provide a cost-effective and facile approach to prepare solar-driven metallic electrodes potentially applicable to photo-electro-chemical fuel cells.

Interfacial atomic structure analysis at sub-angstrom resolution using aberration-corrected STEM.

The atomic structure of a SiGe/Si epitaxial interface grown via molecular beam epitaxy on a single crystal silicon substrate was investigated using an aberration-corrected scanning transmittance electron microscope equipped with a high-angle annular dark-field detector and an energy-dispersive spectrometer. The accuracy required for compensation of the various residual aberration coefficients to achieve sub-angstrom resolution with the electron optics system was also evaluated. It was found that the interfacial layer was composed of a silicon single crystal, connected coherently to epitaxial SiGe nanolaminates. In addition, the distance between the dumbbell structures of the Si and Ge atoms was approximately 0.136 nm at the SiGe/Si interface in the [110] orientation. The corresponding fast Fourier transform exhibited a sub-angstrom scale point resolution of 0.78 Å. Furthermore, the relative positions of the atoms in the chemical composition line scan signals could be directly interpreted from the corresponding incoherent high-angle annular dark-field image.

Effect of In/Al ratios on structural and optical properties of InAlN films grown on Si(100) by RF-MOMBE.

In x Al1-x N films were deposited on Si(100) substrate using metal-organic molecular beam epitaxy. We investigated the effect of the trimethylindium/trimethylaluminum (TMIn/TMAl) flow ratios on the structural, morphological, and optical properties of In x Al1-x N films. Surface morphologies and microstructure of the In x Al1-x N films were measured by atomic force microscopy, scanning electron microscopy, X-ray diffraction (XRD), and transmission electron microscopy (TEM), respectively. Optical properties of all films were evaluated using an ultraviolet/visible/infrared (UV/Vis/IR) reflection spectrophotometer. XRD and TEM results indicated that In x Al1-x N films were preferentially oriented in the c-axis direction. Besides, the growth rates of In x Al1-x N films were measured at around 0.6 µm/h in average. Reflection spectrum shows that the optical absorption of the In x Al1-x N films redshifts with an increase in the In composition.

Improving optical properties of silicon nitride films to be applied in the middle infrared optics by a combined high-power impulse/unbalanced magnetron sputtering deposition technique.

Silicon nitride films are prepared by a combined high-power impulse/unbalanced magnetron sputtering (HIPIMS/UBMS) deposition technique. Different unbalance coefficients and pulse on/off ratios are applied to improve the optical properties of the silicon nitride films. The refractive indices of the Si3N4 films vary from 2.17 to 2.02 in the wavelength ranges of 400-700 nm, and all the extinction coefficients are smaller than 1×10(-4). The Fourier transform infrared spectroscopy and x-ray diffractometry measurements reveal the amorphous structure of the Si3N4 films with extremely low hydrogen content and very low absorption between the near IR and middle IR ranges. Compared to other deposition techniques, Si3N4 films deposited by the combined HIPIMS/UBMS deposition technique possess the highest refractive index, the lowest extinction coefficient, and excellent structural properties. Finally a four-layer coating is deposited on both sides of a silicon substrate. The average transmittance from 3200 to 4800 nm is 99.0%, and the highest transmittance is 99.97% around 4200 nm.

Conductive and transparent multilayer films for low-temperature TiO2/Ag/SiO2 electrodes by E-beam evaporation with IAD.

Conductive and transparent multilayer thin films consisting of three alternating layers (TiO2/Ag/SiO2, TAS) have been fabricated for applications as transparent conducting oxides. Metal oxide and metal layers were prepared by electron-beam evaporation with ion-assisted deposition, and the optical and electrical properties of the resulting films as well as their energy bounding characteristics and microstructures were carefully investigated. The optical properties of the obtained TAS material were compared with those of well-known transparent metal oxide glasses such as ZnO/Ag/ZnO, TiO2/Ag/TiO2, ZnO/Cu/ZnO, and ZnO/Al/ZnO. The weathering resistance of the TAS film was improved by using a protective SiO2 film as the uppermost layer. The transmittance spectra and sheet resistance of the material were carefully measured and analyzed as a function of the layer thickness. By properly adjusting the thickness of the metal and dielectric films, a low sheet resistance of 6.5 ohm/sq and a high average transmittance of over 89% in the 400 to 700 nm wavelength regions were achieved. We found that the Ag layer played a significant role in determining the optical and electrical properties of this film.

Study of a sandwich structure of transparent conducting oxide films prepared by electron beam evaporation at room temperature.

Transparent conducting ZnO/Ag/ZnO multilayer electrodes having electrical resistance much lower than that of widely used transparent electrodes were prepared by ion-beam-assisted deposition (IAD) under oxygen atmosphere. The optical parameters were optimized by admittance loci analysis to show that the transparent conducting oxide (TCO) film can achieve an average transmittance of 93%. The optimum thickness for high optical transmittance and good electrical conductivity was found to be 11 nm for Ag thin films and 40 nm for ZnO films, based on the admittance diagram. By designing the optical thickness of each ZnO layer and controlling process parameters such as IAD power when fabricating dielectric-metal-dielectric films at room temperature, we can obtain an average transmittance of 90% in the visible region and a bulk resistivity of 5 × 10-5 Ω-cm. These values suggest that the transparent ZnO/Ag/ZnO electrodes are suitable for use in dye-sensitized solar cells.

Study of surface morphology control and investigation of hexagonal indium nitride nanorods grown on GaN/sapphire substrate.

Heteroepitaxial growth of metal-catalyst-free indium nitride (InN) nanorods on GaN/sapphire substrates by radio-frequency metal-organic molecular beam epitaxy (RF-MOMBE) system was investigated. We found that different N/In flow ratios together with the growth temperatures greatly influenced the surface morphology of InN nanorods and their structural properties. The InN nanorods have been characterized in detail using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM). Optical property was evaluated by photoluminescence (PL) measurements. At lower growth temperatures, InN nanorods were successfully grown. A pronounced two-dimensional growth mode was observed at higher growth temperature of 500 degrees C, and these films showed preferred orientation along the c-axis. XRD patterns and SEM images reveal that InN nanorods has high quality wurtzite structure with FWHM approaching 900 arcsec, and they have uniform diameters of about 150 nm and length of about 800 nm. Meanwhile, no metallic droplet was observed at the end of the nanostructured InN, and this is strong evidence that the nanorods are grown via the self-catalyst process. The PL peak at 0.8 eV is attributed to the quantum confinement and Moss-Burstein effects. These observations provide some valuable insights into the physical-chemical process for manufacturing InN nanorods devices.

Fine structure of wing scales of butterflies, Euploea mulciber and Troides aeacus.

Wing scales of male Euploea mulciber (E. mulciber) and Troides aeacus (T. aeacus) butterflies were investigated from interest in photonic crystal by scanning electron microscopy and optical reflectance measurement. On the basis of the structural observation, the colouration in different areas in their wings was discussed. It was particularly deduced that a violet-green iridescence characteristic of E. mulciber's forewing is caused only in a wavelength range from ∼380 to ∼510nm by multiple interference from a highly tilted, triple-layered cuticle arrangement on the brown scales. It was also found that T. aeacus does not produce a blue-green sheen such as observed by Troides magellanus because its scales have no multiple cuticle layers but microrib layers unable to produce any backscattering diffraction.